CN109679506B - Water-based polishing solution for fine polishing of SiC single crystal wafer and preparation method thereof - Google Patents
Water-based polishing solution for fine polishing of SiC single crystal wafer and preparation method thereof Download PDFInfo
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- CN109679506B CN109679506B CN201910001859.7A CN201910001859A CN109679506B CN 109679506 B CN109679506 B CN 109679506B CN 201910001859 A CN201910001859 A CN 201910001859A CN 109679506 B CN109679506 B CN 109679506B
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Abstract
A water-based polishing solution for fine polishing of SiC single crystal wafers and a preparation method thereof are disclosed, wherein the initial polishing solution is pretreated to meet a first condition, and the pretreated initial polishing solution is subjected to impurity removal to obtain the water-based polishing solution, and the pretreatment method comprises the following steps: and placing the initial polishing solution into a polishing device to perform rough polishing treatment on the SiC single crystal wafer or the material with the same hardness as the SiC single crystal wafer. The effect of finely polishing the SiC single crystal wafer by the water-based polishing solution obtained by roughly polishing the polishing solution reaches the optimal state; after the SiC single crystal wafer is precisely polished by the water-based polishing solution prepared by the method, the damage and scratches on the surface of the SiC single crystal wafer can be obviously reduced, and the high-quality SiC single crystal wafer can be obtained.
Description
Technical Field
The application belongs to the technical field of ultra-precision surface grinding and polishing, and particularly relates to a water-based polishing solution for fine polishing of a SiC single crystal wafer and a preparation method thereof.
Background
Silicon carbide single crystal is one of the most important third-generation semiconductor materials, and is widely applied to the fields of power electronics, radio frequency devices, photoelectronic devices and the like because of the excellent properties of large forbidden bandwidth, high saturated electron mobility, strong breakdown field, high thermal conductivity and the like. When used as an epitaxial thin film substrate, epitaxial growth is highly substrate-dependent, and a small defect on the substrate also destroys the periodicity of the surface of the silicon carbide single crystal, spreads and spreads on the thin film, and seriously affects the film quality. Even when used as a seed, the bulk single crystal material grown is severely affected by the substrate and all defects on the surface of the substrate are typically replicated as is into the new epitaxial material.
In order to obtain high quality thin films and bulk single crystals, polishing methods are mainly used at present. Chenopodium et al propose to polish wafers by hydrogen, but this method does little to the deep scratches left during mechanical polishing. In addition, lingueming et al propose that the wafer is subjected to plasma etching after being ground, and the method utilizes plasma to bombard the surface of the silicon carbide to remove the damaged layer formed in the grinding process, and the method has high removal rate, but often introduces new damage and defects while removing the damaged layer.
CN102337082A discloses a chemical mechanical polishing solution for silicon carbide substrate, which comprises the following components in percentage by weight as shown below: 1-50 wt% of an abrasive; 0.01 to 8 wt% of a chelating agent; 0.01 to 10 wt% of a surfactant; 0.01 to 10 wt% of a dispersant; 0.1 to 20 wt% of an oxidizing agent; the balance being deionized water. The polishing solution has small damage to the surface of the silicon carbide substrate; the roughness value of the silicon carbide substrate is low, and the roughness Ra value can be less than 0.5 nm; the surface of the substrate has no defects of scratches and corrosion pits; the removal rate is high, and the cleaning is easy; does not corrode processing equipment and pollute the environment; the raw materials are cheap and low in cost; is easy to store. The polishing solution is mainly used for chemical mechanical polishing of silicon carbide crystals for substrates. The application discloses the composition of the polishing solution, but does not explore how the polishing solution is treated to achieve the best use condition.
In CN106349948A, a method for preparing a nano polishing solution is disclosed, which comprises the following steps: uniformly mixing silicon carbide micro powder, water and a dispersing agent according to a mass ratio to obtain a mixture, and then placing the mixture into a sand mill for circular crushing until the particle size of a solid material in the mixture is nano-scale to obtain nano-silicon carbide slurry; secondly, adding water for dilution to obtain a nano silicon carbide suspension; and thirdly, adding a chelating agent, a lubricant, a preservative and a pH regulator, and uniformly stirring to obtain the nano polishing solution. The nano polishing solution prepared by the invention is aqueous, and has the advantages of environmental protection, quick polishing and heat dissipation, strong diluting capability, low cost and the like. The application discloses a method for preparing the polishing solution, but does not explore how the polishing solution can be used optimally during the use process.
In the prior art, the research on the polishing solution mostly focuses on the composition, the proportion and the preparation method of the polishing solution, but neglects how the polishing solution can achieve the best use effect in the use process. Which is often the key to determining the quality of the SiC single wafer after polishing.
Content of application
In order to solve the problems, the application provides a water-based polishing solution for fine polishing of a SiC single crystal wafer and a preparation method thereof, the initial polishing solution is pretreated to meet a first condition, and the pretreated initial polishing solution is subjected to impurity removal to obtain the water-based polishing solution, wherein the pretreatment method comprises the following steps: the initial polishing solution is placed in a polishing device to polish the SiC single crystal wafer or the material with the hardness similar to that of the SiC single crystal wafer, and the SiC single crystal wafer is roughly polished. The material with approximate hardness of the SiC single crystal wafer refers to a material with Mohs hardness not less than 9 and less than 10.
Because different molecules such as abrasive, dispersing agent, polymerization inhibitor, stabilizer and the like exist in the polishing solution, on one hand, the surface of the abrasive cannot be ensured to be smooth, if the surface of the SiC monocrystal wafer is not smooth, the surface of the SiC monocrystal wafer can be damaged or scratched when the SiC monocrystal wafer is subjected to fine polishing treatment, and on the other hand, the quality of the SiC monocrystal wafer is influenced, and on the other hand, the abrasive in the polishing solution can be agglomerated, so that the polishing solution cannot uniformly perform fine polishing treatment on the SiC monocrystal wafer in an initial use state, and a good fine polishing effect cannot be achieved; on the other hand, other auxiliary components added into the polishing solution cannot be matched well in the initial use state, the matching among particles is not in place, and the optimal fine polishing effect cannot be achieved. According to the method, the initial polishing solution is prepared, the SiC single crystal wafer is not subjected to fine polishing treatment immediately, but the initial polishing solution is firstly placed in a polishing device to perform rough polishing treatment on the SiC single crystal wafer or a material with the same hardness as the SiC single crystal wafer, so that the purpose of the treatment is to perform rough polishing treatment on the SiC single crystal wafer on one hand, and damage or scratches on the surface of the original SiC single crystal wafer are reduced; on the other hand, through rough polishing treatment, the surfaces of the grinding particles in the initial polishing solution are smoother and smoother, and the particles in the polishing solution are more uniformly and stably dispersed and have higher matching degree; but also can increase the content of solid components in the grinding fluid and improve the grinding effect. When the initial polishing solution is subjected to rough polishing treatment to reach the first condition, impurity removal is carried out on the initial polishing solution to obtain the water-based polishing solution, and the rough polishing treatment can also be carried out on the initial polishing solution by using a material with the same hardness as the SiC single wafer.
Preferably, the initial polishing solution comprises the following raw materials in parts by weight: 0.1-0.3 part of polymerization inhibitor, 0.2-0.5 part of dispersant, 20-40 parts of stabilizer and 10-20 parts of abrasive. The polishing solution contains the abrasive material as a component playing a polishing role, and the polymerization inhibitor and the dispersant are added into the polishing solution to prevent the abrasive material from agglomerating, so that the dispersibility of particles in the polishing solution is better, the contact area of the abrasive material and the SiC single wafer in the prepared polishing solution is larger, and the polishing efficiency is higher; the stabilizer is added to enhance the stability of the polishing solution.
Preferably, the polymerization inhibitor comprises one or more than two of benzoquinone, aniline, benzenediol, sodium carboxymethylcellulose, polymaleic acid, polyamino acid, sodium polyacrylate, phosphonic acid carboxylic acid, glycerol and propylene glycol, and the mixture ratio of the two or more than two is arbitrary; the dispersing agent comprises one or more than two of water glass, sodium tripolyphosphate, sodium hexametaphosphate, sodium pyrophosphate, triethylhexyl phosphoric acid, sodium dodecyl sulfate, methylpentanol, polyacrylamide, Guel gum and polyethylene glycol fatty acid ester, and the mixture ratio of the two or more than two is arbitrary.
Preferably, the stabilizer comprises one or more of ethanol, propanol, isopropanol, butanol, isobutanol, ethylene glycol, glycerol, glucose, gluconic acid, fructose, mannose and maltose, and the mixture of the two or more is in any proportion.
Preferably, the abrasive is a high-hardness powder material having a median particle diameter of 0.5 to 5 μm.
Preferably, the high-hardness powder material contains at least diamond.
Preferably, the high-hardness powder material further comprises one or a mixture of more than two of cubic boron nitride, boron carbide and aluminum oxide, and the mixture ratio of the two or more is arbitrary.
Preferably, the polishing device is a double-sided polishing machine.
Preferably, the rotation speed of the upper disc of the rough polishing treatment is 16-20rpm, the rotation speed of the lower disc is 20-30rpm, the pressure is 30-40MPa, and the time is 4-6 h.
Preferably, the first condition is that the initial polishing solution is used for not less than 140 hours, and is subjected to filtering treatment; preferably, the filtration treatment is performed under conditions that the polishing solution is passed through a filtration membrane at one or more times, the pore size of the filtration membrane being in the range of 0.5 to 1 μm.
The water-based polishing solution prepared by the preparation method.
This application can bring following beneficial effect: the effect of finely polishing the SiC single crystal wafer by the water-based polishing solution obtained by roughly polishing the polishing solution reaches the optimal state; after the SiC single crystal wafer is precisely polished by the water-based polishing solution prepared by the method, the damage and scratches on the surface of the SiC single crystal wafer can be obviously reduced, and the high-quality SiC single crystal wafer can be obtained.
Detailed Description
Example 1: the preparation method of the initial polishing solution comprises the following steps:
s1, mixing deionized water and 10-20 parts of grinding materials, and uniformly stirring to obtain a mixed solution;
s2, adding 0.1-0.3 part of polymerization inhibitor, 0.2-0.5 part of dispersant and 20-40 parts of stabilizer into the intermediate liquid, and uniformly stirring to obtain the initial polishing solution.
Example 2: the method for pre-treating the initial polishing solution to obtain the water-based polishing solution comprises the following steps:
s1, ultrasonically cleaning the grinded SiC single crystal wafer or the material with the same hardness as the SiC single crystal wafer, wherein the cleaning agent comprises one of hydrochloric acid, nitric acid, sulfuric acid and hydrofluoric acid, the cleaning condition is cleaning for 20min, and the cleaning temperature is controlled at 50 +/-5 ℃.
S2, using the initial polishing solution prepared in the embodiment 1, roughly polishing the grinded SiC single crystal wafer or the material with the same hardness as the SiC single crystal wafer on a double-sided polishing machine, wherein the primary rough polishing process of the SiC single crystal wafer or the material with the same hardness as the SiC single crystal wafer comprises the steps of upper disc rotating speed of 16-20rpm, lower disc rotating speed of 20-30rpm and pressure of 35MPa, and if the rough polishing object is the SiC single crystal wafer, the rough polishing can be completed by controlling the processing time to be 4-6 h.
And S3, after the initial polishing solution is subjected to rough polishing for more than 140 hours, filtering the pretreated water-based polishing solution to obtain the water-based polishing solution, wherein the filtering condition is that the polishing solution passes through a filter membrane once or for many times, and the aperture range of the filter membrane is 0.5-1 μm.
Specific examples are as follows:
the composition of each sample is shown in the following table:
in the above table, the polymerization inhibitor includes: one or more than two of benzoquinone, aniline, benzenediol, sodium carboxymethylcellulose, polymaleic acid, polyamino acid, sodium polyacrylate, phosphonic acid carboxylic acid, glycerol and propylene glycol are mixed, and the mixture ratio of the two or more than two is arbitrary; the dispersant comprises: one or more than two of water glass, sodium tripolyphosphate, sodium hexametaphosphate, sodium pyrophosphate, triethylhexyl phosphoric acid, sodium dodecyl sulfate, methyl amyl alcohol, polyacrylamide, Guergel gum and polyethylene glycol fatty acid ester are mixed, and the mixture ratio of the two or more than two is arbitrary; the stabilizer comprises one or more than two of ethanol, propanol, isopropanol, butanol, isobutanol, ethylene glycol, glycerol, glucose, gluconic acid, fructose, mannose and maltose, and the mixture ratio of the two or more than two is arbitrary; the grinding material is one or the mixture of more than two of diamond, cubic boron nitride, boron carbide and alumina, and the mixture ratio of the two is arbitrary.
Example 3: the step of finely polishing the SiC single crystal wafer using the water-based polishing liquid in example 2:
s1, carrying out ultrasonic cleaning on the SiC single crystal wafer after rough polishing in the embodiment 2, wherein the cleaning condition is that the cleaning time is 20min, and the cleaning temperature is controlled at 50 +/-5 ℃.
S2, inputting the water-based polishing solution obtained in the embodiment 2 into another special polishing machine for fine polishing, and performing fine polishing on the SiC single crystal wafer cleaned in the step 1 by adopting a fine polishing process, wherein the fine polishing process comprises an upper disc rotating speed of 12rpm, a lower disc rotating speed of 17rpm, a pressure of 35MPa and a time of 1.5 h.
Example 4: characterization of
According to the comparison of the experimental results of the comparative example 1 and the example 3, the fact that the removal rate is reduced when the SiC single crystal wafer is polished due to the low content of the polymerization inhibitor, and the surface of the polished SiC single crystal wafer is rougher is also known, because the particles in the polishing solution are agglomerated to different degrees due to the low content of the polymerization inhibitor, the SiC single crystal wafer cannot be uniformly polished when being contacted with the particles in the polishing solution, and the contact area is reduced.
From comparison of the experimental results of comparative example 2 and example 2, it is understood that the reason why the removal rate is decreased when the SiC single crystal wafer is polished due to a small content of the dispersant, the surface of the SiC single crystal wafer after polishing is rougher, and the contact area is decreased because the particles in the polishing liquid are not uniformly dispersed and the SiC single crystal wafer is not uniformly polished when contacting the particles in the polishing liquid.
From the experimental results of comparative example 3 and example 3, it is understood that the removal rate is decreased when the SiC single wafer is polished due to a small content of the stabilizer, the surface of the SiC single wafer is rougher after polishing, and unstable phenomena such as delamination and coagulation of the abrasive may occur during polishing of the SiC single wafer due to an unstable state of the polishing liquid, and the SiC single wafer cannot be stably polished.
From the experimental results of comparative example 4 and example 2, it is understood that the amount of the abrasive is reduced and the removal rate of the SiC single crystal wafer is lowered when polished.
According to the experimental results of comparative example 5 and example 1, when the grinding time is less than 140h, the initial polishing solution is not optimized to the use condition.
According to the experimental results, the following results are obtained: the same polishing conditions and the same polishing process are used for polishing the same SiC single crystal wafer, the initial polishing solution is used for directly polishing, the initial polishing solution is used for roughly polishing to obtain the water-based polishing solution, compared with the step of polishing the SiC single crystal wafer by using the water-based polishing solution, the SiC single crystal wafer obtained by using the water-based polishing solution has higher removal rate and smaller surface roughness, the reason that the initial polishing solution is firstly roughly polished and then the material is polished is fully explained, the polishing efficiency is higher, the surface of the obtained SiC single crystal wafer is smoother, and the quality is higher, is that: on one hand, after rough polishing treatment, the particle dispersibility of the polishing solution is stronger, which is beneficial to polishing; on the other hand, the surface of the particles in the initial polishing solution is not smooth, and after rough polishing treatment, the surface of the abrasive particles in the polishing solution is smoother, which is beneficial to reducing the damage or scratch generated on the surface of the SiC single crystal wafer; on the other hand, through rough polishing treatment, the matching degree of all components in the polishing solution is improved.
According to the experimental results, the following results are obtained: the stability of the water-based polishing solution is better than that of the initial polishing solution, which shows that after the initial polishing solution is polished, the particles in the polishing solution are dispersed more uniformly, the dispersibility is improved, the polishing solution is more stable, and the phenomenon of agglomeration, sedimentation or layering is not easy to occur.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (8)
1. A preparation method of water-based polishing solution for fine polishing of SiC single crystal wafers is characterized by comprising the following steps: pretreating the initial polishing solution until a first condition is met, and removing impurities from the pretreated initial polishing solution to obtain a water-based polishing solution, wherein the pretreatment method comprises the following steps: placing the initial polishing solution into a polishing device to polish the SiC single crystal wafer or the material with the hardness similar to that of the SiC single crystal wafer;
the SiC single crystal wafer is made of a material with approximate hardness, namely a material with Mohs hardness not less than 9 and less than 10;
the initial polishing solution comprises the following raw materials in parts by weight: 0.1-0.3 part of polymerization inhibitor, 0.2-0.5 part of dispersant, 20-40 parts of stabilizer and 10-20 parts of abrasive;
the first condition is that the initial polishing solution is used for not less than 140 hours, and filtering treatment is carried out.
2. The method for preparing the water-based polishing solution for the fine polishing of the SiC single crystal wafer according to claim 1, which is characterized by comprising the following steps: the polymerization inhibitor comprises one or more than two of benzoquinone, aniline, benzenediol, sodium carboxymethylcellulose, polymaleic acid, polyamino acid, sodium polyacrylate, phosphonic acid carboxylic acid, glycerol and propylene glycol, and the mixture ratio of the two or more than two is arbitrary; the dispersing agent comprises one or more than two of water glass, sodium tripolyphosphate, sodium hexametaphosphate, sodium pyrophosphate, triethylhexyl phosphoric acid, sodium dodecyl sulfate, methylpentanol, polyacrylamide, Guel gum and polyethylene glycol fatty acid ester, and the mixture ratio of the two or more than two is arbitrary; the stabilizer comprises one or more than two of ethanol, propanol, isopropanol, butanol, isobutanol, ethylene glycol, glycerol, glucose, gluconic acid, fructose, mannose and maltose, and the mixture ratio of the two or more than two is arbitrary.
3. The method for preparing the water-based polishing solution for the fine polishing of the SiC single crystal wafer according to claim 1, which is characterized by comprising the following steps: the abrasive is a high-hardness powder material, and the median particle size of the high-hardness powder material is 0.5-5 mu m.
4. The method for preparing the water-based polishing solution for the fine polishing of the SiC single crystal wafer according to claim 3, wherein the method comprises the following steps: the high-hardness powder material contains at least diamond.
5. The method for preparing the water-based polishing solution for the fine polishing of the SiC single crystal wafer according to claim 4, wherein the method comprises the following steps: the high-hardness powder material also comprises one or more than two of cubic boron nitride, boron carbide and aluminum oxide, and the mixture ratio of the two or more than two is arbitrary.
6. The method for preparing the water-based polishing solution for the fine polishing of the SiC single crystal wafer according to claim 1, which is characterized by comprising the following steps: the polishing device is a double-sided polishing machine.
7. The method for preparing the water-based polishing solution for the fine polishing of the SiC single crystal wafer according to claim 1, which is characterized by comprising the following steps: the filtering treatment condition is that the polishing solution passes through the filter membrane once or for many times, and the aperture range of the filter membrane is 0.5-1 μm.
8. A water-based polishing liquid obtained by the production method as set forth in any one of claims 1 to 7.
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