CN113980581B - Environment-friendly suspending agent based on sapphire grinding, and preparation method and application thereof - Google Patents
Environment-friendly suspending agent based on sapphire grinding, and preparation method and application thereof Download PDFInfo
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- CN113980581B CN113980581B CN202111429844.4A CN202111429844A CN113980581B CN 113980581 B CN113980581 B CN 113980581B CN 202111429844 A CN202111429844 A CN 202111429844A CN 113980581 B CN113980581 B CN 113980581B
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Abstract
The invention provides an environment-friendly suspending agent based on sapphire grinding, and a preparation method and application thereof. The environment-friendly suspending agent based on sapphire grinding comprises the following components in parts by mass: 0.5-2.5 parts of thickening agent; 3-15 parts of a chelating agent monomer; 5-15 parts of a chelating promoter; 2-8 parts of a dispersing agent; 0.1-1 part of surfactant; 0.1-1 part of defoaming agent; 0.1-1 part of antirust agent; 3-20 parts of a pH regulator; 30-50 parts of ultrapure water. The invention also discloses a preparation method of the environment-friendly suspending agent based on sapphire grinding. The environment-friendly suspending agent based on sapphire grinding has the characteristics of high suspensibility and good stability, and the raw materials involved in the formula are environment-friendly substances; the suspending agent provided by the invention is used for grinding the sapphire wafer, so that the removal rate of the sapphire wafer can be obviously improved, the surface flatness is increased, and the surface roughness is greatly reduced.
Description
Technical Field
The invention relates to a suspending agent technology, in particular to an environment-friendly suspending agent based on sapphire grinding, a preparation method and application thereof.
Background
Sapphire of composition alpha-A12O3The hardness is second to that of diamond, the Mohs hardness is 9 grade, the optical property and the mechanical property are the same as those of natural gem, the thermal property, the electrical property and the dielectric property are good, the infrared transmittance is high, the wear resistance is good, and the stability is good at high temperature. With the rapid development of the photoelectric technology, the demand of photoelectric products for sapphire substrate materials is increasing day by day, and with the continuous expansion of LED elements, sapphire has become one of the most important substrate materials, and has great domestic and foreign market demands.
Sapphire mechanical processing is very difficult, crystal face processing technology is complex, and is one of key subjects of domestic and foreign research, sapphire wafers used in practical production application are all made by cutting and polishing crystal bars, semiconductor crystal bars are generally cut into wafers by using a wire cutting machine or a multi-wire cutting machine, but in the cutting process, processing conditions fluctuate, and therefore deviations exist in the aspects of the thickness and the surface flatness of the cut wafers. In device fabrication, surface defects and surface quality of the substrate wafer affect the quality of subsequent GaN epitaxial growth, and therefore, the surface quality of the wafer is very important for the fabrication of high performance devices. Therefore, sapphire is required to have a surface roughness of less than 2nm for other optical applications, and less than 0.8nm for substrate materials. Therefore, it must be polished by grinding.
At present, the existing grinding and polishing technologies mainly comprise: mechanical lapping and polishing, chemical polishing, laser polishing, ion beam polishing and the like. Wherein the mechanical polishing is liable to generate scratches on the mirror surface; chemical polishing of sapphireThe surface is not smooth and clean, and a large amount of acid or alkaline chemical reagents are needed, so that the pollution is large; the laser and ion beam polished wafer has high surface quality and few defects, but the laser equipment is expensive and the technology is not perfect. Therefore, Chemical Mechanical Polishing (CMP) is the most widely used processing technology in China and abroad. In the CMP, the surface material of a workpiece and polishing solution are subjected to chemical reaction to generate a soft layer which is relatively easy to remove, and then the soft layer is removed under the mechanical action to expose the surface of the workpiece again, so that the surface polishing of the workpiece is completed under the alternating action of chemistry and machinery. Most of the prior polishing and grinding liquids are SiO containing an oxidant and a catalyst2The aqueous solution has low removal rate of sapphire grinding processing, low processing efficiency, poor sapphire surface quality and difficulty in reaching finer degree. In addition, most of the existing suspending agents adopt dangerous chemicals which are difficult to degrade, such as alkane substances, and the hazardous effect to the environment is large. Therefore, the suspending agent raw material involved in the invention adopts environment-friendly substances, and has important significance.
Disclosure of Invention
The invention aims to provide an environment-friendly suspending agent based on sapphire grinding, aiming at the problems of low grinding rate, low wafer flatness, poor stability and great environmental hazard when the existing suspending agent is used for grinding sapphire wafers, wherein the suspending agent has the characteristics of high suspensibility and good stability, and the raw materials involved in the formula are environment-friendly substances; the suspending agent provided by the invention is used for grinding the sapphire wafer, so that the removal rate of the sapphire wafer can be obviously improved, the surface flatness is increased, and the surface roughness is greatly reduced.
In order to realize the purpose, the invention adopts the technical scheme that: an environment-friendly suspending agent based on sapphire grinding comprises the following components in parts by mass:
further, the thickening agent is hydrophilic, alkali-resistant and stable, and is one or more of sodium carboxymethyl cellulose, hydroxyethyl cellulose, sodium caseinate and acacia gum, preferably sodium carboxymethyl cellulose. The thickener is preferably 1-2 parts.
Further, the chelating agent monomer is dopamine hydrochloride, and the chelation accelerator is tris (hydroxymethyl) aminomethane; and reacting the dopamine hydrochloride with Tris (hydroxymethyl) aminomethane (Tris) to generate chelating agent polydopamine. The chelating agent monomer is preferably 10-15 parts, and the chelating promoter is preferably 5-10 parts.
Further, the dispersing agent is one or more of vinyl bis stearamide, glycerol monostearate, butyl stearate, ethylene-acrylic acid copolymer, sodium polyacrylate, magnesium stearate and polyethylene wax, and sodium polyacrylate is preferred. The dispersant is preferably 3 to 5 parts.
Further, the surfactant is a cationic surfactant such as cetyltrimethylammonium bromide, dodecyltrimethylammonium chloride and dodecyldimethylbenzylammonium chloride; or anionic surfactants such as sodium dodecylbenzenesulfonate, sodium lauryl sulfate and sodium lauryl sarcosinate; or nonionic surfactants, e.g. isomeric decyl alcohol polyoxyethylene ethers, isomeric tridecyl alcohol polyoxyethylene ethers and C12-14Fatty alcohol polyoxyethylene ethers, preferably C12-14Fatty alcohol polyoxyethylene ether. The surfactant is preferably 0.2-0.5 parts.
Further, the defoaming agent is one or more of polyoxypropylene glycerol polyether (molecular weight is 1 ten thousand to 10 ten thousand), polyoxypropylene polyoxyethylene glycerol ether (molecular weight is 1 ten thousand to 10 ten thousand), polyoxypropylene polyoxyethylene glycerol polyether ester (molecular weight is 1 ten thousand to 10 ten thousand) and dimethicone and polyether-siloxane copolymer, and dimethicone is preferred. The defoaming agent is preferably 0.3 to 0.5 part.
Further, the antirust agent is one or more of lauric acid, stearic acid, sodium nitrite, potassium dichromate, oleylamine oleate, cyclohexylamine stearate, barium petroleum sulfonate and sodium petroleum sulfonate, and sodium nitrite is preferred. The antirust agent is preferably 0.1-0.5 part.
Further, the pH regulator is one or more of ethylenediamine pentaacetic acid, diethylenetriamine pentaacetic acid, triethylenetriamine pentaacetic acid, N-dimethylaniline and monoethanolamine, and preferably monoethanolamine. The pH regulator is preferably 10-15 parts.
The invention also discloses a preparation method of the environment-friendly suspending agent based on sapphire grinding, which comprises the following steps:
step 1: weighing the components according to the proportion;
and 2, step: adding all the components except the thickening agent into a container, heating to 25-40 ℃, continuously stirring (rotating speed of 100-500 r/min) until all the materials are dissolved, and adding the thickening agent while keeping stirring; and then, the stirring speed is increased (the rotating speed is 300r/min-2000r/min), the mixture is stirred for 20-60min until the mixture is uniform and transparent, and the environment-friendly suspending agent based on sapphire grinding is prepared.
The invention also discloses application of the environment-friendly suspending agent based on sapphire grinding in the field of sapphire wafer grinding or silicon wafer grinding.
Further, the environmentally friendly suspension agent based on sapphire grinding is used for sapphire wafer grinding, and comprises the following steps:
a, step a: preparing an environment-friendly suspending agent based on sapphire grinding into a working solution by using ultrapure water; the mass ratio of the environment-friendly suspending agent for sapphire grinding to the ultrapure water in the working solution is 25-40: 60-75;
step b: and adding grinding sand accounting for 10-40% of the working solution by mass into the working solution, and stirring for 10-30min for grinding the sapphire wafer.
Further, the sapphire wafer grinding process in the step b is as follows:
grinding time: 10-30 min;
grinding rotating speed: 20-80 r/min;
flow rate: 10-50 mL/min;
grinding pressure: 10-20 kg;
plate temperature: 20-40 ℃.
Compared with the prior art, the environment-friendly suspending agent based on sapphire grinding, the preparation method and the application thereof have the following advantages:
1) the chelating agent polydopamine is generated by chelating agent monomer dopamine hydrochloride and chelating accelerator trihydroxymethyl aminomethane. The advantages are as follows: firstly, the polydopamine is electronegative, generates electrostatic repulsion phenomenon with the thickening agent, and enhances the suspension property. Secondly, the surface of the polydopamine is rich in hydroxyl groups and amino groups and has strong hydrophilicity. The polydopamine has a chelating effect, can be used as an intermediate bridge of a solvent and a water phase, effectively enhances the solubility of substances such as a thickening agent and the like in water, and improves the dispersion degree and stability. The suspension property is improved, so that the agglomeration phenomenon of large-size particles in the grinding fluid can be reduced, and the scratch problem of sapphire wafers or silicon wafers is reduced; finally, polydopamine with Al 3+The chelating effect is achieved, the surface of the cut sapphire can be conveniently cleaned, and the used material is environment-friendly and cannot influence the environment.
2) The surface quality of the sapphire wafer can be improved by the poly-dopamine adopted by the invention because when the grinding fluid (suspending agent + B)4C + water), the poly-dopamine can rapidly release the hydroxyl of the poly-dopamine to adjust the pH value, so that the pH value of the grinding liquid is stable, the grinding rate of the sapphire surface is uniform, better surface quality is obtained, and compared with the traditional process, the surface flatness of the sapphire wafer can be obviously improved and the surface roughness is greatly reduced.
3) Based on the action mechanism of steric hindrance, by adding an anionic polymer dispersant, such as sodium polyacrylate, the negative charge on the surface of the abrasive particles is increased, the repulsion force is increased, steric hindrance is formed among the particles to prevent the abrasive particles from agglomerating, and the steric hindrance and strong adsorption substances such as hydroxyl and amino of polydopamine are cooperated to obtain the sapphire wafer with higher grinding rate and better surface quality.
4) The polydopamine adopted by the invention can effectively improve the removal effect on sapphire wafers or silicon wafers for two reasons, namely, the polydopamine has strong hydrolysis effect on sapphire, and the polydopamine suspension of the invention The agent is hydrophilic substance, such as polydopamine and thickener, for B4And C, modifying, compared with the hydrophobic modified fumed silica in the prior art, the scraps are not easy to adhere to the surface of the polished wafer, are easy to combine with water, are convenient to clean and reduce the scratch of the wafer.
In conclusion, the suspending agent has very good application prospect and large-scale industrial popularization potential in the field of sapphire grinding.
Drawings
FIG. 1 shows polydopamine hydrochloride in O2A schematic diagram of polydopamine generated by self-polymerization under the condition.
FIG. 2 is a 100-fold microscopic image of a sapphire wafer after grinding using the suspending agent of example 3.
FIG. 3 is a 100-fold microscopic picture of a sapphire wafer after grinding using the suspending agent of comparative example 2.
As is clear from the figure, the width of the scratches on the wafer surface after the grinding of the comparative example is wider, while the scratches on the wafer surface after the grinding of the example suspending agent are extremely narrower, which shows that the quality of the sapphire surface after the grinding of the example suspending agent prepared by the invention is better, and is greatly improved compared with the comparative example.
Fig. 4 is a sapphire wafer roughness test site diagram.
Detailed Description
The invention is further illustrated by the following examples:
Examples 1 to 10
The components and formulation ratios of the environmentally friendly suspending agents based on sapphire milling of examples 1-10 are shown in table 1. The principle of dopamine hydrochloride reacting with Tris (hydroxymethyl) aminomethane (Tris) to produce polydopamine is shown in fig. 1.
The preparation process of examples 1-10 includes the following steps:
step 1: weighing the components according to the proportion;
step 2: adding all the components except the thickening agent into a container, heating to 30 ℃, continuously stirring (rotating speed of 100r/min) until all the materials are dissolved, and adding the thickening agent while keeping stirring; and then, the stirring speed is increased (the rotating speed is 1000r/min), the mixture is stirred for 50min to be uniform and transparent, and the environment-friendly suspending agent based on sapphire grinding is prepared.
TABLE 1 Components and compounding ratios of examples 1-10
Comparative examples 1 to 4
The components and proportions of the suspending agents of comparative examples 1 to 4 are shown in Table 2, and the preparation method thereof is the same as that of example 3.
TABLE 2 Components and proportions of suspending agents for comparative examples 1-4
Performance testing
Preparing a grinding fluid: preparing a suspending agent into working solution by using ultrapure water; the mass ratio of the suspending agent to the ultrapure water in the working solution is 1: and 3, adding grinding sand accounting for 20% of the working solution by mass into the working solution, and stirring for 30min to prepare the grinding solution. The results of the performance tests of the suspending agent-containing slurry are shown in table 3:
Table 3 results of performance tests of examples 1 to 10 and comparative examples 1 to 4
Through comparison, the suspending agents of examples 1-10 of the invention have better effect than those of comparative examples 1-4, and the suspending agents of examples 1-10 have much better stability and suspensibility than those of comparative examples 1-4; compared with a comparative example, the grinding liquid containing the suspending agent can effectively reduce the surface roughness and the surface scratch width of the sapphire wafer and increase the removal rate.
Wherein:
the performance 1 removal rate was tested as follows:
mass m before wafer grinding1(g) Mass m after grinding2(g) The grinding time is t(s), and rho is the density of the sapphire wafer (g/cm)3) And s is the sapphire area (cm)2) The formula is as follows:
MRR＝(m1-m2)/ρst
the performance 2 roughness test method comprises the following steps:
grinding the sapphire wafer by using grinding fluid, wherein the grinding time is as follows: 25 min; grinding rotating speed: 80 r/min; flow rate: 40 mL/min; grinding pressure: 18 kg; plate temperature: at 25 ℃.
And cleaning and drying the ground sapphire wafer by using ethanol, carrying out 3 roughness tests on 5 points on the front and back surfaces of the sapphire wafer, and then averaging to determine the roughness of the sapphire wafer. Fig. 4 is a sapphire wafer roughness test site diagram.
The polished wafer was cleaned and observed with a microscope. Example 3 and comparative example 2 sapphire wafers were enlarged by 100-fold microscopic pictures after suspension grinding as shown in fig. 2 and 3, respectively.
adding water and grinding sand (B) to the suspending agent4C) Then, the corresponding proportions are: suspending agent water and grinding sand are mixed at a ratio of 1:30:1.6, stirred for 5-15min and then kept stand, and the suspension time of the grinding sand is observed and recorded.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. The environment-friendly suspending agent based on sapphire grinding is characterized by comprising the following components in parts by mass:
the chelating agent monomer is dopamine hydrochloride, and the chelating accelerator is trihydroxymethyl aminomethane; the chelating agent is polydopamine generated by reacting dopamine hydrochloride with trihydroxymethyl aminomethane;
The pH regulator is one or more of ethylenediamine pentaacetic acid, diethylenetriamine pentaacetic acid, triethylenetriamine pentaacetic acid, N-dimethylaniline and monoethanolamine.
2. The environmentally friendly suspending agent based on sapphire milling of claim 1, wherein the thickener is one or more of sodium carboxymethylcellulose, hydroxyethylcellulose, sodium caseinate or acacia gum.
3. The environmentally friendly suspending agent based on sapphire milling according to claim 1, wherein the dispersant is one or more selected from the group consisting of vinyl bis stearamide, glycerol monostearate, butyl stearate, ethylene-acrylic acid copolymer, sodium polyacrylate, magnesium stearate and polyethylene wax.
4. The environmentally friendly suspension concentrate based on sapphire milling of claim 1, wherein the surfactant is a cationic surfactant, an anionic surfactant, or a nonionic surfactant.
5. The environmentally friendly suspension concentrate based on sapphire milling of claim 1, wherein the antifoaming agent is one or more of polyoxypropylene glycerol polyether, polyoxypropylene polyoxyethylene glycerol ether, polyoxypropylene polyoxyethylene glycerol polyether ester, and dimethicone and polyether-siloxane copolymer.
6. The environmentally friendly suspension concentrate based on sapphire milling of claim 1, wherein the rust inhibitor is one or more of lauric acid, stearic acid, sodium nitrite, potassium dichromate, octadecylamine oleate, cyclohexylamine stearate, barium petroleum sulfonate, and sodium petroleum sulfonate.
7. The method for preparing the environmentally friendly suspending agent based on sapphire grinding as described in any one of claims 1-6, comprising the following steps:
step 1: weighing the components according to the proportion;
step 2: adding all the components except the thickening agent into a container, heating to 25-40 ℃, continuously stirring until all the materials are dissolved, and adding the thickening agent while keeping stirring; and then, the stirring speed is increased, the mixture is stirred for 20-60min to be uniform and transparent, and the environment-friendly suspending agent based on sapphire grinding is prepared.
8. Use of the environmentally friendly suspension concentrate based on sapphire milling of any one of claims 1-6 in the field of sapphire wafer milling or silicon wafer milling.
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| CN115044299B (en) * | 2022-07-04 | 2023-11-17 | 浙江奥首材料科技有限公司 | Water-soluble high-specific-gravity large-size abrasive suspension auxiliary agent, preparation method and application thereof, and grinding fluid containing water-soluble high-specific-gravity large-size abrasive suspension auxiliary agent |
| CN115181545B (en) * | 2022-07-22 | 2023-12-05 | 福建省佑达环保材料有限公司 | Suspension for semiconductor manufacturing process |
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| CN105086837B (en) * | 2015-09-18 | 2017-10-17 | 蓝思科技（长沙）有限公司 | A kind of sapphire Liquid diamond |
| CN107189693B (en) * | 2017-05-12 | 2021-12-28 | 江南大学 | Polishing solution for chemical mechanical polishing of A-direction sapphire and preparation method thereof |
| CN109096990A (en) * | 2017-06-21 | 2018-12-28 | 圣戈本陶瓷及塑料股份有限公司 | The modified abrasive grains in surface, abrasive article with and forming method thereof |
| US20200254136A1 (en) * | 2017-10-02 | 2020-08-13 | Aleo Bme, Inc. | Water-based tissue adhesives |
| CN108642496A (en) * | 2018-04-20 | 2018-10-12 | 吴伟华 | A kind of preparation method of stainless steel products special solid polishing agent |
| CN110669439A (en) * | 2019-09-12 | 2020-01-10 | 江苏吉星新材料有限公司 | Coarse grinding fluid for sapphire grinding |
| CN111098237A (en) * | 2019-12-24 | 2020-05-05 | 常州万博金属构件厂 | Preparation method of non-adhesive polished wafer |
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