CN104599993A - Method for detecting quality of silicon substrate - Google Patents
Method for detecting quality of silicon substrate Download PDFInfo
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- CN104599993A CN104599993A CN201410856256.2A CN201410856256A CN104599993A CN 104599993 A CN104599993 A CN 104599993A CN 201410856256 A CN201410856256 A CN 201410856256A CN 104599993 A CN104599993 A CN 104599993A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/30—Structural arrangements specially adapted for testing or measuring during manufacture or treatment, or specially adapted for reliability measurements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/30—Structural arrangements specially adapted for testing or measuring during manufacture or treatment, or specially adapted for reliability measurements
- H01L22/34—Circuits for electrically characterising or monitoring manufacturing processes, e. g. whole test die, wafers filled with test structures, on-board-devices incorporated on each die, process control monitors or pad structures thereof, devices in scribe line
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Abstract
The invention provides a method for detecting quality of a silicon substrate. The method comprises the steps: firstly, the silicon substrate is heated and cooled; secondly, when the damaged layer of the back of the substrate has poor gettering effect or the supplied material of the silicon substrate is stained, dirt on the back and the edges of the silicon substrate or dirt in heating and cooling equipment overflows and transfers to the front side of the substrate; an epitaxial layer is developed on the silicon substrate, so that the integrity of the epitaxial growth lattices at the stained position of the silicon substrate is damaged, resulting in epitaxial growth defects; when the epitaxial layer on the silicon substrate is corroded, the epitaxial growth defects are exposed; the quality of the silicon substrate is judged by detecting the defects on the surface of the epitaxial layer by means of a metallographic microscope; the stained situation of the silicon substrate can be detected in advance without additionally arranging expensive detection equipment when the silicon substrate is supplied; therefore, the batch scrapping of the pipelining chips of sensitive devices is avoided and the delay of order delivery is prevented.
Description
Technical field
The present invention relates to semiconductor fabrication techniques field, particularly relate to a kind of method checking silicon substrate quality.
Background technology
In the single crystal preparation process of silicon substrate, the grinding process such as cylindrical barreling, locating surface grinding, section are the important sources that metal impurities stain, the metal ions such as sodium, magnesium, calcium, iron may be brought in grinding process, it can be ensconced the damage layer of grinding generation and stain in layer, contamination source is brought to later process, as it can not effectively remove by single track or rear road, silicon substrate metal quality will be had a strong impact on.
The machining damage layer that silicon substrate produces in grinding process and contamination layer, generally tentatively removed by chemical corrosion.Chemical Corrosion for Silicon Wafer liquid is divided into acid and alkalescence two kinds usually.Because alkaline corrosion liquid has the advantages such as cost is low, corrosion process controls easily, environmental protection treatment is relatively easy, thus silicon substrate supplier is more prone to use alkaline corrosion liquid.But the purity of alkaline corrosion liquid is poor, the technique of caustic corrosion is simultaneously the endothermic reaction, and processing temperature is high, and while removal machining damage layer, easily introduce metal contamination, compared with acid corrosion, its surface metal stains a concentration generally high order of magnitude.In addition, after silicon substrate completes chemical corrosion, need to carry out retrofit by CMP (Chemical Mechanical Polishing) process effects on surface, the polishing fluid that CMP (Chemical Mechanical Polishing) process is commonly used contains alkali and other metal ingredient, this also can bring metal contamination, if effectively can not remove the quality that these metal contaminations will certainly affect silicon substrate.
Industry generally improves silicon substrate metal contamination problem by back side gettering process.Back side gettering process comprises Intrinsic gettering and extrinsic absorption two class.Intrinsic gettering refers to that the oxygen precipitation by producing in wafer bulk induces dislocation or other lattice defect, and then the impurity absorbed on silicon chip or defect.Extrinsic absorption refers to sets up stress or back side damage (back of the body damage layer) at silicon chip back side, and then the impurity absorbed on silicon chip or defect.Stress by deposition film material as silicon nitride or polysilicon produce.Back side damage is introduced by the method for machinery, as sandblasting, scrub, Ar+ion implantation etc.The back side of silicon substrate is damaged the part metals produced in the adsorbable silicon substrate course of processing and is stain, impurity contamination in epitaxial process also on adsorbable epitaxial system and epitaxial furnace pedestal, the impurity contamination of adsorbable boiler tube and quartz boat in first step oxidizing annealing process.Consider cost and control complexity, current domestic vendors generally uses blasting craft to set up damage at silicon chip back side, and it can bring stable back side damage effect, but brings metal contamination as controlled bad meeting.Also there is part supplier to adopt and scrub technique in silicon chip back side foundation damage, but it is very high to process control needs, as controlled the bad back side damage effect often bringing instability, cause in the technical processs such as subsequent epitaxial, oxidation, annealing, the damage of silicon chip back side effectively can not absorb the contamination of front side of silicon wafer, has a strong impact on device quality.If the back of the body damages layer damage effect own effectively can not absorb impurity on silicon chip or defect not, or adsorbs the contamination brought in the too much substrate course of processing, all can bring hidden danger to device fabrication, as do not found ahead of time, will cause batch to be scrapped and order loses.
At present, silicon substrate producer generally uses total Reflection X-ray Fluorescence Spectrometry (Total X-rayFluorescence, TXRF) elemental analyser to carry out metal ion (metal contamination) in test silicon substrate, but it can only reach 1.0E
10the precision of atoms/cm2, this just occurs that TXRF elemental analyser detection display does not have metal ion to exceed standard, but the actual situation having metal contamination to exist.Although for common product and technique, 1.0 ~ 5.0E
10the metal contamination impact of atoms/cm2 is little, but for the device of sensitivity or processing procedure, then can cause the problems such as extension microdefect, MOS short channel leakage are large, the superfine potential barrier pin hole of Xiao, the yield of serious harm device and reliability.
Summary of the invention
The object of this invention is to provide a kind of method checking silicon substrate quality, to detect contamination in silicon substrate ahead of time when silicon substrate supplied materials.
In order to solve the problem, the invention provides a kind of method detecting silicon substrate quality, comprising:
Silicon substrate is heated up and process of lowering the temperature;
At described silicon substrate growing epitaxial layers; And
Described epitaxial loayer is corroded, and adopts metallomicroscope to carry out surface defects detection to described silicon substrate, judged the quality of described silicon substrate by the quantity of blemish.
Further, epitaxial furnace is adopted to heat up to described silicon substrate and process of lowering the temperature.Further, described epitaxial furnace is the epitaxial furnace adopting RF heating.
Further, carry out, in hyperthermic treatment process, in 10-24 minute, silicon substrate temperature being risen to more than 1100 DEG C to silicon substrate.Further, described hyperthermic treatment process specifically comprises: in hydrogen atmosphere, in 6-15 minute, silicon substrate temperature is risen to 850-900 DEG C from 100 DEG C; And in hydrogen atmosphere, in 4-9 minute, silicon substrate temperature is risen to more than 1100 DEG C from 850-900 DEG C.
Further, carry out, in cooling processing procedure, in 18-35 minute, silicon substrate temperature being down to less than 150 DEG C to silicon substrate.Further, described cooling processing procedure specifically comprises: in hydrogen atmosphere, in 6-10 minute, silicon substrate temperature is down to 700-850 DEG C; And close hydrogen inflated with nitrogen, in 12-25 minute, silicon substrate temperature is down to 100 DEG C.
Further, before described hyperthermic treatment, also comprise: import in epitaxial furnace by the epitaxial furnace pedestal being placed with silicon substrate, the air in extension cavity is driven out of by inflated with nitrogen; And the temperature keeping extension cavity original, fill hydrogen and the nitrogen in extension cavity is driven out of.
Further, epitaxial furnace is adopted to heat up to silicon substrate and process of lowering the temperature.Further, described epitaxial furnace is the epitaxial furnace adopting RF heating.
Further, chromic acid is adopted to corrode described epitaxial loayer.
The invention provides a kind of method checking silicon substrate quality, first silicon substrate is heated up and process of lowering the temperature, when there is contamination in substrate back damage layer gettering poor effect or silicon substrate supplied materials, contamination in the contamination at the silicon substrate back side and edge or heating and cooling equipment can be overflowed and be transferred to substrate face, grown epitaxial layer on a silicon substrate again, the position epitaxial growth perfection of lattice such silicon substrate existing contamination will be damaged and produce epitaxial growth defect, when corroding the epitaxial loayer on silicon substrate, epitaxial growth defect will be exposed, metallomicroscope is adopted to carry out the quality that epi-layer surface defects detection just can judge silicon substrate, do not need to increase expensive checkout equipment, the situation of the metal contamination detected in silicon substrate can be done sth. in advance when silicon substrate supplied materials, responsive device flow batch is avoided to scrap, prevention order is paid and is postponed.
Accompanying drawing explanation
With reference to accompanying drawing, according to detailed description below, clearly the present invention can be understood.For the sake of clarity, in figure, the relative thickness of each layer and the relative size of given zone are not drawn in proportion.In the accompanying drawings:
Fig. 1 is the schematic flow sheet of the method detecting silicon substrate quality in one embodiment of the invention;
Fig. 2 is the defect distribution schematic diagram in one embodiment of the invention on silicon substrate;
Fig. 3 is the defect pattern schematic diagram in one embodiment of the invention on silicon substrate.
Embodiment
Present inventor finds, various metal contamination may be introduced in the manufacturing process of silicon substrate, the existence of these metal contaminations is by the yield of serious harm device and reliability, though back side gettering process can be adopted to improve silicon substrate metal contamination situation, but back side gettering process can not address this problem completely, and the detection means accuracy of detection that silicon substrate producer adopts is lower, can not effectively detect the situation of staiing in substrate.Based on this, the invention provides a kind of method checking silicon substrate quality, first silicon substrate is heated up and process of lowering the temperature, when there is contamination in substrate back damage layer gettering poor effect or silicon substrate supplied materials, contamination in the contamination at the silicon substrate back side and edge or heating and cooling equipment can be overflowed and be transferred to substrate face, then grown epitaxial layer on a silicon substrate, position epitaxial growth perfection of lattice silicon substrate existing contamination will be damaged, carry out corrosion to the epitaxial loayer on silicon substrate defect to be come out, such employing metallomicroscope carries out the quality that epi-layer surface defects detection can judge silicon substrate, just contamination in silicon substrate can be known when silicon substrate supplied materials, after avoiding flow, batch is scrapped, prevention order is paid and is postponed.
For making content of the present invention clearly understandable, below in conjunction with Figure of description, content of the present invention is described further.Certain the present invention is not limited to this specific embodiment, and the general replacement known by those skilled in the art is also encompassed in protection scope of the present invention.
As shown in Figure 1, the invention provides a kind of method checking silicon substrate quality, comprise the following steps:
S01: silicon substrate is heated up and process of lowering the temperature;
S02: at described silicon substrate growing epitaxial layers;
S03: described epitaxial loayer is corroded; And
S04: adopt metallomicroscope to carry out surface defects detection to described silicon substrate, judged the quality of described silicon substrate by the quantity of blemish.
In the present embodiment, the epitaxial furnace of RF heating is adopted to heat up to silicon substrate and process of lowering the temperature.Conventional epitaxial mode of heating is divided into infrared radiation heating and radio frequency heating two kinds, infrared radiation heating mode directly heats silicon substrate, and RF heating first heats epitaxial furnace pedestal, then realized the rising of silicon substrate temperature by epitaxial furnace pedestal and silicon substrate transmission of heat by contact.RF heating makes the temperature of epitaxial furnace pedestal higher than the temperature of silicon substrate, and the temperature at the silicon substrate back side is higher than the temperature in silicon substrate front simultaneously, is conducive to the effusion of the metal contamination at the silicon substrate back side and edge, is more conducive to metal contamination and transfers to front.For LPE2061 epitaxial furnace, corresponding epitaxial furnace pedestal is higher than silicon substrate temperature about 20 DEG C, and silicon substrate back temperature is higher than positive surface temperature simultaneously, through overtesting, under equal conditions, uses the effect of radio frequency heating epitaxial furnace more obvious.It should be noted that, the epitaxial furnace adopting RF heating is a kind of preferred version, other equipment also can be adopted to heat up to silicon substrate and the object processing and overflow with the metal contamination reached in silicon substrate of lowering the temperature.
In preferred version, carry out in 10-24 minute, silicon substrate temperature being risen to more than 1100 DEG C in hyperthermic treatment process to silicon substrate, carry out at least in 18-35 minute, silicon substrate temperature being down to less than 150 DEG C in cooling processing procedure to silicon substrate, be rapidly heated and express delivery temperature-fall period by above-mentioned, be conducive to staiing in silicon substrate fully evaporate and nucleation be fixed on silicon substrate front, so that subsequent detection.Further, described hyperthermic treatment process specifically comprises: in hydrogen atmosphere, in 6-15 minute, silicon substrate temperature is risen to 850-900 DEG C from 100 DEG C; And in hydrogen atmosphere, in 4-9 minute, silicon substrate temperature is risen to more than 1100 DEG C from 850-900 DEG C.Described cooling processing procedure specifically comprises: in hydrogen atmosphere, in 6-10 minute, silicon substrate temperature is down to 700-850 DEG C; And close hydrogen inflated with nitrogen, in 12-25 minute, silicon substrate temperature is down to 100 DEG C.
Shown in associative list 1, in the present embodiment, step S01 can specifically comprise six sub-steps: inflation 1, inflation 2, intensification 1, intensification 2, cooling 1, cooling 2.
| Sub-step | Gas | Temperature (DEG C) | Time (minute) |
| Inflation 1 | Nitrogen | 100 | 3 |
| Inflation 2 | Hydrogen | 100 | 3 |
| Heat up 1 | Hydrogen | 100-900 | 6 |
| Heat up 2 | Hydrogen | 900-1120 | 9 |
| Cooling 1 | Hydrogen | 1120-800 | 10 |
| Cooling 2 | Nitrogen | 800-100 | 15 |
Table 1
In sub-step inflation 1, put into by silicon substrate on epitaxial furnace pedestal, and epitaxial furnace pedestal to be imported into standby temperature be in the epitaxial furnace of 100 DEG C, the air in extension cavity is driven out of by inflated with nitrogen for 3 minutes;
In sub-step inflation 2, keep the temperature that epitaxial furnace is original, fill hydrogen and the nitrogen in extension cavity was driven out of in 3 minutes;
In sub-step intensification 1, in hydrogen atmosphere, by heating epitaxial furnace pedestal, in 6 minutes, silicon substrate is rapidly heated to 900 DEG C from 100 DEG C;
In sub-step intensification 2, in hydrogen atmosphere, by the control to extension furnace foundation seat temperature, in 9 minutes, silicon substrate is warmed up to 1120 DEG C from 900 DEG C;
In sub-step cooling 1, in hydrogen atmosphere, by the control to extension furnace foundation seat temperature, in 10 minutes, silicon substrate is cooled to 800 DEG C from 1120 DEG C;
In sub-step cooling 2, close heater, close hydrogen, by inflated with nitrogen cooling epitaxial furnace pedestal and silicon substrate, silicon substrate is cooled to the standby temperature of 100 DEG C in 15 minutes from 800 DEG C.
Found through experiments, adopt aforesaid way can make to stain in silicon substrate fully to evaporate to transfer to silicon substrate front, and nucleation is fixed on silicon substrate front in temperature-fall period, so that subsequent detection.Certainly, above-mentioned explanation is not intended to limit the present invention, also can according to the technological parameter in the apparatus adaptability adjustment intensification adopted and temperature-fall period.
As the preferred embodiment of the invention, in step S02, the mode of original position extension can be adopted, namely adopt the epitaxial furnace used in step S01 at described silicon substrate growing epitaxial layers, compared to heating and cooling processing procedure, only need during grown epitaxial layer additionally to pass into silicon source again, like this without the need to transferred silicon substrate between board, production efficiency is higher.
As the preferred embodiment of the invention, in step S03, chromic acid can be adopted to corrode described epitaxial loayer, chromic acid is chemical corrosion liquid conventional in semiconductor production, adopt chromic acid to carry out corrosion and be easier to control corrosion rate speed, too fastly epitaxial loayer can not be caused to erode rapidly cannot observe defect effect owing to corroding.
By the way, when silicon substrate back side damage effect is not good enough effectively can not absorb clamper metal contamination time, utilize silicon substrate being rapidly heated and lowering the temperature in epitaxial furnace, the trace meter contamination at the silicon substrate back side in silicon substrate manufacture process or edge can be evaporated and partly transfers to silicon substrate front, and nucleation is fixed on silicon substrate front in fast cooling process.When silicon substrate back side damage effect is good, or metal contamination is slight, and silicon substrate being rapidly heated and process of lowering the temperature in epitaxial furnace, metal contamination can't in the front nucleation of silicon substrate.When described silicon substrate growing epitaxial layers, metal contamination nucleation site epitaxial growth perfection of lattice will be damaged formation defect, and there is no the epitaxial growth lattice perfection of metal contamination nucleation site, be similar to by epitaxial growth and amplify staiing in silicon substrate, when subsequently chromic acid corrosion being carried out to the silicon substrate of described formation epitaxial loayer, metal contamination nucleation site epitaxial growth defect etching out (defective position can form step), and there is no the epitaxial growth zero defect of metal contamination nucleation site, finally carry out observation with metallomicroscope and can find defect, the quality of silicon substrate is judged by the presence or absence epitaxial growth defect of surface of silicon and the quantity of epitaxial growth defect.
Present inventor adopts said method to confirm Different Silicon substrate supplier difference production numbering batch, find that wherein a collection of surface of silicon has epitaxial growth defect, as shown in Figure 2, epitaxial growth defect is mainly distributed in the border area 101 of silicon substrate, and the zone line 102 of silicon substrate does not almost have.As shown in Figure 3, find through metallography microscope sem observation, the roughly triangular in shape or strip of the epitaxial growth defect pattern that substrate distributes.Arrange sensitive product flow process experiment to this batch of silicon substrate, and find after carrying out failure analysis, defect analysis result and silicon substrate defect etching distribute basically identical.As can be seen here, by above-mentioned detection method, do not need to increase expensive checkout equipment, the situation of the metal contamination in silicon substrate can be detected when silicon substrate supplied materials ahead of time.
Although the present invention discloses as above with preferred embodiment; so itself and be not used to limit the present invention; have in any art and usually know the knowledgeable; without departing from the spirit and scope of the present invention; when doing a little change and retouching, therefore protection scope of the present invention is when being as the criterion depending on those as defined in claim.
Claims (11)
1. detect a method for silicon substrate quality, it is characterized in that, comprising:
Silicon substrate is heated up and process of lowering the temperature;
At described silicon substrate growing epitaxial layers; And
Described epitaxial loayer is corroded, and adopts metallomicroscope to carry out surface defects detection to described silicon substrate, judged the quality of described silicon substrate by the quantity of blemish.
2. the method detecting silicon substrate quality as claimed in claim 1, is characterized in that, adopts epitaxial furnace to heat up to described silicon substrate and process of lowering the temperature.
3. the method detecting silicon substrate quality as claimed in claim 2, is characterized in that, described epitaxial furnace is the epitaxial furnace adopting RF heating.
4. the method detecting silicon substrate quality as claimed in claim 1, is characterized in that, carry out, in hyperthermic treatment process, in 10-24 minute, silicon substrate temperature being risen to more than 1100 DEG C to silicon substrate.
5. the method detecting silicon substrate quality as claimed in claim 4, it is characterized in that, described hyperthermic treatment process specifically comprises:
In hydrogen atmosphere, in 6-15 minute, silicon substrate temperature is risen to 850-900 DEG C from 100 DEG C; And
In hydrogen atmosphere, in 4-9 minute, silicon substrate temperature is risen to more than 1100 DEG C from 850-900 DEG C.
6. the method detecting silicon substrate quality as claimed in claim 1, is characterized in that, carry out, in cooling processing procedure, in 18-35 minute, silicon substrate temperature being down to less than 150 DEG C to silicon substrate.
7. the method detecting silicon substrate quality as claimed in claim 6, it is characterized in that, it is characterized in that, described cooling processing procedure specifically comprises:
In hydrogen atmosphere, in 6-10 minute, silicon substrate temperature is down to 700-850 DEG C; And
Close hydrogen inflated with nitrogen, in 12-25 minute, silicon substrate temperature is down to 100 DEG C.
8. the method detecting silicon substrate quality as claimed in claim 1, is characterized in that, before described hyperthermic treatment, also comprise:
Import in epitaxial furnace by the epitaxial furnace pedestal being placed with silicon substrate, the air in extension cavity is driven out of by inflated with nitrogen; And
Keep the temperature that extension cavity is original, fill hydrogen and the nitrogen in extension cavity is driven out of.
9. the method detecting silicon substrate quality as claimed in claim 1, is characterized in that, adopts epitaxial furnace to heat up to silicon substrate and process of lowering the temperature.
10. the method detecting silicon substrate quality as claimed in claim 9, is characterized in that, described epitaxial furnace is the epitaxial furnace adopting RF heating.
11. methods detecting silicon substrate quality as claimed in claim 1, is characterized in that, adopt chromic acid to corrode described epitaxial loayer.
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| CN106328549A (en) * | 2015-06-19 | 2017-01-11 | 中芯国际集成电路制造(上海)有限公司 | Detection method for oxygen precipitation in wafer |
| CN106898568A (en) * | 2015-12-18 | 2017-06-27 | 中芯国际集成电路制造(上海)有限公司 | A kind of monitoring method of chamber degree of purity |
| CN107689334A (en) * | 2016-08-05 | 2018-02-13 | 中芯国际集成电路制造(北京)有限公司 | The preparation method and quality determining method of polysilicon quality testing sample |
| TWI617809B (en) * | 2016-03-22 | 2018-03-11 | 中美矽晶製品股份有限公司 | Method of examining quality of silicon material |
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