CN100500951C - Device and method for high-speed growth of diamond single-crystal - Google Patents
Device and method for high-speed growth of diamond single-crystal Download PDFInfo
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- CN100500951C CN100500951C CNB2007100553264A CN200710055326A CN100500951C CN 100500951 C CN100500951 C CN 100500951C CN B2007100553264 A CNB2007100553264 A CN B2007100553264A CN 200710055326 A CN200710055326 A CN 200710055326A CN 100500951 C CN100500951 C CN 100500951C
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Abstract
The inventive apparutus and method for growing diamond monocrystal at high-speed belongas to the technical field of diamond materials. The said apparatus is provided with sample tray 5 on the substrate holder in the settling chamber of chemical vaporous depositon system; sample tray 5 being provided with close annular frame 2 on the multi-crystal diamond film. It can also be provided with diamond powder 3 in the cavern in the close annular frame 2. The inventive method is that, monocrystal diamond crystallon 4 is placed into the settling chamber through the cavern in the close annular frame 2 and is etched in advance by plasma in situ; then diamond monocrystal is grown in the atmosphere of methane, hydrogen and nitrogen. The method includes that possible non-diamond phase and structural cavern are determined to be treated by observing brightness variation of growth face. The inventive apparatus is simple and easy to machine; and it does not bring any pollution for growing monocrystal diamond and has good thermal conduction. Transparent diamond monocrystal can be produced by the inventive method, and the growing speed can be more than 100 mm/hour.
Description
Technical field
The invention belongs to diamond single crystal material and preparing technical field thereof, relate to the apparatus and method of plasma activated chemical vapour deposition method two-forty rapid growth of diamond single-crystal.
Background technology
Early 1980s, adopt the chemical vapor deposition (CVD) method, in heterogeneous substrate, grow polycrystalline diamond films.But this method is developed rapidly because of characteristics such as the low depositing large-area polycrystalline diamond of its cost films, and ripe technically.But, can't satisfy the requirement of diamond at aspects such as electron devices owing to have a large amount of crystal boundaries and defective in the polycrystalline film; And the growth velocity of iso-epitaxy method rapid growth of diamond single-crystal is slower, be generally less than the 5-10 micron/hour, growth thickness is that millimetre-sized diamond single crystal film needed more than continuous growth 100-200 hour, stability requirement to growing system is very high, rolled up cost, distance satisfies diamond fully still has very big distance in the requirement of the extensive popularization of aspects such as electron device application.2002, Washington, DC Ka Neiji institute developed the high-speed rapid growth method of isoepitaxial growth single-crystal diamond, and growth velocity can obtain 10 carats diamond single crystal up to 50-150 μ m/h.Be different from the method for common High Temperature High Pressure diamond synthesis monocrystalline, the CVD method is produced diamond single crystal, advantage such as have that equipment is simple, easy to operate, good reproducibility, crystalline growth size are unrestricted.Just becoming the most promising method low-cost, large-particle monocrystal diamond of producing from this as can be seen method of long-range development trend.
Immediate with the present invention is the patent of invention (application number 02826062.7) of Carnegie Inst of Washington, and the anchor clamps and the temperature survey of this patent of invention lay special stress on seed crystal need be carried out key technological transformation to equipment, and cost is higher.
Summary of the invention
The technical problem to be solved in the present invention is, designs a kind of apparatus and method of new high-speed rapid growth of diamond single-crystal, and it is simple to have method, fast growth, and cost is low, pollutes advantages such as little, to satisfy and the application of aspects such as exploitation electronics, machinery.
The device of high-speed rapid growth of diamond single-crystal of the present invention is a plasma chemical vapor deposition system, it is characterized in that, the sample holder is housed on the substrate holder in the apparatus for plasma chemical vapor deposition sediment chamber; Said sample holder is that closed ring frame is housed on polycrystalline diamond films.
Also can place diadust in the hole in ring frame.The granularity of diadust can be that micron order is or/and nano level.
Ring frame can be the polycrystalline diamond mould material.Hole in sample holder and the ring frame can be made circular or square, or according to the shape and size Design and Machining of seed crystal.
During use, the sample holder is placed on the substrate holder in the plasma chemical vapor deposition system sediment chamber, and the hole in the ring frame is used to place seed crystal; Perhaps below seed crystal, fill diadust with the gap of seed crystal and sample holder.
Polycrystalline diamond films plays the effect of supporting ring frame, diadust and seed crystal.Polycrystalline diamond films will more help modulating diamond single crystal growth temperature and the diamond or the original substrate holder of carbon material contaminated system that prevent to generate in the process of growth, and the diamond single crystal of growth is polluted in the use of other non-diamond materials in process of growth.This patent is not limited to use bortz powder, also comprises the powder that other high temperature resistant chemical stabilities are good, as molybdenum powder.
Sample holder of the present invention also can only be used closed ring frame, this sample is propped up place on the original molybdenum system substrate holder of reactive system, fills diadust in the hole of ring frame.
Sample holder of the present invention possesses following advantage: simple in structure being suitable for; Use laser cutting CVD polycrystalline diamond films, be easy to processing; The seed crystal of applicable different shape is grown; The growing single-crystal diamond is not produced any pollution; Heat conduction is good; Be easy to adjust the temperature of sample in the process of growth; Be easy to control and modulate in the reaction cavity and the plasma density of sample surfaces.
The method of high-speed rapid growth of diamond single-crystal of the present invention is:
The using plasma chemical gas-phase deposition system, in sample holder of the present invention, can directly put the single-crystal diamond seed crystal after mechanical polishing, acetone supersound process, perhaps below seed crystal and the gap of seed crystal and sample holder filling diadust, to increase contacting of seed crystal and sample holder better.Sample holder and seed crystal are placed in the plasma chemical vapor deposition system sediment chamber.
Single crystal growth process is, in the sediment chamber seed crystal carried out hydrogen plasma on the throne or hydrogen/nitrogen plasma etching in advance.Then in base reservoir temperature 900---rapid growth of diamond single-crystal in 1300 ℃ of scopes, under 13kPa-20kPa air pressure, in methane, hydrogen and nitrogen atmosphere.
Take out sample holder and sample at last, boiling in the vitriol oil and concentrated nitric acid, holder separates with sample to make sample.Said seed crystal can be the diamond single crystal of high temperature and high pressure method growth, also can be that the CVD single-crystal diamond is as seed crystal.Seed size can be equal to or greater than 1 * 1 millimeter
2(100) face of the most handy seed crystal is as aufwuchsplate.
Below seed crystal and the gap of seed crystal and sample holder fill diadust, can strengthen contacting of seed crystal and sample holder, promotion heat conduction is even.When filling diadust, also can in the diadust of inserting, splash into alcohol again, under the not dried state of alcohol, seed crystal is inserted wherein, can strengthen contacting of seed crystal and bortz powder like this.
Said storing seed crystal, (100) aufwuchsplate of seed crystal is slightly high more fair or lower slightly than sample holder upper surface.Difference of altitude can change the single crystal growing temperature on the seed crystal, can have influence on the growth velocity or the quality of diamond single crystal early growth period.
Also can change the single crystal growing temperature by the air pressure of change sediment chamber or the power of plasma body.
In the rapid growth of diamond single-crystal process, when etching in advance, gas in the sediment chamber and throughput ratio are hydrogen: nitrogen=500:0-3; When diamond single crystal was grown, gas in the sediment chamber and throughput ratio were hydrogen: methane: nitrogen=500:50-70:1-3.
In acid cooking, the vitriol oil by volume: concentrated nitric acid=1-2:2-1.
In the method for the present invention, can also among the rapid growth of diamond single-crystal process, carry out the repetitive process of plasma etching treatment and rapid growth of diamond single-crystal, to keep single crystal growing better.The multiplicity of the repetitive process of plasma etching treatment and rapid growth of diamond single-crystal can be 1-5 times.Wherein the growth conditions of rapid growth of diamond single-crystal remains in 900-1300 ℃ of scopes of base reservoir temperature, under 13kPa-20kPa air pressure, and rapid growth of diamond single-crystal in methane, hydrogen and nitrogen atmosphere.Each plasma etching treatment can be at 2-3 hours, and the time of each diamond single crystal growth can be at 4-8 hours.
Sample can be taken out observation from the sediment chamber in the middle of the repetitive process of hydrogen plasma etching processing and rapid growth of diamond single-crystal; Can not take out yet,, or feed methane and nitrogen off and on by the time as long as feed methane gas off and on by the time.
The present invention also provides a kind of method that judges whether to be fit to continued growth.By there being bright spot to occur on the direct viewing single crystal growing face in process of growth, be exactly the brightness of this place's brightness above other positions, this place just has graphite to reach other non-diamonds mutually to occur mutually.The projecting temperature of explanation bright spot place's local temperature appears in bright spot in the process of growth, causes single crystal growing disturbance to occur, is unfavorable for growing complete smooth monocrystalline.Localized hyperthermia may be that its growth velocity is accelerated, and protrudes in single crystal growing face owing to there is graphite to equate that non-diamond takes place mutually, and plasma body is attracted, and causes this place's plasma density to increase.Require this moment to stop growing.
The method that processing graphite reaches other non-diamond phases mutually is: sample and sample holder are taken out, separate with boiling in the concentrated nitric acid at the vitriol oil, remove graphite and reach other non-diamond phases mutually, obtain smooth single crystal growing face by mechanical polishing again; Single-crystal diamond is reloaded in the sample holder process of continued growth diamond single crystal.
Occur mutually if having only a spot of graphite to reach other non-diamonds mutually, also can not take out sample, original position is carried out hydrogen plasma or hydrogen/nitrogen plasma etching, removes graphite and reaches other non-diamond phases, the process of continued growth diamond single crystal afterwards mutually.
The said seed crystal of the present invention can be the diamond single crystal that high-quality high temperature and high pressure method is grown, and does not contain or contain the impurity and the wrap of minute quantity; Also can be to contain part or a spot of impurity and wrap, but the aufwuchsplate of this seed crystal need polished finish, obtains smooth (100) face, again according to method rapid growth of diamond single-crystal of the present invention.
Impurity in the seed crystal and wrap may cause hole, appearance hole in the process of growth, treatment process: sample is taken out from the sediment chamber, remove with the method for mechanical polishing, carry out hydrogen plasma or hydrogen/nitrogen plasma etching, continued growth then again; Perhaps,, continue growth in situ, fill and lead up through the transversal epitaxial growth process and cheat the hole, obtain complete smooth (100) diamond single crystal through the regular hour when cheating hole size hour (tens arrive about the hundreds of micron).
Method of the present invention can obtain transparent diamond single crystal.(100) aufwuchsplate of seed crystal can be or atypical facing all to grow (100) diamond single crystal on seed crystal.The diamond single crystal speed of growth greater than the 20-100 micron/hour, but more than the thickness 2-4 millimeter.
Description of drawings
Fig. 1 is a kind of sample holder structure front view of the present invention.
Fig. 2 is the side-view of the sample holder structure of Fig. 1.
Embodiment
Implementing example below is to further specify of the present invention, rather than limits the scope of the invention.
Embodiment 1
The device of accompanying drawings high-speed rapid growth of diamond single-crystal of the present invention---the structure of sample holder.Among Fig. 1 and Fig. 2,1 is polycrystalline diamond films, and 2 is ring frame, and polycrystalline diamond films 1 and ring frame 2 constitute sample holder 5.Be that sample holder 5 is that closed ring frame 2 is housed on polycrystalline diamond films 1.3 are diadust (granularity is that micron order is or/and nano level), and 4 is seed crystal.
During use, diamond seed 4 can be placed in the hole in the ring frame 2, directly carry out the growth of diamond single crystal.Also diadust 3 can be placed in the hole in the ring frame 2 of sample holder 5, seed crystal 4 is placed in the hole of ring frame 2, and makes the below of seed crystal 4 and seed crystal 4 and the gap location of ring frame 2 be filled with diadust 3.
Also can substitute diadust 3 in the present embodiment with molybdenum powder.
Embodiment 2
ASTex 5250 type 5kw (2.45GHz) the microwave plasma CVD equipment of Seki company are adopted in experiment, adopt High Temperature High Pressure Ib type monocrystalline (100) diamond as seed crystal, thereon iso-epitaxy high-speed rapid growth single-crystal diamond.Handle through mechanical polishing on (100) two sides about the diamond seed, and ultrasonic cleaning in acetone then is placed in the polycrystalline diamond sample holder of particular design (referring to Fig. 1) at last, and sample is put into the sediment chamber.Earlier pressure in the sediment chamber is evacuated to below the 0.1Pa.Gases used in the experiment is high-purity methane (4N), hydrogen (5N) and nitrogen (5N).Experiment is divided into etching and two stages of growth.In etch stages, only feed hydrogen and nitrogen, flow is respectively 500sccm and 1.8sccm, under the condition of pressure 17kPa, microwave power 2.5kw to the aufwuchsplate etching of diamond substrate 3 hours.Keep other condition constant then, feed the methane of 60sccm, the process of beginning isoepitaxial growth single-crystal diamond.The seed temperature that measures etching and growth phase by optical pyrometer (Shanghai self-service instrument three WGG2-201 of factory types) is respectively 950 ℃ and 1000 ℃.Process of growth continues to repeat etching process once more after 6 hours, hydrogen/nitrogen etching 2 hours, and then feeds methane continued growth 6 hours.The High Temperature High Pressure diamond seed (Ib) of thickness 1.0mm can increase thickness and reach 1.23mm through 12 hours process of growth, and the speed of growth is about 100 microns/hour.
After this can also repeat etching process and single crystal growth process.
The described single crystal diamond film method of present embodiment is to carry out in the sediment chamber of microwave plasma CVD system (MWPCVD), but be not limited to the microwave plasma CVD method, in other adamantine systems of possibility growing single-crystal, as hot filament CVD, DC arc plasma is sprayed CVD, and systems such as hot-cathode direct-current plasma CVD are suitable equally.
Claims (10)
1, a kind of device of high-speed rapid growth of diamond single-crystal is a plasma chemical vapor deposition system, it is characterized in that, sample holder (5) is housed on the substrate holder in the plasma chemical vapor deposition system sediment chamber; Said sample holder (5) is that closed ring frame (2) is housed on polycrystalline diamond films (1).
2, according to the device of the high-speed rapid growth of diamond single-crystal of claim 1, it is characterized in that, place diadust (3) in the hole in ring frame (2); The granularity of said diadust (3) is that micron order is or/and nano level.
3, a kind of method of using the device high-speed rapid growth of diamond single-crystal of claim 1, the using plasma chemical gas-phase deposition system, it is characterized in that, in sample holder (5), directly put through mechanical polishing, single-crystal diamond seed crystal (4) after the acetone supersound process, perhaps fill diadust (3) in the below of seed crystal (4) and the gap of seed crystal and sample holder (5), sample holder (5) and seed crystal (4) are placed in the plasma chemical vapor deposition system sediment chamber, and said sample holder (5) is that closed ring frame (2) is housed on polycrystalline diamond films (1); Single crystal growth process is in the sediment chamber seed crystal to be carried out hydrogen plasma or hydrogen and nitrogen plasma etching in advance; Then in 900-1300 ℃ of scopes of base reservoir temperature, under 13kPa-20kPa air pressure, in methane, hydrogen and nitrogen atmosphere rapid growth of diamond single-crystal; Take out sample holder (5) and sample at last, boiling in the vitriol oil and concentrated nitric acid, holder separates with sample to make sample.
According to the method for the described high-speed rapid growth of diamond single-crystal of claim 3, it is characterized in that 4, said seed crystal (4) is the diamond single crystal or the CVD single-crystal diamond of high temperature and high pressure method growth; In the rapid growth of diamond single-crystal process, when etching in advance, gas in the sediment chamber and throughput ratio are hydrogen: nitrogen=500:0-3; When diamond single crystal was grown, gas in the sediment chamber and throughput ratio were hydrogen: methane: nitrogen=500:50-70:1-3.
According to the method for claim 3 or 4 described high-speed rapid growth of diamond single-crystal, it is characterized in that 5, said filling diadust (3) splashes into alcohol again in the diadust of inserting (3), under the not dried state of alcohol, seed crystal (4) is inserted wherein.
6, according to the method for claim 3 or 4 described high-speed rapid growth of diamond single-crystal, it is characterized in that, among the rapid growth of diamond single-crystal process, carry out the repetitive process of plasma etching treatment and rapid growth of diamond single-crystal; Multiplicity is 1-5 times; Each plasma etching treatment was at 2-3 hours, and the time of each diamond single crystal growth was at 4-8 hours.
7, according to the method for claim 3 or 4 described high-speed rapid growth of diamond single-crystal, it is characterized in that having bright spot to occur on the seed crystal, judge that having graphite to reach other non-diamonds mutually occurs mutually by observing; The method that processing graphite reaches other non-diamond phases mutually is: sample and sample holder are taken out, separate with boiling in the concentrated nitric acid at the vitriol oil, remove graphite and reach other non-diamond phases mutually, obtain smooth single crystal growing face by mechanical polishing again; Single-crystal diamond is reloaded in the sample holder process of continued growth diamond single crystal; Or original position carries out hydrogen plasma or hydrogen and nitrogen plasma etching, removes graphite and reaches other non-diamond phases, the process of continued growth diamond single crystal afterwards mutually.
8, according to the method for the described high-speed rapid growth of diamond single-crystal of claim 6, it is characterized in that having bright spot to occur on the seed crystal, judge that having graphite to reach other non-diamonds mutually occurs mutually by observing; The method that processing graphite reaches other non-diamond phases mutually is: sample and sample holder are taken out, separate with boiling in the concentrated nitric acid at the vitriol oil, remove graphite and reach other non-diamond phases mutually, obtain smooth single crystal growing face by mechanical polishing again; Single-crystal diamond is reloaded in the sample holder process of continued growth diamond single crystal; Or original position carries out hydrogen plasma or hydrogen and nitrogen plasma etching, removes graphite and reaches other non-diamond phases, the process of continued growth diamond single crystal afterwards mutually.
9, according to the method for claim 3 or 4 described high-speed rapid growth of diamond single-crystal, it is characterized in that, impurity in the seed crystal and wrap cause the treatment process that occurs the hole, hole in the process of growth: sample is taken out from the sediment chamber, method with mechanical polishing is removed, carry out hydrogen plasma or hydrogen and nitrogen plasma etching, continued growth then again; Perhaps, continue growth in situ, fill and lead up the hole, hole through the transversal epitaxial growth process.
10, according to the method for the described high-speed rapid growth of diamond single-crystal of claim 6, it is characterized in that, impurity in the seed crystal and wrap cause the treatment process that occurs the hole, hole in the process of growth: sample is taken out from the sediment chamber, method with mechanical polishing is removed, carry out hydrogen plasma or hydrogen and nitrogen plasma etching, continued growth then again; Perhaps, continue growth in situ, fill and lead up the hole, hole through the transversal epitaxial growth process.
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