CN115926747A - Concentrated aqueous grinding aid and preparation method thereof - Google Patents
Concentrated aqueous grinding aid and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a concentrated aqueous grinding aid, which consists of the following raw materials in parts by weight: 30-50 parts of deionized water, 5-10 parts of a composite thixotropic agent, 5-10 parts of an emulsion stabilizer, 20-30 parts of a lubricant, 1-5 parts of a bactericide and 1-5 parts of an antifoaming agent. The concentrated aqueous grinding aid is applied to grinding processing of silicon carbide and gallium nitride wafers, so that the processing cost of directly using diamond grinding fluid finished products can be greatly reduced; meanwhile, the diamond abrasive particles can be quickly dispersed and suspended, and a stable suspension with thixotropic property is formed. The lubricant can effectively reduce the friction resistance in the grinding process, increase the lubricity, effectively improve the quality of the grinding surface and greatly shorten the polishing time of the subsequent wafer in the using process.
Description
Technical Field
The invention belongs to the technical field of ultra-precision grinding and polishing, and particularly relates to a concentrated aqueous grinding aid for processing silicon carbide and gallium nitride wafers and a preparation method thereof.
Background
Third-generation semiconductor materials, such as silicon carbide and gallium nitride, are considered to be ideal materials for semiconductor chips because of their characteristics, such as high breakdown voltage, low loss, and high efficiency, and have become a new focus of the leading edge of semiconductor technology research and the competition of industries in various countries. The ultra-precision grinding is a subsequent process for processing silicon carbide and gallium nitride wafers, is a key step for ensuring the surfaces of the silicon carbide and gallium nitride wafers to be ultra-smooth, free of defects and free of damage, and directly determines the quality of the wafers and power devices. However, since silicon carbide, gallium nitride and the like belong to high-hardness and brittle materials, the processing difficulty is far greater than that of sapphire, silicon wafers, stainless steel and the like, and the problems of low removal efficiency, large surface roughness, difficulty in controlling scratches and the like are specifically shown.
The grinding aid is a uniform and stable aid integrating multiple functions of dispersion, suspension, wetting, lubrication and the like, can be used with an abrasive and a solvent in situ, and can be applied to grinding and processing silicon carbide and gallium nitride wafers to reduce the surface roughness of the wafers.
At present, the grinding processing usually uses diamond grinding fluid or boron carbide, alumina powder to add water and grind the processing, and diamond grinding fluid dispersion is even and has certain suspension lubricating property, and machining efficiency is high, surface roughness is low, but the price is expensive, and boron carbide, alumina abrasive processing are mostly that the direct water distribution of abrasive uses, and the cost is lower relatively, but because it lacks essential dispersion suspension and lubricating property and leads to machining efficiency low and surface roughness big. Based on this, research and development of new grinding aids are needed to meet the processing requirements of existing materials such as silicon carbide and gallium nitride.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a concentrated aqueous grinding aid for processing silicon carbide and gallium nitride wafers, which can reduce the grinding processing cost and keep relatively high processing efficiency and quality.
The invention also provides a preparation method of the concentrated aqueous grinding aid.
In order to realize the purpose, the invention adopts the following technical scheme:
a concentrated aqueous grinding aid is composed of the following raw materials in parts by weight: 30-50 parts of deionized water, 5-10 parts of a composite thixotropic agent, 5-10 parts of an emulsion stabilizer, 20-30 parts of a lubricant, 1-5 parts of a bactericide and 1-5 parts of an antifoaming agent.
Specifically, the compound thixotropic agent can be one or a mixture of more than two of hydrogenated castor oil, castor oil polyoxyethylene ether, water-based bentonite, nano silicon dioxide and the like.
Further, the emulsion stabilizer can be one or a mixture of more than two of fatty amine polyoxyethylene ether, polyethylene glycol monomethyl ether, polypropylene glycol monomethyl ether, fatty alcohol-polyoxyethylene ether and the like.
Specifically, the lubricant may be one or a mixture of two or more of propylene glycol, glycerin, polyethylene glycol, hydroxyethyl cellulose, polyvinylpyrrolidone, and the like.
Further, the bactericide may be a non-oxidizing bactericide such as dodecylbenzyl ammonium chloride, dodecyldimethylbenzyl ammonium bromide, or the like.
Specifically, the defoamer may be a silicone defoamer.
The invention provides a preparation method of the concentrated aqueous grinding aid, which comprises the following steps: taking the raw materials according to a certain proportion, uniformly mixing deionized water and a lubricant, slowly adding the composite thixotropic agent and the emulsion stabilizer into the solution under the stirring condition, fully and uniformly stirring to form an emulsion, finally slowly adding the bactericide and the defoaming agent, and uniformly stirring to form the concentrated aqueous grinding aid.
The invention also provides a use method of the concentrated aqueous grinding aid, which comprises the following steps: fully and uniformly stirring and mixing diamond grinding materials and water, slowly adding a concentrated aqueous grinding aid accounting for 1-10wt% of the water under the stirring condition, fully stirring and dissolving to form a uniform diamond suspension, and directly grinding and processing silicon carbide and gallium nitride wafers.
In the application method of the concentrated aqueous grinding aid, the addition amount of the diamond grinding material is 1-10% of the mass of water. Further, the addition amount of the concentrated aqueous grinding aid is preferably 3 to 5wt% based on the mass of water.
The concentrated aqueous grinding aid is applied to grinding processing of silicon carbide and gallium nitride wafers, so that the processing cost of directly using diamond grinding fluid finished products can be greatly reduced; meanwhile, the diamond abrasive particles can be quickly dispersed and suspended, and a stable suspension with thixotropic property is formed. The lubricant can effectively reduce the frictional resistance in the grinding process, increase the lubricity, effectively improve the quality of the grinding surface and greatly shorten the polishing time of the subsequent wafer in the using process.
Compared with the prior art, the invention has the following beneficial effects:
in order to reduce the grinding processing cost and keep relatively high processing efficiency and quality, the invention provides a concentrated aqueous grinding aid, wherein the composite thixotropic agent with a net structure uniformly locks and suspends abrasive particles in a solution, and meanwhile, the emulsion stabilizer can keep a limit concentrated system stable for a long time. The concentrated aqueous grinding aid can be used in situ with diamond abrasive and solvent, is applied to grinding silicon carbide and gallium nitride wafers, can quickly disperse and suspend diamond abrasive particles while greatly reducing the cost, forms thixotropic stable suspension with a space network structure, keeps the abrasive suspended for a long time, and can reduce the friction resistance in the grinding process, increase the lubricity, effectively improve the grinding surface quality, quickly reduce the surface roughness and shorten the subsequent polishing time in the use process. The invention provides a preparation process and a use method of a concentrated aqueous grinding aid, which greatly reduce the cost of the existing finished product of directly using a diamond grinding fluid and improve the grinding effect of directly using boron carbide, alumina powder and water.
Drawings
FIG. 1 is a photograph of a diamond polishing solution prepared in example 3 under a microscope at 100 times magnification;
FIG. 2 is a photograph of the diamond polishing solution prepared in comparative example 1 under a microscope at an magnification of 100 times;
FIG. 3 is a photograph of the silicon carbide surface polished by the polishing slurry of example 3 under a microscope of 100 times;
FIG. 4 is a photograph of the silicon carbide surface polished by the polishing slurry of comparative example 3 under a microscope at a magnification of 100 times.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following examples, but the scope of the present invention is not limited thereto.
In the following examples, the starting materials used were all ordinary commercially available products which were directly purchased or were prepared according to a conventional method in the art. Hydrogenated castor oil, for example, is purchased from basf, germany as hydrogenated castor oil CO40; the water-based bentonite is purchased from Zhejiang Kangbaixin New materials Co., ltd; the bactericide is purchased from dodecyl benzyl ammonium chloride of Jinan Ming chemical engineering Co., ltd; the defoamer was purchased from MY-208 silicone defoamer, of mays chemicals ltd.
Example 1
A concentrated aqueous grinding aid is composed of the following raw materials in parts by weight: 50g of deionized water, 20g of propylene glycol lubricant, 10g of hydrogenated castor oil thixotropic agent, 10g of lauryl amine polyoxyethylene ether emulsion stabilizer, 5g of bactericide and 5g of defoaming agent.
The concentrated aqueous grinding aid is prepared by the following steps: uniformly mixing deionized water and a lubricant, slowly adding the composite thixotropic agent and the emulsion stabilizer into the solution in sequence under the stirring condition, fully and uniformly stirring to form emulsion, finally slowly adding the bactericide and the defoaming agent, and uniformly stirring to form the concentrated aqueous grinding aid.
The use method of the diamond grinding fluid prepared by the concentrated aqueous grinding aid comprises the following steps: 50g of diamond grinding material (the granularity is 4.5 mu m) and 1000g of water are taken to be stirred and mixed evenly by ultrasound, 10g of concentrated aqueous grinding aid is slowly added under the stirring condition, and after the mixture is fully stirred and dissolved, uniform diamond suspension is formed.
Example 2
A concentrated aqueous grinding aid is composed of the following raw materials in parts by weight: 50g of deionized water, 30g of propylene glycol lubricant, 8g of hydrogenated castor oil thixotropic agent, 8g of lauryl amine polyoxyethylene ether emulsion stabilizer, 2g of bactericide and 2g of defoaming agent.
The preparation method of the concentrated aqueous grinding aid is described in example 1.
The use method of the diamond grinding fluid prepared by the concentrated aqueous grinding aid comprises the following steps: 50g of diamond grinding material (with the granularity of 4.5 mu m) and 1000g of water are taken to be stirred and mixed evenly by ultrasound, 30g of concentrated aqueous grinding aid is slowly added under the stirring condition, and the diamond grinding material is stirred and dissolved fully to form uniform diamond suspension.
Example 3
A concentrated aqueous grinding aid is composed of the following raw materials in parts by weight: 50g of deionized water, 20g of polyethylene glycol lubricant, 10g of waterborne bentonite thixotropic agent, 10g of polypropylene glycol monomethyl ether emulsion stabilizer, 5g of bactericide and 5g of defoaming agent.
The preparation method of the concentrated aqueous grinding aid is described in example 1.
The use method of the diamond grinding fluid prepared from the concentrated aqueous grinding aid comprises the following steps: 50g of diamond grinding material (with the granularity of 4.5 mu m) and 1000g of water are taken to be stirred and mixed evenly by ultrasound, 50g of concentrated aqueous grinding aid is slowly added under the stirring condition, and after the mixture is fully stirred and dissolved, uniform diamond suspension is formed.
FIG. 1 shows a picture of the diamond slurry prepared in example 3 under a microscope with a magnification of 100 times; as can be seen in fig. 1: the diamond grinding fluid prepared by the grinding aid of the invention has the advantages of uniform dispersion of abrasive particles and no agglomeration of the abrasive particles.
Example 4
A concentrated aqueous grinding aid is composed of the following raw materials in parts by weight: 50g of deionized water, 30g of polyvinylpyrrolidone lubricant, 8g of waterborne bentonite thixotropic agent, 8g of polypropylene glycol monomethyl ether emulsion stabilizer, 2g of bactericide and 2g of defoamer.
The preparation method of the concentrated aqueous grinding aid is described in example 1.
The use method of the diamond grinding fluid prepared by the concentrated aqueous grinding aid comprises the following steps: 50g of diamond grinding material (the granularity is 4.5 mu m) and 1000g of water are taken to be stirred and mixed evenly by ultrasound, 100g of concentrated aqueous grinding aid is slowly added under the stirring condition, and after the mixture is fully stirred and dissolved, uniform diamond suspension is formed.
Example 5
The concentrated aqueous grinding aid comprises, by weight, 50g of deionized water, 30g of a glycerol lubricant, 5g of a castor oil polyoxyethylene ether thixotropic agent, 5g of a fatty alcohol polyoxyethylene ether emulsion stabilizer, 5g of a bactericide and 5g of a defoaming agent.
The preparation method of the concentrated aqueous grinding aid is described in example 1.
The use method of the diamond grinding fluid prepared by the concentrated aqueous grinding aid comprises the following steps: 50g of diamond grinding material (the granularity is 4.5 mu m) and 1000g of water are taken to be stirred and mixed evenly by ultrasound, 50g of concentrated aqueous grinding aid is slowly added under the stirring condition, and after the mixture is fully stirred and dissolved, uniform diamond suspension is formed.
Example 6
The concentrated aqueous grinding aid comprises, by weight, 50g of deionized water, 25g of hydroxyethyl cellulose lubricant, 10g of castor oil polyoxyethylene ether thixotropic agent, 5g of fatty alcohol polyoxyethylene ether emulsion stabilizer, 5g of bactericide and 5g of defoamer.
The preparation method of the concentrated aqueous grinding aid is described in example 1.
The use method of the diamond grinding fluid prepared from the concentrated aqueous grinding aid comprises the following steps: 50g of diamond grinding material (the granularity is 4.5 mu m) and 1000g of water are taken to be stirred and mixed evenly by ultrasound, under the stirring condition, 50g of concentrated aqueous grinding aid is slowly added, and after the mixture is fully stirred and dissolved, uniform diamond suspension is formed.
Comparative example 1
The diamond grinding fluid consists of the following raw materials in parts by weight: 50g of diamond grit (4.5 μm particle size), 1000g of water. The preparation method comprises the following steps: and (3) taking 50g of diamond grinding material and 1000g of water, ultrasonically stirring and uniformly mixing to form the diamond grinding fluid.
FIG. 2 shows a 100-fold microscopic image of the diamond polishing slurry prepared in comparative example 1; as can be seen in fig. 2: the grinding fluid without the grinding aid of the invention has the advantages of uneven dispersion of abrasive particles and serious agglomeration.
Comparative example 2
A conventional W-4.5-MA type diamond abrasive fluid is commercially available.
Comparative example 3
The boron carbide grinding fluid is composed of the following raw materials in parts by weight: 200g of boron carbide abrasive (particle size 5 μm), 1000g of water. The preparation method comprises the following steps: and (3) taking 200g of diamond grinding material and 1000g of water, ultrasonically stirring and uniformly mixing to form the boron carbide grinding fluid.
Comparative example 4
The grinding aid consists of the following raw materials in parts by weight: 60g of deionized water, 20g of propylene glycol lubricant, 10g of lauryl amine polyoxyethylene ether emulsion stabilizer, 5g of bactericide and 5g of defoaming agent.
The above grinding aid was prepared by the method described in example 1.
The use method of the diamond grinding fluid prepared from the grinding aid comprises the following steps: 50g of diamond grinding material (the granularity is 4.5 mu m) and 1000g of water are taken to be stirred and mixed evenly by ultrasound, 10g of concentrated aqueous grinding aid is slowly added under the stirring condition, and after the mixture is fully stirred and dissolved, uniform diamond suspension is formed.
Comparative example 5
The grinding aid consists of the following raw materials in parts by weight: 31g of deionized water, 30g of propylene glycol lubricant, 20g of hydrogenated castor oil thixotropic agent, 15g of lauryl amine polyoxyethylene ether emulsion stabilizer, 2g of bactericide and 2g of defoaming agent.
The above grinding aid was prepared by the method described in example 1.
The use method of the diamond grinding fluid prepared from the concentrated aqueous grinding aid comprises the following steps: 50g of diamond grinding material (the granularity is 4.5 mu m) and 1000g of water are taken to be stirred and mixed evenly by ultrasound, 30g of concentrated aqueous grinding aid is slowly added under the stirring condition, and after the mixture is fully stirred and dissolved, uniform diamond suspension is formed.
The diamond polishing liquids of examples 1 to 6 and comparative examples 1 to 5 above were used to polish 4-inch-diameter silicon carbide substrate pieces. A YM-18LX type single-side grinder with a pressure of 200g/cm2, a rotation speed of 45rpm, a diamond polishing solution flow rate of 5ml/min, and a grinding time of 30min was used. The efficiency detection is calculated by measuring the thickness change before and after grinding by using a decimetric meter, the surface roughness is measured by using a roughness meter, and the scratch detection is carried out under a naked eye strong light. The specific test results are as follows:
TABLE 1 comparison of grinding application Properties
As can be seen from Table 1: the diamond grinding fluid prepared by the grinding aid has the advantages that the abrasive particles are uniformly dispersed, the grinding efficiency is highest when the addition amount is 5%, the abrasive particles are not less than 1.35 mu m/min, the surface roughness is not more than 0.013 mu m, no scratch is generated, and the diamond grinding fluid is obviously superior to the commercially available finished diamond grinding fluid in the comparative example 2. When the grinding aid of the invention is not added, the abrasive of the diamond grinding fluid of the comparative example 1 is unevenly dispersed, the removal efficiency is only 0.88 μm/min, the surface roughness is 0.046 μm, and simultaneously scratches are generated. When the boron carbide abrasive described in comparative example 3 was used in combination with water, the removal efficiency was only 0.75 μm/min, and the surface roughness was 0.063 μm, which is significantly lower than the processing level of the diamond suspension formulated in the present invention. When part of the raw material of the present invention was not added or part of the raw material was added in excess (comparative examples 4 and 5), the removal rate was significantly reduced, the surface roughness was increased, and scratches were generated, resulting in deterioration of the surface quality.
FIGS. 3 and 4 show 100-fold microscopic images of the silicon carbide surface after polishing with the polishing slurry of example 3 and comparative example 3, respectively. As can be seen from fig. 3 and 4: the diamond grinding fluid prepared by the grinding aid of the invention has uniform and consistent lines on the surface of the silicon carbide after grinding and no scratch, while the grinding lines on the surface of the silicon carbide are disordered and the scratch is obvious after the grinding fluid of the comparative example 3 is adopted for grinding.
In summary, the concentrated aqueous grinding aid formulation of the present invention is an organic whole, and beyond this system, poor grinding results. Meanwhile, the data show that the cost of the existing diamond grinding fluid finished product directly used is greatly reduced, the grinding effect of directly using boron carbide and alumina powder mixed with water is improved, the grinding efficiency and the surface quality can be obviously improved, and the addition amount of the concentrated aqueous grinding aid is preferably 3-5%.
Claims (9)
1. The concentrated aqueous grinding aid is characterized by comprising the following raw materials in parts by weight: 30-50 parts of deionized water, 5-10 parts of a composite thixotropic agent, 5-10 parts of an emulsion stabilizer, 20-30 parts of a lubricant, 1-5 parts of a bactericide and 1-5 parts of an antifoaming agent.
2. The concentrated aqueous grinding aid according to claim 1, wherein the composite thixotropic agent is one or a mixture of more than two of hydrogenated castor oil, castor oil polyoxyethylene ether, aqueous bentonite and nano-silica.
3. The concentrated aqueous grinding aid of claim 1, wherein the emulsion stabilizer is one or a mixture of two or more of fatty amine polyoxyethylene ether, polyethylene glycol monomethyl ether, polypropylene glycol monomethyl ether, and fatty alcohol polyoxyethylene ether.
4. The concentrated aqueous grinding aid according to claim 1, wherein the lubricant is one or a mixture of two or more of propylene glycol, glycerin, polyethylene glycol, hydroxyethyl cellulose, and polyvinylpyrrolidone.
5. The concentrated aqueous grinding aid of claim 1, wherein the biocide is a non-oxidizing biocide.
6. A concentrated aqueous grinding aid according to claim 1, wherein the defoamer is a silicone defoamer.
7. A method of preparing a concentrated aqueous grinding aid according to any one of claims 1 to 6, comprising the steps of: taking the raw materials according to a certain proportion, uniformly mixing deionized water and a lubricant, adding a compound thixotropic agent and an emulsion stabilizer into the solution under the stirring condition, uniformly stirring to form an emulsion, finally adding a bactericide and an antifoaming agent, and uniformly stirring to obtain the emulsion.
8. The use method of the concentrated aqueous grinding aid according to any one of claims 1 to 6, characterized in that diamond grinding materials and water are uniformly stirred, the concentrated aqueous grinding aid accounting for 1-10wt% of the water is added under the stirring condition, and after stirring and dissolving, a uniform diamond suspension is formed and is directly used for grinding silicon carbide and gallium nitride wafers.
9. The method of using a concentrated aqueous grinding aid according to claim 8, wherein the diamond grit is added in an amount of 1 to 10% by mass of water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118064061A (en) * | 2024-04-18 | 2024-05-24 | 浙江大学 | Silicon carbide wafer polishing liquid for double-sided synchronous polishing, preparation method and application |
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