EP0603411A1 - Ceramic heating/cooling device - Google Patents

Ceramic heating/cooling device Download PDF

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Publication number
EP0603411A1
EP0603411A1 EP93913596A EP93913596A EP0603411A1 EP 0603411 A1 EP0603411 A1 EP 0603411A1 EP 93913596 A EP93913596 A EP 93913596A EP 93913596 A EP93913596 A EP 93913596A EP 0603411 A1 EP0603411 A1 EP 0603411A1
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EP
European Patent Office
Prior art keywords
heating
ceramics
cooling apparatus
sintered body
cooling
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Granted
Application number
EP93913596A
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German (de)
French (fr)
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EP0603411A4 (en
EP0603411B1 (en
Inventor
Keiichi Katoh
Syuzi Ueda
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Individual
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Individual
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Priority claimed from JP19155393A external-priority patent/JPH0699085A/en
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Publication of EP0603411A4 publication Critical patent/EP0603411A4/en
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/20Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
    • H05B3/22Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
    • H05B3/28Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material
    • H05B3/283Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material the insulating material being an inorganic material, e.g. ceramic
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L7/00Heating or cooling apparatus; Heat insulating devices
    • B01L7/52Heating or cooling apparatus; Heat insulating devices with provision for submitting samples to a predetermined sequence of different temperatures, e.g. for treating nucleic acid samples
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28FDETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F21/00Constructions of heat-exchange apparatus characterised by the selection of particular materials
    • F28F21/04Constructions of heat-exchange apparatus characterised by the selection of particular materials of ceramic; of concrete; of natural stone
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/10Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material

Definitions

  • the present invention relates to a heating/cooling apparatus made of a ceramics, which permits a rapid heating and a rapid cooling of various samples in such fields as biotechnology, chemistry, medicine and bioengineering, and achievement of a precise temperature control of the sample and a uniform temperature distribution in the sample.
  • a heating/cooling apparatus of any of these types, a receptacle made of a metal such as aluminum or the like for receiving an object to be heated or cooled, i.e., a sample, and a heating means are configured as two separate components. This results in a poorer heat transfer coefficiency from the heating means to the receptacle for the sample, makes it difficult to rapidly heat the sample, and furthermore, leads to a non-uniform temperature distribution in the sample. It is therefore difficult to achieve a desired heating pattern.
  • the available cooling means of the sample include, on the other hand, a spontaneous cooling, a forced cooling with the use of a coolant such as a gas or a liquid, and a combination thereof. It is however difficult to precisely control a cooling rate by such a cooling means alone. It is thus conceivable to control the cooling rate by using any of the above-mentioned cooling means while supplying a prescribed heat quantity from the heating means to the sample. In this manner of cooling, however, the heat supplied by the heating means cannot be efficiently transferred to the receptacle for the sample. It is therefore difficult to rapidly decrease the sample temperature to a desired temperature, and moreover, the temperature distribution in the sample is non-uniform, resulting in difficulty in achieving a desired cooling pattern.
  • An object of the present invention is therefore to provide a heating/cooling apparatus made of a ceramics, which solves the above-mentioned problems, and permits a rapid heating and a rapid cooling of various samples, allows a precise temperature control of the sample, thereby enabling a temperature control of the sample in accordance with a predetermined temperature pattern, and achieving a uniform temperature distribution in the sample.
  • At least one of a face, at least one hole, at least one recess and at least one groove, the shape of which coincides with that of an object to be heated or cooled, i.e., a sample, for receiving the sample, to increase a contact area with the sample, is formed at an arbitrary position on a sintered body comprising an electrically insulating ceramics having a thermal conductivity of at least 10 W/(m ⁇ k) .
  • An electrically conductive resistance-heating element comprising a metal, an electrically conductive ceramics or carbon is buried into the sintered body.
  • the whole of the above-mentioned sintered body may comprise an electrically conductive ceramics, thereby the sintered body itself forming a resistance-heating element as a heating means.
  • the heating/cooling apparatus made of a ceramics of the present invention further comprises a cooling means.
  • the cooling means comprises a coolant feeder, provided outside the sintered body, for feeding a coolant such as a gas or a liquid to the sintered body, on the one hand, and at least one of part of a surface of the sintered body, a rugged portion formed on part of a surface of the sintered body, at least one cooling through-hole, through which the coolant passes, formed in the sintered body, a heat-radiating plate having fins, provided on the sintered body, and a heat-radiating plate having a honeycomb structure, provided on the sintered body, each for effecting a heat exchange, on the other hand.
  • the heat-radiating plate comprises any one of a metal and a ceramics.
  • the sample is in contact with the face, at least one hole, at least one recess or at least one groove, each for receiving the sample, provided on the sintered body having a satisfactory thermal conductivity, so that the temperature of the sample rapidly becomes equal to the temperature of the sintered body, thus permitting a precise temperature control during the heating and the cooling of the sample.
  • Fig. 1 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a first embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
  • Fig. 2 is a schematic sectional view of Fig. 1 cut along the line A-A'.
  • Fig. 3 is a schematic exploded perspective view illustrating a manufacturing process of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention shown in Fig. 1.
  • Fig. 4 is a schematic descriptive view illustrating a combination of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention shown in Fig. 1, and a coolant feeder.
  • Fig. 5 is a graph illustrating a predetermined temperature pattern in a performance test of a heating/cooling apparatus made of a ceramics.
  • Fig. 6 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a second embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
  • Fig. 7 is a schematic sectional view of Fig. 6 cut along the line A-A'.
  • Fig. 8 is a schematic perspective view illustrating two green blocks for the heating/cooling apparatus made of a ceramics of the second embodiment of the present invention shown in Fig. 6.
  • Fig. 9 is a schematic perspective view illustrating the state in which a resistance-heating element is attached onto one of the two green blocks shown in Fig. 8.
  • Fig. 10 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a third embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and a heat-radiating plate having fins, as a cooling means.
  • Fig. 11 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fourth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and at least one cooling through-hole as a cooling means, formed in the sintered body.
  • Fig. 12 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fifth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising silicon carbide.
  • Fig. 13 is a schematic perspective view illustrating a green block for the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention shown in Fig. 12.
  • Fig. 14 is a schematic perspective view illustrating a green block having holes formed therein for receiving objects to be heated or cooled, i.e., samples, for the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention shown in Fig. 12.
  • Fig. 15 is a schematic descriptive view illustrating a combination of the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention shown in Fig. 12, and a coolant feeder.
  • Fig. 16 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a sixth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, provided with at least one peephole.
  • Fig. 17 is a schematic sectional view of Fig. 16 cut along the line A-A'.
  • Fig. 18 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a seventh embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
  • Fig. 19 is a schematic sectional view of Fig. 18 cut along the line A-A'.
  • Fig. 20 is a schematic sectional view of Fig. 18 cut along the line B-B', illustrating the heating/cooling apparatus made of a ceramics of the seventh embodiment of the present invention shown in Fig. 18, which is attached with a sample receptacle.
  • Fig. 1 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a first embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride
  • Fig. 2 is a schematic sectional view of Fig. 1 cut along the line A-A'.
  • the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention is manufactured as follows. As shown in Fig. 3, holes 2 and 3 for receiving samples are formed in each of green sheets 7, 8 and 10 made of a ceramics comprising aluminum nitride.
  • a resistance-heating element 5 is formed on the surface of the green sheet 8 by a method such as a screen printing. Then, the green sheets 7, 8 and 10 are piled one upon another, and a sintered body 1 is formed by sintering these green sheets 7, 8 and 10 thus piled up.
  • the sintered body 1 thus formed has a shape as shown in Fig. 1, and the side surfaces opposite to each other have electrodes 4 and 4', respectively, connected to the resistance-heating element 5.
  • FIG. 4 is a schematic descriptive view illustrating a combination of the above-mentioned heating/cooling apparatus of the first embodiment of the present invention, and a coolant feeder.
  • a cooling gas was supplied to the heating/cooling apparatus by means of a blower 11 as a coolant feeder.
  • test tubes having a thermocouple received therein was inserted into each of the holes 2 and 3 to investigate the performance of the heating/cooling apparatus.
  • Temperature of each test tube was subjected to a PID (abbreviation of proportional-plus-integral-plus-derivative) control on the basis of the temperature measured by the thermocouple, so that the temperature of the test tube coincide with a target temperature.
  • Electric power of the resistance-heating element 5 was controlled with the use of a thyristor.
  • the performance test was carried out as follows. Two test tubes filled with objects to be heated or cooled, i.e., samples, were inserted respectively into the holes 2 and 3 for receiving samples of the heating/cooling apparatus, and the samples were heated or cooled with the use of the above-mentioned heating/cooling apparatus in accordance with a predetermined temperature pattern as shown in Fig. 5, thereby precisely controlling the temperature of the samples. More specifically, the test tubes each receiving 1.5 ml of pure water were inserted respectively into the holes 2 and 3, each having an inside diameter agreeing with the outside diameter of the test tubes, of the heating/cooling apparatus shown in Fig. 1. A thermocouple for measuring temperature was immersed into the middle of pure water received in each of the test tubes. Pure water in each of the two test tubes showed an initial temperature of 17 °C, as measured by the thermocouple.
  • a program regarding set temperatures and set periods for heating and cooling pure water was input into a controller for controlling the operation of the heating/cooling apparatus.
  • the above-mentioned program comprised, as shown in Fig. 5: increasing the temperature of pure water to 95°C (hereinafter referred to as the "first set temperature”), then keeping this temperature for ten minutes (hereinafter referred to as the "first set period”), then decreasing the temperature of pure water to 4°C (hereinafter referred to as the "second set temperature”), then keeping this temperature for 60 minutes (hereinafter referred to as the "second set period”), then increasing again the temperature of pure water to 25°C (hereinafter referred to as the "third set temperature”), then keeping this temperature for 20 minutes (hereinafter referred to as the "third set period” ), and then discontinuing the operation of the heating/cooling apparatus.
  • the heating/cooling apparatus was operated under the control by means of the controller, and actual changes in temperature with time of pure water received in each of the two test tubes, were measured by the thermocouple.
  • the results of measurement were as follows. Upon the lapse of eight seconds after the start of operation of the heating/cooling apparatus, the temperature of pure water in each of the test tubes increased to 95 °C which was the first set temperature. Thereafter, during ten minutes which were the first set period, the temperature of pure water in each of the test tubes was kept at a temperature of 95 ⁇ 0.1°C. Then, upon the lapse of 20 seconds after the first set period, the temperature of pure water in each of the test tubes decreased to 4°C which was the second set temperature.
  • the temperature of pure water in each of the test tubes was kept at a temperature of 4 ⁇ 0.1°C. Subsequently, upon the lapse of two seconds after the second set period, the temperature of pure water in each of the test tubes increased to 25°C which was the third set temperature. Then, during 20 minutes which were the third set period, the temperature of pure water in each of the test tubes was kept at a temperature of 25 ⁇ 0.1°C, and thereafter, the operation of the heating/cooling apparatus was discontinued.
  • the sintered body 1 of the heating/cooling apparatus made of a ceramics of the above-mentioned first embodiment of the present invention has been described above as comprising an electrically insulating ceramics comprising aluminum nitride.
  • the sintered body 1 may however comprise an electrically insulating ceramics comprising at least one of silicon carbide, silicon nitride, aluminum oxide and beryllium oxide, other than aluminum nitride.
  • the material for forming the resistance-heating element 5 is not limited to at least one metal selected from the group consisting of tungsten, molybdenum and rhenium, but may be carbon, and furthermore, may be at least one electrically conductive ceramics selected from the group consisting of silicon carbide, titanium nitride, molybdenum silicide, zirconium boride, tungsten carbide and tantalum carbide.
  • the resistance-heating element 5 is buried in the form of a single layer into the sintered body 1.
  • a resistance-heating element comprising a plurality of layers may be buried into the sintered body 1.
  • the holes 2 and 3 for receiving the samples may have any shape in any number.
  • Fig. 6 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a second embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride
  • Fig. 7 is a schematic sectional view of Fig. 6 cut along the line A-A'.
  • the heating-cooling apparatus made of a ceramics of the second embodiment of the present invention is manufactured as follows. A powdery raw material comprising aluminum nitride is charged into a metallic mold not shown to form two green blocks 21 and 22 as shown in Fig. 8.
  • resistance-heating elements 19 and 20 each comprising a coiled wire made of at least one metal selected from the group consisting of tungsten, molybdenum and rhenium, are arranged on the surface of the green block 22 as shown in Fig. 9.
  • the other green block 21 is placed upon the green block 22, and as shown in Figs. 6 and 7, holes 13, 14, 15 and 16 for receiving samples are formed by means of a cutting.
  • the two green blocks thus provided with the holes are sintered by a hot press method, thereby preparing a sintered body 12 made of a ceramics comprising aluminum nitride having the resistance-heating elements 19 and 20 buried therein.
  • the side surfaces of the sintered body 12 are ground to expose ends of the coiled wires as the resistance-heating elements 19 and 20.
  • electrodes 17 and 18 are brazed onto the ends of the coiled wires thus exposed.
  • a performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned second embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of the ceramics of the first embodiment of the present invention.
  • a blower as a coolant feeder was arranged below the heating/cooling apparatus, thereby blowing a cooling gas toward the heating-cooling apparatus to cool same.
  • the temperature of the sample was controlled also in the same manner as in the performance test of the heating/cooling apparatus of the first embodiment of the present invention.
  • the heating/cooling apparatus of the second embodiment of the present invention there were obtained excellent results of the performance test as in the heating/cooling apparatus of the first embodiment of the present invention. Furthermore, the heating/cooling apparatus of the second embodiment of the present invention was improved by providing a rugged portion or fins by means of a grinding on part of the surface of the sintered body 12, and the same performance test as described above was carried out for each of such improvements. There were obtained excellent results of the performance test as in the heating/cooling apparatus of the second embodiment of the present invention. Particularly within a range of temperature of from 100 to 600°C, there was available a cooling rate higher than that in the heating/cooling apparatus of the first embodiment of the present invention.
  • the holes 13, 14, 15 and 16 for receiving samples may be of any shape in any number, and the resistance-heating elements 19 and 20 may be in any number.
  • Fig. 10 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a third embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and a heat-radiating plate having fins, as a cooling means.
  • the heating/cooling apparatus of the third embodiment of the present invention is configured by forming a metallic layer comprising at least one metal of copper, nickel, molybdenum and manganese on the lower surface of the heating/cooling apparatus of the above-mentioned second embodiment of the present invention, and then brazing a metallic heat-radiating plate 30 having fins, as a cooling means, onto the metallic layer.
  • 23 is a sintered body; 24, 25, 26 and 27 are holes for receiving samples; and 28 and 29 are electrodes.
  • a performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned third embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention. Also in the performance test of the heating/cooling apparatus of the third embodiment of the present invention, there were obtained excellent results of the performance test as in the heating/cooling apparatus of the first embodiment of the present invention. Particularly within a range of temperature of from 100 to 600°C, there was available a cooling rate higher than that of the heating/cooling apparatus of the first embodiment of the present invention.
  • the metallic heat-radiating plate 30 having fins, as a cooling means has been described as being provided on the lower surface of the sintered body 23.
  • the above-mentioned heat-radiating plate 30 may be provided on a surface other than the lower surface of the sintered body 23, for example, on a side surface thereof.
  • the above-mentioned heat-radiating plate 30 may have a honeycomb structure in place of the fins.
  • Fig. 11 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fourth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and at least one cooling through-hole as a cooling means, formed in the sintered body.
  • the heating/cooling apparatus of the fourth embodiment of the present invention is configured by forming cooling through-holes 38 and 39 as cooling means, as shown in Fig. 11, by means of an ultrasonic working, a diamond grinding or the like, in the sintered body of the heating/cooling apparatus of the second embodiment of the present invention.
  • 31 is a sintered body; 32, 33, 34 and 35 are holes for receiving samples; and 36 and 37 are electrodes.
  • a cooling gas is supplied into the cooling through-holes 38 and 39.
  • a performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned fourth embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention. Also in the performance test of the heating/cooling apparatus of the fourth embodiment of the present invention, there were obtained excellent results of the performance test as in the heating/cooling apparatus of the first embodiment of the present invention. Particularly within a range of temperature of from 100 to 600 °C, there was available a cooling rate higher than that of the heating/cooling apparatus of the first embodiment of the present invention.
  • a cooling gas has been described as being supplied into the cooling through-holes 38 and 39 as the cooling means.
  • a liquid coolant may be supplied into the cooling through-holes 38 and 39.
  • a partition having a honeycomb structure may be provided as required in each of the cooling through-holes 38 and 39.
  • Fig. 12 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fifth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising silicon carbide.
  • 40 is a sintered body made of an electrically conductive ceramics comprising silicon carbide; and 41 and 42 are holes for receiving samples.
  • the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention is manufactured as follows. A powdery raw material comprising an electrically conductive ceramics comprising silicon carbide is charged into a metallic mold not shown to form a green block 45 as shown in Fig. 13. Then, as shown in Fig. 14, holes 41 and 42 for receiving samples are formed in the green block 45 by means of a cutting.
  • the green block 45 thus provided with the holes 41 and 42 is sintered under the known sintering conditions.
  • metallic layers as electrodes 43 and 44 are attached, as shown in Fig. 12, onto the opposing side surfaces of the resultant sintered body 40, respectively.
  • the sintered body 40 itself forms a resistance-heating element serving as a heating means. There is no need therefore to specifically provide resistance-heating element in the sintered body 40.
  • a performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned fifth embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention.
  • a blower 50 as a coolant feeder was arranged, as shown in Fig. 15, below the heating/cooling apparatus, thereby blowing a cooling gas toward the heating/cooling apparatus to cooling same.
  • the sintered body 40 of the heating/cooling apparatus of the fifth embodiment of the present invention has been described above as comprising an electrically conductive ceramics comprising silicon carbide, but the sintered body 40 may comprise any one electrically conductive ceramics selected from the group consisting of titanium nitride, a mixture of aluminum nitride and carbon and a mixture of silicon nitride and molybdenum silicide, other than silicon carbide.
  • the heating/cooling apparatus of the fifth embodiment of the present invention has been described above as having the two holes 41 and 42 for receiving samples. It is not however limited to this structure, but the holes may be of any shape in any number. It is also possible, as required, to provide the sintered body 40 with a heat-radiating plate having fins, a heat-radiating plate having a honeycomb structure, or at least one cooling through-hole, as a cooling means.
  • Fig. 16 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a sixth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, provided with at least one peephole.
  • 51 is a sintered body
  • 52 and 53 are holes for receiving samples
  • 54 is an electrode
  • 55 and 56 are peepholes for visually and optically observing samples in test tubes, for example
  • 57, 58 and 59 are cooling through-holes, as cooling means, through which a coolant passes.
  • Fig. 17 is a schematic sectional view of Fig. 16 cut along the line A-A'.
  • Fig. 17, 63 is a resistance-heating element.
  • the heating/cooling apparatus of the sixth embodiment of the present invention it is possible to observe, through the peepholes 55 and 56, the state of samples while appropriately controlling the temperature of the samples.
  • the peepholes 55 and 56 may be of any shape in any number. It is possible to form optical paths for observation by filling the peepholes 55 and 56 with any one of an optically permeable ceramics, an optically permeable glass and an optically permeable resin.
  • the heating/cooling apparatus of the sixth embodiment of the present invention there is used a combination of: (1) any one of the several kinds of the chemical composition of the sintered body, and (2) any one of the several kinds of the chemical composition of the resistance-heating element, as described above in relation to the above-mentioned first to fifth embodiments of the present invention.
  • the holes 52 and 53 for receiving samples may be of any shape in any number.
  • Fig. 18 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramic of a seventh embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
  • 60 is a sintered body made of a ceramics comprising aluminum nitride;
  • 61 is an electrode;
  • 62 are a plurality of cooling through-holes as cooling means, through which a coolant passes.
  • Fig. 19 is a schematic sectional view of Fig. 18 cut along the line A-A'.
  • 66 is a resistance-heating element comprising tungsten, connected to the electrode 61.
  • Fig. 20 is a schematic sectional view of Fig.
  • FIG. 18 cut along the line B-B', illustrating the heating/cooling apparatus of the seventh embodiment of the present invention shown in Fig. 18, which is attached with a sample receptacle 64.
  • Fig. 20 65 are a plurality of recesses for samples; and 62 is a cooling through-hole as a cooling means.
  • a performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned seventh embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention. Pure water identical with that in the performance test of the heating/cooling apparatus of the first embodiment of the present invention, was poured into each of the recesses for samples 65. Also in the performance test of the heating/cooling apparatus of the seventh embodiment of the present invention, there was employed the same temperature controlling method as that in the performance test of the heating/cooling apparatus of the first embodiment of the present invention.
  • control of temperature was effected on the basis of the temperatures of pure water measured by means of the thermocouple immersed into pure water received in each of the recesses for samples 65. Satisfactory results of the performance test were obtained in the performance test of the heating/cooling apparatus of the seventh embodiment of the present invention. An error between the temperature of pure water in each of the recesses for samples 65 and the target temperature was within ⁇ 1°C.
  • heating/cooling apparatus of the seventh embodiment of the present invention there is used a combination of: (1) any one of the several kinds of the chemical composition of the sintered body, (2) any one of the several kinds of the chemical composition of the resistance-heating element, and (3) any one of the several kinds of the cooling means, as described above in relation to the above-mentioned first to fifth embodiments of the present invention.
  • the heating/cooling apparatus made of a ceramics of the present invention it is possible to rapidly heat and cool various samples, to precisely control the temperature of the sample, to keep a uniform temperature distribution in the sample, and to conduct a precise temperature control in accordance with a predetermined complicated temperature program, which was impossible by any of the conventional technologies, thus providing useful effects in such fields as biotechnology, chemistry, medicine and bioengineering, and providing industrially useful effects.

Abstract

The invention aims at enabling various precise temperature control and programmed temperature management and control, which have been impossible by the prior art technology, thereby developing an epoch-making scientific technique and new uses and applications thereof in the field of biotechnology and the fields relating to chemistry, medicine and engineering. The device of the invention is made from a sinter with good heat conductivity, which sinter has holes or grooves for supporting an object on an arbitrary face thereof, a heat-generating resistor buried therein, and a cooling surface. This device has such a wide area of contact with the object as to permit efficient heat conduction from the device to the object. Therefore it is possible to effect rapid temperature rise and fall toward a predetermined temperature and secure a high accuracy of temperature distribution, thus realizing precise temperature control.

Description

    FIELD OF THE INVENTION
  • The present invention relates to a heating/cooling apparatus made of a ceramics, which permits a rapid heating and a rapid cooling of various samples in such fields as biotechnology, chemistry, medicine and bioengineering, and achievement of a precise temperature control of the sample and a uniform temperature distribution in the sample.
  • BACKGROUND OF THE INVENTION
  • Various types of heating/cooling apparatus have conventionally been employed in the above-mentioned fields for the purpose of rapidly and accurately heating and cooling various samples under a precise temperature control. In a heating/cooling apparatus of any of these types, a receptacle made of a metal such as aluminum or the like for receiving an object to be heated or cooled, i.e., a sample, and a heating means are configured as two separate components. This results in a poorer heat transfer coefficiency from the heating means to the receptacle for the sample, makes it difficult to rapidly heat the sample, and furthermore, leads to a non-uniform temperature distribution in the sample. It is therefore difficult to achieve a desired heating pattern. The available cooling means of the sample include, on the other hand, a spontaneous cooling, a forced cooling with the use of a coolant such as a gas or a liquid, and a combination thereof. It is however difficult to precisely control a cooling rate by such a cooling means alone. It is thus conceivable to control the cooling rate by using any of the above-mentioned cooling means while supplying a prescribed heat quantity from the heating means to the sample. In this manner of cooling, however, the heat supplied by the heating means cannot be efficiently transferred to the receptacle for the sample. It is therefore difficult to rapidly decrease the sample temperature to a desired temperature, and moreover, the temperature distribution in the sample is non-uniform, resulting in difficulty in achieving a desired cooling pattern.
  • An object of the present invention is therefore to provide a heating/cooling apparatus made of a ceramics, which solves the above-mentioned problems, and permits a rapid heating and a rapid cooling of various samples, allows a precise temperature control of the sample, thereby enabling a temperature control of the sample in accordance with a predetermined temperature pattern, and achieving a uniform temperature distribution in the sample.
  • DISCLOSURE OF THE INVENTION
  • In the heating/cooling apparatus made of a ceramics of the present invention, at least one of a face, at least one hole, at least one recess and at least one groove, the shape of which coincides with that of an object to be heated or cooled, i.e., a sample, for receiving the sample, to increase a contact area with the sample, is formed at an arbitrary position on a sintered body comprising an electrically insulating ceramics having a thermal conductivity of at least 10 W/(m · k)
    Figure imgb0001
    . An electrically conductive resistance-heating element comprising a metal, an electrically conductive ceramics or carbon is buried into the sintered body. In the heating/cooling apparatus made of a ceramics of the present invention, the whole of the above-mentioned sintered body may comprise an electrically conductive ceramics, thereby the sintered body itself forming a resistance-heating element as a heating means.
  • The heating/cooling apparatus made of a ceramics of the present invention further comprises a cooling means. The cooling means comprises a coolant feeder, provided outside the sintered body, for feeding a coolant such as a gas or a liquid to the sintered body, on the one hand, and at least one of part of a surface of the sintered body, a rugged portion formed on part of a surface of the sintered body, at least one cooling through-hole, through which the coolant passes, formed in the sintered body, a heat-radiating plate having fins, provided on the sintered body, and a heat-radiating plate having a honeycomb structure, provided on the sintered body, each for effecting a heat exchange, on the other hand. The heat-radiating plate comprises any one of a metal and a ceramics.
  • According to the heating/cooling apparatus made of a ceramics having the construction as described above, the sample is in contact with the face, at least one hole, at least one recess or at least one groove, each for receiving the sample, provided on the sintered body having a satisfactory thermal conductivity, so that the temperature of the sample rapidly becomes equal to the temperature of the sintered body, thus permitting a precise temperature control during the heating and the cooling of the sample.
  • BRIEF DESCRIPTION OF THE DRAWINGS
  • Fig. 1 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a first embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
  • Fig. 2 is a schematic sectional view of Fig. 1 cut along the line A-A'.
  • Fig. 3 is a schematic exploded perspective view illustrating a manufacturing process of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention shown in Fig. 1.
  • Fig. 4 is a schematic descriptive view illustrating a combination of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention shown in Fig. 1, and a coolant feeder.
  • Fig. 5 is a graph illustrating a predetermined temperature pattern in a performance test of a heating/cooling apparatus made of a ceramics.
  • Fig. 6 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a second embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
  • Fig. 7 is a schematic sectional view of Fig. 6 cut along the line A-A'.
  • Fig. 8 is a schematic perspective view illustrating two green blocks for the heating/cooling apparatus made of a ceramics of the second embodiment of the present invention shown in Fig. 6.
  • Fig. 9 is a schematic perspective view illustrating the state in which a resistance-heating element is attached onto one of the two green blocks shown in Fig. 8.
  • Fig. 10 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a third embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and a heat-radiating plate having fins, as a cooling means.
  • Fig. 11 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fourth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and at least one cooling through-hole as a cooling means, formed in the sintered body.
  • Fig. 12 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fifth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising silicon carbide.
  • Fig. 13 is a schematic perspective view illustrating a green block for the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention shown in Fig. 12.
  • Fig. 14 is a schematic perspective view illustrating a green block having holes formed therein for receiving objects to be heated or cooled, i.e., samples, for the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention shown in Fig. 12.
  • Fig. 15 is a schematic descriptive view illustrating a combination of the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention shown in Fig. 12, and a coolant feeder.
  • Fig. 16 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a sixth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, provided with at least one peephole.
  • Fig. 17 is a schematic sectional view of Fig. 16 cut along the line A-A'.
  • Fig. 18 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a seventh embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
  • Fig. 19 is a schematic sectional view of Fig. 18 cut along the line A-A'.
  • Fig. 20 is a schematic sectional view of Fig. 18 cut along the line B-B', illustrating the heating/cooling apparatus made of a ceramics of the seventh embodiment of the present invention shown in Fig. 18, which is attached with a sample receptacle.
  • DESCRIPTION OF THE PREFERRED EMBODIMENTS
  • Now, the heating/cooling apparatus made of a ceramics of the present invention is described further in detail with reference to the drawings.
  • Fig. 1 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a first embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and Fig. 2 is a schematic sectional view of Fig. 1 cut along the line A-A'. The heating/cooling apparatus made of a ceramics of the first embodiment of the present invention is manufactured as follows. As shown in Fig. 3, holes 2 and 3 for receiving samples are formed in each of green sheets 7, 8 and 10 made of a ceramics comprising aluminum nitride. With the use of a paste prepared by kneading at least one powdery raw material selected from the group consisting of tungsten, molybdenum and rhenium, a resistance-heating element 5 is formed on the surface of the green sheet 8 by a method such as a screen printing. Then, the green sheets 7, 8 and 10 are piled one upon another, and a sintered body 1 is formed by sintering these green sheets 7, 8 and 10 thus piled up. The sintered body 1 thus formed has a shape as shown in Fig. 1, and the side surfaces opposite to each other have electrodes 4 and 4', respectively, connected to the resistance-heating element 5.
  • Then, a performance test was carried out by using the heating/cooling apparatus made of a ceramics prepared as described above. Fig. 4 is a schematic descriptive view illustrating a combination of the above-mentioned heating/cooling apparatus of the first embodiment of the present invention, and a coolant feeder. When heating a sample, voltage was impressed on the electrodes 4 and 4'. When cooling the sample, a cooling gas was supplied to the heating/cooling apparatus by means of a blower 11 as a coolant feeder. Each of test tubes having a thermocouple received therein was inserted into each of the holes 2 and 3 to investigate the performance of the heating/cooling apparatus. Temperature of each test tube was subjected to a PID (abbreviation of proportional-plus-integral-plus-derivative) control on the basis of the temperature measured by the thermocouple, so that the temperature of the test tube coincide with a target temperature. Electric power of the resistance-heating element 5 was controlled with the use of a thyristor.
  • The performance test was carried out as follows. Two test tubes filled with objects to be heated or cooled, i.e., samples, were inserted respectively into the holes 2 and 3 for receiving samples of the heating/cooling apparatus, and the samples were heated or cooled with the use of the above-mentioned heating/cooling apparatus in accordance with a predetermined temperature pattern as shown in Fig. 5, thereby precisely controlling the temperature of the samples. More specifically, the test tubes each receiving 1.5 mℓ of pure water were inserted respectively into the holes 2 and 3, each having an inside diameter agreeing with the outside diameter of the test tubes, of the heating/cooling apparatus shown in Fig. 1. A thermocouple for measuring temperature was immersed into the middle of pure water received in each of the test tubes. Pure water in each of the two test tubes showed an initial temperature of 17 °C, as measured by the thermocouple.
  • Subsequently, a program regarding set temperatures and set periods for heating and cooling pure water, was input into a controller for controlling the operation of the heating/cooling apparatus. The above-mentioned program comprised, as shown in Fig. 5: increasing the temperature of pure water to 95°C (hereinafter referred to as the "first set temperature"), then keeping this temperature for ten minutes (hereinafter referred to as the "first set period"), then decreasing the temperature of pure water to 4°C (hereinafter referred to as the "second set temperature"), then keeping this temperature for 60 minutes (hereinafter referred to as the "second set period"), then increasing again the temperature of pure water to 25°C (hereinafter referred to as the "third set temperature"), then keeping this temperature for 20 minutes (hereinafter referred to as the "third set period" ), and then discontinuing the operation of the heating/cooling apparatus.
  • Then, the heating/cooling apparatus was operated under the control by means of the controller, and actual changes in temperature with time of pure water received in each of the two test tubes, were measured by the thermocouple. The results of measurement were as follows. Upon the lapse of eight seconds after the start of operation of the heating/cooling apparatus, the temperature of pure water in each of the test tubes increased to 95 °C which was the first set temperature. Thereafter, during ten minutes which were the first set period, the temperature of pure water in each of the test tubes was kept at a temperature of 95 ± 0.1°C. Then, upon the lapse of 20 seconds after the first set period, the temperature of pure water in each of the test tubes decreased to 4°C which was the second set temperature. Then, during 60 minutes which were the second set period, the temperature of pure water in each of the test tubes was kept at a temperature of 4 ± 0.1°C. Subsequently, upon the lapse of two seconds after the second set period, the temperature of pure water in each of the test tubes increased to 25°C which was the third set temperature. Then, during 20 minutes which were the third set period, the temperature of pure water in each of the test tubes was kept at a temperature of 25 ± 0.1°C, and thereafter, the operation of the heating/cooling apparatus was discontinued.
  • The sintered body 1 of the heating/cooling apparatus made of a ceramics of the above-mentioned first embodiment of the present invention, has been described above as comprising an electrically insulating ceramics comprising aluminum nitride. The sintered body 1 may however comprise an electrically insulating ceramics comprising at least one of silicon carbide, silicon nitride, aluminum oxide and beryllium oxide, other than aluminum nitride. The material for forming the resistance-heating element 5 is not limited to at least one metal selected from the group consisting of tungsten, molybdenum and rhenium, but may be carbon, and furthermore, may be at least one electrically conductive ceramics selected from the group consisting of silicon carbide, titanium nitride, molybdenum silicide, zirconium boride, tungsten carbide and tantalum carbide. In addition, in the heating/cooling apparatus made of the ceramics of the above-mentioned first embodiment of the present invention, the resistance-heating element 5 is buried in the form of a single layer into the sintered body 1. However, a resistance-heating element comprising a plurality of layers may be buried into the sintered body 1. In the heating/cooling apparatus of the above-mentioned first embodiment of the present invention, the holes 2 and 3 for receiving the samples may have any shape in any number.
  • Fig. 6 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a second embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and Fig. 7 is a schematic sectional view of Fig. 6 cut along the line A-A'. The heating-cooling apparatus made of a ceramics of the second embodiment of the present invention is manufactured as follows. A powdery raw material comprising aluminum nitride is charged into a metallic mold not shown to form two green blocks 21 and 22 as shown in Fig. 8. Then, resistance- heating elements 19 and 20 each comprising a coiled wire made of at least one metal selected from the group consisting of tungsten, molybdenum and rhenium, are arranged on the surface of the green block 22 as shown in Fig. 9. Then, the other green block 21 is placed upon the green block 22, and as shown in Figs. 6 and 7, holes 13, 14, 15 and 16 for receiving samples are formed by means of a cutting. Thereafter, the two green blocks thus provided with the holes are sintered by a hot press method, thereby preparing a sintered body 12 made of a ceramics comprising aluminum nitride having the resistance- heating elements 19 and 20 buried therein. Then, the side surfaces of the sintered body 12 are ground to expose ends of the coiled wires as the resistance- heating elements 19 and 20. Then, electrodes 17 and 18 are brazed onto the ends of the coiled wires thus exposed.
  • A performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned second embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of the ceramics of the first embodiment of the present invention. As in the performance test of the heating/cooling apparatus of the first embodiment of the present invention, a blower as a coolant feeder was arranged below the heating/cooling apparatus, thereby blowing a cooling gas toward the heating-cooling apparatus to cool same. The temperature of the sample was controlled also in the same manner as in the performance test of the heating/cooling apparatus of the first embodiment of the present invention. Also in the performance test of the heating/cooling apparatus of the second embodiment of the present invention, there were obtained excellent results of the performance test as in the heating/cooling apparatus of the first embodiment of the present invention. Furthermore, the heating/cooling apparatus of the second embodiment of the present invention was improved by providing a rugged portion or fins by means of a grinding on part of the surface of the sintered body 12, and the same performance test as described above was carried out for each of such improvements. There were obtained excellent results of the performance test as in the heating/cooling apparatus of the second embodiment of the present invention. Particularly within a range of temperature of from 100 to 600°C, there was available a cooling rate higher than that in the heating/cooling apparatus of the first embodiment of the present invention. In the heating/cooling apparatus of the second embodiment of the present invention, the holes 13, 14, 15 and 16 for receiving samples may be of any shape in any number, and the resistance- heating elements 19 and 20 may be in any number.
  • Fig. 10 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a third embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and a heat-radiating plate having fins, as a cooling means. The heating/cooling apparatus of the third embodiment of the present invention is configured by forming a metallic layer comprising at least one metal of copper, nickel, molybdenum and manganese on the lower surface of the heating/cooling apparatus of the above-mentioned second embodiment of the present invention, and then brazing a metallic heat-radiating plate 30 having fins, as a cooling means, onto the metallic layer. In Fig. 10, 23 is a sintered body; 24, 25, 26 and 27 are holes for receiving samples; and 28 and 29 are electrodes.
  • A performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned third embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention. Also in the performance test of the heating/cooling apparatus of the third embodiment of the present invention, there were obtained excellent results of the performance test as in the heating/cooling apparatus of the first embodiment of the present invention. Particularly within a range of temperature of from 100 to 600°C, there was available a cooling rate higher than that of the heating/cooling apparatus of the first embodiment of the present invention. In the heating/cooling apparatus of the third embodiment of the present invention, the metallic heat-radiating plate 30 having fins, as a cooling means, has been described as being provided on the lower surface of the sintered body 23. However, the above-mentioned heat-radiating plate 30 may be provided on a surface other than the lower surface of the sintered body 23, for example, on a side surface thereof. Furthermore, the above-mentioned heat-radiating plate 30 may have a honeycomb structure in place of the fins.
  • Fig. 11 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fourth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and at least one cooling through-hole as a cooling means, formed in the sintered body. The heating/cooling apparatus of the fourth embodiment of the present invention is configured by forming cooling through- holes 38 and 39 as cooling means, as shown in Fig. 11, by means of an ultrasonic working, a diamond grinding or the like, in the sintered body of the heating/cooling apparatus of the second embodiment of the present invention. In Fig. 11, 31 is a sintered body; 32, 33, 34 and 35 are holes for receiving samples; and 36 and 37 are electrodes. When cooling samples with the use of the heating/cooling apparatus of the fourth embodiment of the present invention, a cooling gas is supplied into the cooling through- holes 38 and 39.
  • A performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned fourth embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention. Also in the performance test of the heating/cooling apparatus of the fourth embodiment of the present invention, there were obtained excellent results of the performance test as in the heating/cooling apparatus of the first embodiment of the present invention. Particularly within a range of temperature of from 100 to 600 °C, there was available a cooling rate higher than that of the heating/cooling apparatus of the first embodiment of the present invention. In the performance test of the heating/cooling apparatus of the fourth embodiment of the present invention, a cooling gas has been described as being supplied into the cooling through- holes 38 and 39 as the cooling means. However, a liquid coolant may be supplied into the cooling through- holes 38 and 39. A partition having a honeycomb structure may be provided as required in each of the cooling through- holes 38 and 39.
  • Fig. 12 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fifth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising silicon carbide. In Fig. 12, 40 is a sintered body made of an electrically conductive ceramics comprising silicon carbide; and 41 and 42 are holes for receiving samples. The heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention is manufactured as follows. A powdery raw material comprising an electrically conductive ceramics comprising silicon carbide is charged into a metallic mold not shown to form a green block 45 as shown in Fig. 13. Then, as shown in Fig. 14, holes 41 and 42 for receiving samples are formed in the green block 45 by means of a cutting. Subsequently, the green block 45 thus provided with the holes 41 and 42 is sintered under the known sintering conditions. Then, metallic layers as electrodes 43 and 44 are attached, as shown in Fig. 12, onto the opposing side surfaces of the resultant sintered body 40, respectively. In the heating/cooling apparatus of the fifth embodiment of the present invention, the sintered body 40 itself forms a resistance-heating element serving as a heating means. There is no need therefore to specifically provide resistance-heating element in the sintered body 40.
  • A performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned fifth embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention. As in the performance test of the heating/cooling apparatus of the first embodiment of the present invention, a blower 50 as a coolant feeder was arranged, as shown in Fig. 15, below the heating/cooling apparatus, thereby blowing a cooling gas toward the heating/cooling apparatus to cooling same. Also in the performance test of the heating/cooling apparatus of the fifth embodiment of the present invention, there were obtained excellent results of the performance test as in the heating/cooling apparatus of the first embodiment of the present invention.
  • The sintered body 40 of the heating/cooling apparatus of the fifth embodiment of the present invention has been described above as comprising an electrically conductive ceramics comprising silicon carbide, but the sintered body 40 may comprise any one electrically conductive ceramics selected from the group consisting of titanium nitride, a mixture of aluminum nitride and carbon and a mixture of silicon nitride and molybdenum silicide, other than silicon carbide. The heating/cooling apparatus of the fifth embodiment of the present invention has been described above as having the two holes 41 and 42 for receiving samples. It is not however limited to this structure, but the holes may be of any shape in any number. It is also possible, as required, to provide the sintered body 40 with a heat-radiating plate having fins, a heat-radiating plate having a honeycomb structure, or at least one cooling through-hole, as a cooling means.
  • Fig. 16 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a sixth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, provided with at least one peephole. In Fig. 16, 51 is a sintered body; 52 and 53 are holes for receiving samples; 54 is an electrode; 55 and 56 are peepholes for visually and optically observing samples in test tubes, for example; and 57, 58 and 59 are cooling through-holes, as cooling means, through which a coolant passes. Fig. 17 is a schematic sectional view of Fig. 16 cut along the line A-A'. In Fig. 17, 63 is a resistance-heating element. According to the heating/cooling apparatus of the sixth embodiment of the present invention, it is possible to observe, through the peepholes 55 and 56, the state of samples while appropriately controlling the temperature of the samples. The peepholes 55 and 56 may be of any shape in any number. It is possible to form optical paths for observation by filling the peepholes 55 and 56 with any one of an optically permeable ceramics, an optically permeable glass and an optically permeable resin. In the heating/cooling apparatus of the sixth embodiment of the present invention, there is used a combination of: (1) any one of the several kinds of the chemical composition of the sintered body, and (2) any one of the several kinds of the chemical composition of the resistance-heating element, as described above in relation to the above-mentioned first to fifth embodiments of the present invention. The holes 52 and 53 for receiving samples may be of any shape in any number.
  • Fig. 18 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramic of a seventh embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride. In Fig. 18, 60 is a sintered body made of a ceramics comprising aluminum nitride; 61 is an electrode; and 62 are a plurality of cooling through-holes as cooling means, through which a coolant passes. Fig. 19 is a schematic sectional view of Fig. 18 cut along the line A-A'. In Fig. 19, 66 is a resistance-heating element comprising tungsten, connected to the electrode 61. Fig. 20 is a schematic sectional view of Fig. 18 cut along the line B-B', illustrating the heating/cooling apparatus of the seventh embodiment of the present invention shown in Fig. 18, which is attached with a sample receptacle 64. In Fig. 20, 65 are a plurality of recesses for samples; and 62 is a cooling through-hole as a cooling means.
  • A performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned seventh embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention. Pure water identical with that in the performance test of the heating/cooling apparatus of the first embodiment of the present invention, was poured into each of the recesses for samples 65. Also in the performance test of the heating/cooling apparatus of the seventh embodiment of the present invention, there was employed the same temperature controlling method as that in the performance test of the heating/cooling apparatus of the first embodiment of the present invention. More specifically, the control of temperature was effected on the basis of the temperatures of pure water measured by means of the thermocouple immersed into pure water received in each of the recesses for samples 65. Satisfactory results of the performance test were obtained in the performance test of the heating/cooling apparatus of the seventh embodiment of the present invention. An error between the temperature of pure water in each of the recesses for samples 65 and the target temperature was within ± 1°C. In the heating/cooling apparatus of the seventh embodiment of the present invention, there is used a combination of: (1) any one of the several kinds of the chemical composition of the sintered body, (2) any one of the several kinds of the chemical composition of the resistance-heating element, and (3) any one of the several kinds of the cooling means, as described above in relation to the above-mentioned first to fifth embodiments of the present invention.
  • INDUSTRIAL APPLICABILITY
  • According to the heating/cooling apparatus made of a ceramics of the present invention, as described above in detail, it is possible to rapidly heat and cool various samples, to precisely control the temperature of the sample, to keep a uniform temperature distribution in the sample, and to conduct a precise temperature control in accordance with a predetermined complicated temperature program, which was impossible by any of the conventional technologies, thus providing useful effects in such fields as biotechnology, chemistry, medicine and bioengineering, and providing industrially useful effects.

Claims (19)

  1. A heating/cooling apparatus made of a ceramics, which comprises:
       a sintered body having at least one of a face, at least one hole, at least one recess and at least one groove, each for receiving an object to be heated or cooled; and
       at least one resistance-heating element, as a heating means, provided in said sintered body.
  2. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       a cooling means is provided on a surface of, or in an interior of, said sintered body.
  3. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       said cooling means comprises a rugged portion formed on a surface of said sintered body, or part of a surface of said sintered body.
  4. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       said cooling means comprises a heat-radiating plate having fins, a heat-radiating plate having a honeycomb structure, or at least one cooling pipe, each provided on a surface of said sintered body.
  5. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       said cooling means comprises at least one cooling through-hole, at least one cooling pipe, or at least one cooling through-hole having a honeycomb structure, each provided in an interior of said sintered body.
  6. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       said sintered body has at least one peephole or at least one optical path for observation, each having a desired shape, for observing an object to be heated or cooled, at an arbitrary position of said sintered body.
  7. A heating/cooling apparatus made of a ceramics as claimed in Claim 6, wherein:
       said peephole or said optical path for observation comprises a through-hole.
  8. A heating/cooling apparatus made of a ceramics as claimed in Claim 6, wherein:
       said peephole or said optical path for observation is filled with an optically permeable ceramics.
  9. A heating/cooling apparatus made of a ceramics as claimed in Claim 6, wherein:
       said peephole or said optical path for observation is filled with an optically permeable glass.
  10. A heating/cooling apparatus made of a ceramics as claimed in Claim 6, wherein:
       said peephole or said optical path for observation is filled with an optically permeable resin.
  11. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       said sintered body has a thermal conductivity of at least 10 W/(m · k)
    Figure imgb0002
    .
  12. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       said sintered body comprises an electrically insulating ceramics.
  13. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       the whole of said sintered body comprises an electrically conductive ceramics, thereby said sintered body itself forming a resistance-heating element.
  14. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       said resistance-heating element comprises an electrically conductive inorganic material.
  15. A heating/cooling apparatus made of a ceramics as claimed in Claim 14, wherein:
       said resistance-heating element comprises a metal.
  16. A heating/cooling apparatus made of a ceramics as claimed in Claim 14, wherein:
       said resistance-heating element comprises an electrically conductive ceramics.
  17. A heating/cooling apparatus made of a ceramics as claimed in Claim 14, wherein:
       said resistance-heating element comprises carbon.
  18. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       said sintered body comprises a ceramics comprising aluminum nitride.
  19. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:
       said sintered body comprises a ceramics comprising silicon carbide.
EP93913596A 1992-07-01 1993-06-28 Ceramic heating/cooling device Expired - Lifetime EP0603411B1 (en)

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JP211937/92 1992-07-01
JP21193792 1992-07-01
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JP19155393A JPH0699085A (en) 1992-07-01 1993-06-23 Ceramic heater/cooler
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4409436A1 (en) * 1994-03-19 1995-09-21 Boehringer Mannheim Gmbh Process for processing nucleic acids
WO1997026993A1 (en) * 1996-01-25 1997-07-31 Bjs Company Ltd. Heating
WO1998039479A1 (en) * 1997-03-03 1998-09-11 Regents Of The University Of Minnesota Thermal cycling or temperature control device and method using alumina plate
WO1998047442A1 (en) * 1997-04-24 1998-10-29 Jouvin Jean Luc Hydrocolloid conditioning module
WO1998038487A3 (en) * 1997-02-28 1998-11-19 Cepheid Heat exchanging, optically interrogated chemical reaction assembly
WO1998058524A1 (en) * 1997-06-17 1998-12-23 Delta Theta Limited Heating elements
US6300149B1 (en) * 1996-08-06 2001-10-09 Cavendish Kinetics Limited Integrated circuit device manufacture
EP1191361A1 (en) * 2000-09-25 2002-03-27 Sumitomo Electric Industries, Ltd. Heater module for optical waveguide device
US7255833B2 (en) 2000-07-25 2007-08-14 Cepheid Apparatus and reaction vessel for controlling the temperature of a sample
US7462323B1 (en) 1999-12-21 2008-12-09 Cepheid Apparatus for performing heat-exchanging chemical reactions
CN105536903A (en) * 2015-12-24 2016-05-04 青岛顺昕电子科技有限公司 Method for extending application range of heating device
WO2016083301A1 (en) * 2014-11-24 2016-06-02 Ceramtec Gmbh Thermal management in the field of e-mobility

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6524532B1 (en) 1995-06-20 2003-02-25 The Regents Of The University Of California Microfabricated sleeve devices for chemical reactions
US6635492B2 (en) 1996-01-25 2003-10-21 Bjs Company Ltd. Heating specimen carriers
JPH10117765A (en) * 1996-10-18 1998-05-12 Ngk Insulators Ltd Specimen holder and its production
US5958349A (en) * 1997-02-28 1999-09-28 Cepheid Reaction vessel for heat-exchanging chemical processes
US6300124B1 (en) 1999-11-02 2001-10-09 Regents Of The University Of Minnesota Device and method to directly control the temperature of microscope slides
KR100416993B1 (en) * 2001-07-21 2004-02-05 삼성전자주식회사 Optical element integrated heat transferring device for plc

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60256375A (en) * 1984-05-31 1985-12-18 Shimadzu Corp Bioreactor
JPS6418974A (en) * 1987-07-13 1989-01-23 Ibiden Co Ltd Production of heat-exchanger made of sintered silicon carbide
JPH0193472A (en) * 1987-09-30 1989-04-12 Toshiba Corp Heat-exchanger
US4865986A (en) * 1988-10-06 1989-09-12 Coy Corporation Temperature control apparatus
US4950608A (en) * 1989-04-25 1990-08-21 Scinics Co., Ltd. Temperature regulating container
EP0400965A2 (en) * 1989-05-30 1990-12-05 Takara Shuzo Co. Ltd. Reagent reactor

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60256375A (en) * 1984-05-31 1985-12-18 Shimadzu Corp Bioreactor
JPS6418974A (en) * 1987-07-13 1989-01-23 Ibiden Co Ltd Production of heat-exchanger made of sintered silicon carbide
JPH0193472A (en) * 1987-09-30 1989-04-12 Toshiba Corp Heat-exchanger
US4865986A (en) * 1988-10-06 1989-09-12 Coy Corporation Temperature control apparatus
US4950608A (en) * 1989-04-25 1990-08-21 Scinics Co., Ltd. Temperature regulating container
EP0400965A2 (en) * 1989-05-30 1990-12-05 Takara Shuzo Co. Ltd. Reagent reactor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of WO9401529A1 *

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4409436A1 (en) * 1994-03-19 1995-09-21 Boehringer Mannheim Gmbh Process for processing nucleic acids
WO1997026993A1 (en) * 1996-01-25 1997-07-31 Bjs Company Ltd. Heating
US6300149B1 (en) * 1996-08-06 2001-10-09 Cavendish Kinetics Limited Integrated circuit device manufacture
US8029733B2 (en) 1997-02-28 2011-10-04 Cepheid Thermal cycler with optical detector
WO1998038487A3 (en) * 1997-02-28 1998-11-19 Cepheid Heat exchanging, optically interrogated chemical reaction assembly
US9316590B2 (en) 1997-02-28 2016-04-19 Cepheid Apparatus for controlling and monitoring reactions
WO1998039479A1 (en) * 1997-03-03 1998-09-11 Regents Of The University Of Minnesota Thermal cycling or temperature control device and method using alumina plate
WO1998047442A1 (en) * 1997-04-24 1998-10-29 Jouvin Jean Luc Hydrocolloid conditioning module
FR2762505A1 (en) * 1997-04-24 1998-10-30 Jean Luc Jouvin HYDROCOLLOID CONDITIONER MODULE FOR TAKING DENTAL IMPRESSIONS
WO1998058524A1 (en) * 1997-06-17 1998-12-23 Delta Theta Limited Heating elements
US8293064B2 (en) 1998-03-02 2012-10-23 Cepheid Method for fabricating a reaction vessel
US7462323B1 (en) 1999-12-21 2008-12-09 Cepheid Apparatus for performing heat-exchanging chemical reactions
US7255833B2 (en) 2000-07-25 2007-08-14 Cepheid Apparatus and reaction vessel for controlling the temperature of a sample
EP1191361A1 (en) * 2000-09-25 2002-03-27 Sumitomo Electric Industries, Ltd. Heater module for optical waveguide device
WO2016083301A1 (en) * 2014-11-24 2016-06-02 Ceramtec Gmbh Thermal management in the field of e-mobility
JP2018503217A (en) * 2014-11-24 2018-02-01 セラムテック ゲゼルシャフト ミット ベシュレンクテル ハフツングCeramTec GmbH Thermal management in the field of e-mobility
CN105536903A (en) * 2015-12-24 2016-05-04 青岛顺昕电子科技有限公司 Method for extending application range of heating device

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DE69320449T2 (en) 1999-02-18
CA2115360A1 (en) 1994-01-20
WO1994001529A1 (en) 1994-01-20
EP0603411B1 (en) 1998-08-19
DE69320449D1 (en) 1998-09-24
KR100346861B1 (en) 2003-01-08

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