CN109679506A - A kind of SiC single crystal piece essence throwing water base polishing fluid and preparation method thereof - Google Patents
A kind of SiC single crystal piece essence throwing water base polishing fluid and preparation method thereof Download PDFInfo
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- CN109679506A CN109679506A CN201910001859.7A CN201910001859A CN109679506A CN 109679506 A CN109679506 A CN 109679506A CN 201910001859 A CN201910001859 A CN 201910001859A CN 109679506 A CN109679506 A CN 109679506A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/04—Aqueous dispersions
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Abstract
A kind of SiC single crystal piece essence throwing water base polishing fluid and preparation method thereof, initial burnishing liquid is pre-processed to meeting first condition, water base polishing fluid will be obtained after the removal of impurities of pretreated initial burnishing liquid, the pretreated method includes: that initial burnishing liquid is placed in burnishing device to carry out rough polishing processing to SiC single crystal piece or material identical with SiC single crystal sheet hardness.The application reaches optimum state by carrying out the effect that the water base polishing fluid obtained after rough polishing pretreatment carries out smart throwing to SiC single crystal piece to polishing fluid；After being thrown by water base polishing fluid prepared by the application to SiC single crystal piece essence, it can be substantially reduced damage and the scratch on SiC single crystal piece surface, obtain the SiC single crystal piece of high quality.
Description
Technical field
The application belongs to superfinishing surface grinding polishing technology field, and in particular to a kind of water base throwing of SiC single crystal piece essence throwing
Light liquid and preparation method thereof.
Background technique
Single-crystal silicon carbide is one of most important third generation semiconductor material, because its with forbidden bandwidth big, saturated electrons
The excellent properties such as mobility is high, breakdown field is powerful, thermal conductivity is high, and it is widely used in power electronics, radio-frequency devices, photoelectron
The fields such as device.When as epitaxial film substrate, epitaxial growth is very strong to substrate dependence, and the defect of very little also can on substrate
The periodicity for destroying silicon carbide single-crystal surface, spreads and expands on film, and seriously affect film quality.Even as seed
Crystalline substance, the bulk single crystal materials to grow out also will receive substrate and seriously affect, and all defect on substrate surface generally can be former
Sample copies in new epitaxial material.
In order to obtain the film and bulk single crystal of high quality, the grinding and polishing method mainly used at present.Chen little Long et al. is proposed
Grinding and polishing carries out hydrogen decorations to chip, but this method, to the deeper scratch left in mechanical polishing process, effect is little.Separately
Outside, plasma etching is carried out after the bright equal proposition wafer grinding of Lin Yue, this method utilizes plasma bombardment silicon carbide, removal
The damaging layer formed in process of lapping, this method removal rate is very high, but often introduces newly while removing damaging layer
Damage and defect.
A kind of silicon carbide substrates chemical mechanical polishing liquid is disclosed in CN102337082A, it includes weights as follows
Measure the following components of percentage: 1~50 weight % of abrasive material；0.01~8 weight % of chelating agent；0.01~10 weight of surfactant
Measure %；0.01~10 weight % of dispersing agent；0.1~20 weight % of oxidant；Remaining is deionized water.The polishing fluid is to carbonization
Surface of silicon damage is small；Silicon carbide substrates roughness value is low, can reach roughness Ra value less than 0.5nm；Substrate surface without draw
The defect of trace and etch pit；Removal rate is high, is readily cleaned；Process equipment, free from environmental pollution is not corroded；The prices of raw materials are just
Preferably, at low cost；It is easily stored.The polishing fluid is mainly used for the chemically mechanical polishing of the carborundum crystals of substrate.This application is public
The composition of polishing fluid has been opened, but has not probed into its polishing fluid and how to handle and can be only achieved optimal use state.
A kind of preparation method of nanometer burnishing liquid is disclosed in CN106349948A, comprising the following steps: one, will carbonization
Silicon powder is uniformly mixed in mass ratio with water and dispersing agent, obtains mixture, and then the mixture is placed in sand mill
Circulation crushes, until the partial size of solid material is nanoscale in mixture, obtains nanometer silicon carbide slurry；Two, it is diluted with water, obtains
To nano silicon carbide silicon suspension；Three, chelating agent, lubricant, preservative and pH adjusting agent is added, obtains nanometer throwing after mixing evenly
Light liquid.Use nanometer burnishing liquid prepared by the present invention to be aqueous, have environmentally protective, polishing rapid heat dissipation, dilution capacity it is strong, at
This low advantage.That application discloses the preparation methods of polishing fluid, but do not probe into yet polishing fluid in use how
Reach optimal use state.
The composition for mostly laying stress on polishing fluid, proportion are probed into, in preparation method to polishing fluid in the prior art, but
It is all to have ignored how polishing fluid can be only achieved best use effect in use.And this often determines SiC single crystal piece
The key of quality after being polished.
Apply for content
To solve the above-mentioned problems, present applicant proposes a kind of SiC single crystal piece essences to throw with water base polishing fluid and its preparation side
Initial burnishing liquid is pre-processed to first condition is met, will be obtained after the removal of impurities of pretreated initial burnishing liquid water base by method
Polishing fluid, the pretreated method include: that initial burnishing liquid is placed in burnishing device to SiC single crystal piece or and SiC single crystal
The approximate material of sheet hardness is processed by shot blasting, it should be noted that is rough polishing processing for SiC single crystal piece.SiC single crystal piece is hard
Spending approximate material refers to Mohs' hardness not less than 9, the material less than 10.
Due to the molecule different there are abrasive material, dispersing agent, polymerization inhibitor, stabilizer etc. in polishing fluid, on the one hand cannot be guaranteed
Abrasive surface be it is smooth, then, will be to SiC single crystal piece table when carrying out essence to SiC single crystal piece and throwing processing if not smooth
Damage or scratch are caused in face, affect the quality of SiC single crystal piece instead, on the other hand, in polishing fluid between abrasive material there may be
Agglomeration, so that polishing fluid under initial use state, uniformly cannot carry out smart throwing processing to SiC single crystal piece, be not achieved
Essence throws effect well；In another aspect, other auxiliary elements being added in polishing fluid are also impossible under initial use state just
Can it is mutually matched very well, cooperate between particle it is not in place, be also not achieved it is optimal essence throw effect.The application is preparing initial throwing
Light liquid is not to carry out smart throwing processing to SiC single crystal piece at once, but first initial burnishing liquid is placed in burnishing device to SiC
Single-chip or material identical with SiC single crystal sheet hardness carry out rough polishing processing, and on the one hand the purpose handled in this way is can be to SiC
Single-chip carries out rough polishing processing, mitigates the existing damage in script SiC single crystal piece surface or scratch；On the other hand, at by rough polishing
Reason, the polishing particles surface more smooth in initial burnishing liquid is smooth, and each particle dispersion in lapping liquid more evenly, it is more steady
Calmly, fitness is also higher；But also the content of solid component in lapping liquid can be increased, improve grinding effect.It is thrown when to initial
Light liquid carries out being cleaned to obtain water base polishing fluid to it after rough polishing processing reaches first condition, and the application can also use and SiC
The identical material of monocrystalline sheet hardness carries out rough polishing processing.
Preferably, initial burnishing liquid includes the raw material of following parts by weight: 0.1-0.3 parts of polymerization inhibitor, dispersing agent 0.2-0.5
Part, 20-40 parts of stabilizer, 10-20 parts of abrasive material.The ingredient that polishing action is played in polishing fluid is abrasive material, is added in polishing fluid
Polymerization inhibitor and dispersing agent are that abrasive material is reunited in order to prevent, so that particle dispersibility is more preferable in polishing fluid, prepares obtain in this way
Polishing fluid in abrasive material and SiC single crystal piece contact area it is bigger, polishing efficiency is higher；It is to enhance polishing fluid that stabilizer, which is added,
Stability.
Preferably, the polymerization inhibitor includes benzoquinones, aniline, benzenediol, sodium carboxymethylcellulose, poly, poly- amino
The mixing of one or more of acid, Sodium Polyacrylate, phosphonic acids yl carboxylic acid, glycerine, propylene glycol, when two or more mixing
Arbitrarily to match；The dispersing agent includes waterglass, sodium tripolyphosphate, calgon, sodium pyrophosphate, triethyl group hexyl phosphorus
One or both of acid, lauryl sodium sulfate, methyl anyl alcohol, polyacrylamide, guar gum, cithrol with
On mixing, be any proportion when two or more mixing.
Preferably, the stabilizer includes ethyl alcohol, propyl alcohol, isopropanol, butanol, isobutanol, ethylene glycol, glycerine, grape
The mixing of one or more of sugar, gluconic acid, fructose, mannose, maltose is arbitrarily matched when two or more mixing
Than.
Preferably, the abrasive material is high rigidity dusty material, and the median of the high rigidity dusty material is 0.5-5 μ
m。
Preferably, at least contain diamond in the high rigidity dusty material.
Preferably, the high rigidity dusty material further includes one or both of cubic boron nitride, boron carbide, aluminium oxide
Above mixing is any proportion when two or more mixing.
Preferably, the burnishing device is Twp-sided polishing machine.
Preferably, the upper disk rotating speed of the rough polishing processing is 16-20rpm, and lower disk rotating speed is 20-30rpm, pressure 30-
40MPa, time 4-6h.
Preferably, the first condition is that initial burnishing liquid uses the time to be not less than 140h, and carries out filtration treatment；It is preferred that
, the condition of the filtration treatment be polishing fluid is one or many through filter membrane, filter membrane pore diameter range is at 0.5-1 μm.
The water base polishing fluid that above-mentioned preparation method obtains.
The application can be brought the following benefits: the application passes through to the water obtained after polishing fluid progress rough polishing pretreatment
The effect that base polishing fluid carries out smart throwing to SiC single crystal piece reaches optimum state；The water base polishing fluid prepared by the application is to SiC
After single-chip essence is thrown, it can be substantially reduced damage and the scratch on SiC single crystal piece surface, obtain the SiC single crystal piece of high quality.
Specific embodiment
Embodiment 1: the preparation method of initial burnishing liquid the following steps are included:
S1, first deionized water and 10-20 parts of abrasive material mixed, and is uniformly mixing to obtain mixed liquor；
S2, by 0.1-0.3 parts of polymerization inhibitor, 0.2-0.5 parts of dispersing agent, 20-40 parts of stabilizer are added in intermediate liquid, and
It is uniformly mixing to obtain initial burnishing liquid.
Embodiment 2: the method for being pre-processed to obtain water base polishing fluid of initial burnishing liquid:
S1, ultrasonic cleaning is carried out to SiC single crystal piece after grinding or material identical with SiC single crystal sheet hardness, wherein clearly
Lotion includes one kind of hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, and cleaning condition is cleaning 20min, and cleaning temperature is controlled at 50 DEG C ± 5
℃。
S2, using the initial burnishing liquid prepared in embodiment 1, on Twp-sided polishing machine to SiC single crystal piece after grinding or
Material identical with SiC single crystal sheet hardness carries out rough polishing processing, to SiC single crystal piece or material identical with SiC single crystal sheet hardness
It is 16-20rpm that the processing technology for carrying out a rough polishing, which is upper disk rotating speed, lower disk rotating speed be 20-30rpm, pressure 35MPa, if
Rough polishing object is SiC single crystal piece, then process time control can complete rough polishing in 4-6h.
S3, for initial burnishing liquid, rough polishing technique carries out after the time is more than 140h, by the water base polishing fluid pre-processed into
Water base polishing fluid is obtained by filtration in row, and the condition of the filtration treatment is that polishing fluid is one or many through filter membrane, filtering fenestra
Diameter range is at 0.5-1 μm.
Specific embodiment is as follows:
The composition of each sample see the table below:
In upper table, the polymerization inhibitor includes: benzoquinones, aniline, benzenediol, sodium carboxymethylcellulose, poly, poly- amino
The mixing of one or more of acid, Sodium Polyacrylate, phosphonic acids yl carboxylic acid, glycerine, propylene glycol, when two or more mixing
Arbitrarily to match；The dispersing agent includes: waterglass, sodium tripolyphosphate, calgon, sodium pyrophosphate, triethyl group hexyl phosphorus
One or both of acid, lauryl sodium sulfate, methyl anyl alcohol, polyacrylamide, guar gum, cithrol with
On mixing, be any proportion when two or more mixing；The stabilizer include ethyl alcohol, propyl alcohol, isopropanol, butanol, isobutanol,
The mixing of one or more of ethylene glycol, glycerine, glucose, gluconic acid, fructose, mannose, maltose, two kinds
It is any proportion when the above mixing；The abrasive material is one or both of diamond, cubic boron nitride, boron carbide, aluminium oxide
Above mixing is any proportion when two or more mixing.
Embodiment 3: the step of essence is thrown is carried out to SiC single crystal piece using the water base polishing fluid in embodiment 2:
S1, the SiC single crystal piece after progress rough polishing in embodiment 2 is carried out to ultrasonic cleaning, cleaning condition is cleaning
20min, cleaning temperature are controlled at 50 DEG C ± 5 DEG C.
S2, the water base polishing fluid for obtaining embodiment 2 input another essence and throw in special glazing machine, are thrown using essence and process work
Skill carries out smart throwing to the SiC single crystal piece after cleaning in step 1, and it is upper disk rotating speed 12rpm that essence, which throws processing technology, and lower disk rotating speed is
17rpm, pressure 35MPa, time 1.5h.
Embodiment 4: characterization
According to the comparison of the experimental result of comparative example 1 and embodiment 3 it is found that level of inhibitor is few, SiC single crystal piece is gone when polishing
Removal rates can decline, and SiC single crystal piece surface is also more coarse after polishing, this is because level of inhibitor is very little, in polishing fluid
Different degrees of reunion can occur for grain, just can not uniformly be polished, be connect when SiC single crystal piece is with particle contact in polishing fluid
Contacting surface product also becomes smaller.
According to the comparison of the experimental result of comparative example 2 and embodiment 2 it is found that dispersant is few, SiC single crystal piece is gone when polishing
Removal rates can decline, and SiC single crystal piece surface is also more coarse after polishing, and being also due to particle dispersion in polishing fluid, unevenly, SiC is mono-
It just can not uniformly be polished when chip is with particle contact in polishing fluid, the reason of contact area becomes smaller.
According to the experimental result of comparative example 3 and embodiment 3 it is found that stabiliser content is few, removal speed when SiC single crystal piece polishes
Rate can decline, and SiC single crystal piece surface is also more coarse after polishing, be also due to polishing fluid state labile, and SiC single crystal piece is polishing
When, it is understood that there may be wild effects, the SiC single crystal pieces such as layering, coagulation, which occur, for abrasive material cannot carry out stable polishing.
According to the experimental result of comparative example 4 and embodiment 2 it is found that amount of abrasive is reduced, removal rate when SiC single crystal piece polishes
It can decline.
According to the experimental result of comparative example 5 and embodiment 1 it is found that 140h is not achieved between upon grinding, to initial burnishing
Use condition is not achieved in the optimization of liquid.
According to experimental result: same polishing condition and polishing process polish same SiC single crystal piece, make
Polishing is directly carried out with initial burnishing liquid to handle to obtain water base polishing fluid with by initial burnishing liquid progress rough polishing, utilizes water base polishing
Liquid carries out polishing to SiC single crystal piece and compares, and the SiC single crystal piece removal rate obtained using water base polishing fluid is higher, and surface is thick
Rugosity is smaller, and when absolutely proving initial burnishing liquid first carrying out rough polishing processing, then polishing to material, polishing efficiency is higher,
Obtained SiC single crystal piece surface is smoother, and quality is higher, and reason is: on the one hand after rough polishing is handled, the particle of polishing fluid
Dispersibility is stronger, is conducive to be polished；On the other hand, particle surface and unsmooth in initial burnishing liquid, is handled by rough polishing
Afterwards, the abrasive particle surface in polishing fluid is smoother, advantageously reduces SiC single crystal piece surface and generates damage or scratch；Another side
Face is handled by rough polishing, and the fitness in polishing fluid between each ingredient improves.
According to experimental result: the stability of water base polishing fluid is more preferable than the stability of initial burnishing liquid, illustrates to first
After beginning polishing fluid is processed by shot blasting, more evenly, dispersibility is improved, and polishing fluid is just more stable, does not allow for particle dispersion in polishing fluid
Easily there is a phenomenon where sedimentation or the layerings of reuniting.
All the embodiments in this specification are described in a progressive manner, same and similar portion between each embodiment
Dividing may refer to each other, and each embodiment focuses on the differences from other embodiments.Especially for system reality
For applying example, since it is substantially similar to the method embodiment, so being described relatively simple, related place is referring to embodiment of the method
Part explanation.
The above description is only an example of the present application, is not intended to limit this application.For those skilled in the art
For, various changes and changes are possible in this application.All any modifications made within the spirit and principles of the present application are equal
Replacement, improvement etc., should be included within the scope of the claims of this application.
Claims (10)
1. the preparation method that a kind of SiC single crystal piece essence throws water base polishing fluid, it is characterised in that: located initial burnishing liquid in advance
Reason will obtain water base polishing fluid, the pretreated method after the removal of impurities of pretreated initial burnishing liquid to first condition is met
It include: that initial burnishing liquid is placed in burnishing device to SiC single crystal piece or is polished with the approximate material of SiC single crystal sheet hardness
Processing.
2. the preparation method that a kind of SiC single crystal piece essence according to claim 1 throws water base polishing fluid, which is characterized in that
Initial burnishing liquid includes the raw material of following parts by weight: 0.1-0.3 parts of polymerization inhibitor, 0.2-0.5 parts of dispersing agent, and stabilizer 20-40
Part, 10-20 parts of abrasive material.
3. the preparation method that a kind of SiC single crystal piece essence according to claim 1 throws water base polishing fluid, it is characterised in that:
The polymerization inhibitor includes benzoquinones, aniline, benzenediol, sodium carboxymethylcellulose, poly, polyaminoacid, Sodium Polyacrylate, phosphine
The mixing of one or more of acidic group carboxylic acid, glycerine, propylene glycol is any proportion when two or more mixing；It is described
Dispersing agent includes waterglass, sodium tripolyphosphate, calgon, sodium pyrophosphate, triethyl group hexyl phosphoric acid, dodecyl sulphate
The mixing of one or more of sodium, methyl anyl alcohol, polyacrylamide, guar gum, cithrol, two kinds with
It is any proportion when upper mixing；The stabilizer include ethyl alcohol, propyl alcohol, isopropanol, butanol, isobutanol, ethylene glycol, glycerine,
The mixing of one or more of glucose, gluconic acid, fructose, mannose, maltose, two or more mixing Shi Weiren
Meaning proportion.
4. a kind of preparation method of water base polishing fluid of SiC single crystal slice lapping according to claim 1, it is characterised in that:
The abrasive material is high rigidity dusty material, and the median of the high rigidity dusty material is 0.5-5 μm.
5. a kind of preparation method of water base polishing fluid of SiC single crystal slice lapping according to claim 4, it is characterised in that:
At least contain diamond in the high rigidity dusty material.
6. a kind of preparation method of water base polishing fluid of SiC single crystal slice lapping according to claim 5, it is characterised in that:
The high rigidity dusty material further includes the mixing of one or more of cubic boron nitride, boron carbide, aluminium oxide, and two kinds
It is any proportion when the above mixing.
7. the preparation method that a kind of SiC single crystal piece essence according to claim 1 throws water base polishing fluid, it is characterised in that:
The burnishing device is Twp-sided polishing machine.
8. the preparation method that a kind of SiC single crystal piece essence according to claim 7 throws water base polishing fluid, it is characterised in that:
The upper disk rotating speed of the rough polishing processing is 16-20rpm, and lower disk rotating speed is 20-30rpm, time 4-6h.
9. the preparation method that a kind of SiC single crystal piece essence according to claim 1 throws water base polishing fluid, it is characterised in that:
The first condition is that initial burnishing liquid uses the time to be not less than 140h, and carries out filtration treatment；Preferably, the filtration treatment
Condition be polishing fluid is one or many through filter membrane, filter membrane pore diameter range is at 0.5-1 μm.
10. the water base polishing fluid that any preparation method of claim 1-9 obtains.
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Cited By (2)
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| CN110539240A (en) * | 2019-07-18 | 2019-12-06 | 浙江博蓝特半导体科技股份有限公司 | Processing method of silicon carbide single crystal substrate |
| CN114346765A (en) * | 2021-11-23 | 2022-04-15 | 宁夏金昱元广拓能源有限公司 | Method for treating outer surface of carbon steel drum |
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| CN114346765A (en) * | 2021-11-23 | 2022-04-15 | 宁夏金昱元广拓能源有限公司 | Method for treating outer surface of carbon steel drum |
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