CN105462504A - C-direction sapphire polishing solution and preparation method thereof - Google Patents
C-direction sapphire polishing solution and preparation method thereof Download PDFInfo
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- CN105462504A CN105462504A CN201510919953.2A CN201510919953A CN105462504A CN 105462504 A CN105462504 A CN 105462504A CN 201510919953 A CN201510919953 A CN 201510919953A CN 105462504 A CN105462504 A CN 105462504A
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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
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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Abstract
The invention firstly aims at providing a C-direction sapphire polishing solution. The C-direction sapphire polishing solution comprises silica sol, an auxiliary polishing agent, a complexing agent, oxidant, surfactant, humectant, a pH adjusting agent and water. The C-direction sapphire polishing solution has the advantages that the wafer surface is oxidized into a soft oxidation layer through the oxidant; the soft oxidation layer formed on the wafer surface is removed through the silica sol, and polishing efficiency is improved; roughness of the wafer surface is lowered through the auxiliary polishing agent; contamination of impurity irons is reduced through the complexing agent; the surfactant facilitates cleaning and removal; crystallization generated in the polishing process is greatly reduced through the humectant; the PH value of a polishing solution system and chemical action in the polishing process are adjusted through the pH adjusting agent. The invention secondly aims at providing a preparation method of the C-direction sapphire polishing solution. The C-direction sapphire polishing solution and the preparation method thereof have the advantages that the process steps are simple, the process parameters are easy to control, and the C-direction sapphire polishing solution and the preparation method thereof are suitable for mass production.
Description
Technical field
The present invention relates to Sapphire Polishing Technology field, particularly a kind of C is to sapphire polishing liquid and preparation method thereof.
Background technology
Sapphire, also known as white stone, be artificial single crystal's material, main component is Al
2o
3, be hexagonal crystallographic texture.Sapphire extreme hardness (Mohs' hardness 9.2 ~ 9.4), and sapphire has the performances such as high temperature resistant, wear-resistant, anticorrosive and transmission region is wide, is a kind of optical function material of high-quality.
Not only CMP (chemically machinery polished) the technological synthesis double dominant of chemical rightenning and mechanical polishing, can obtain perfect surface while can obtaining high polishing speed.In current CMP polishing fluid, 60-95% is water, and freight charges are high, and polishing fluid is short for work-ing life.Our company's early-stage Study goes out a kind of C to sapphire polishing liquid (application number is 201510245942.0), specifically comprises the component of following weight part: silicon sol 90-97 part, brightening agent 0.01-2 part, active dispersing agents 0.01-2 part, oxygenant 0.01-1 part, synergistic agent 0.01-2 part and deionized water 0-5 part.This kind of C is high to sapphire polishing liquid thousand consumptions, and in polishing process, crystallization is comparatively serious, increases the workload of producing line, reduces production efficiency, also affect sapphire quality to a certain extent.
Therefore, few and polishing fluid obtaining good product performance of crystallization in a kind of polishing process and preparation method thereof is badly in need of finding in industry to overcome the deficiencies in the prior art.
Summary of the invention
The first object of the present invention is to provide a kind of C to sapphire polishing liquid, comprises following component with its raw material of weight parts: silicon sol 90-95 part, help rumbling compound 0.01-2 part, complexing agent 0.5-1 part, oxygenant 0.01-1 part, tensio-active agent 0.5-1 part, wetting Agent for Printing Inks 3-6 part, pH adjusting agent 0.5-2 part and water 1.0-5.0 part.
Preferred in above technical scheme, the particle diameter of described silicon sol is 50-80 nanometer, and its concentration is 35%-45%; The colloid proterties of described silicon sol is spherical, and its Mohs' hardness is 7.
Preferred in above technical scheme, described in help rumbling compound to be at least one in sodium-chlor, Repone K, sodium iodide, potassiumiodide, Sodium Fluoride and Potassium monofluoride.
Preferred in above technical scheme, described complexing agent is at least one in diethanolamine, diethylenetriamine, quadrol, hydroxyethylethylene diamine and EDETATE SODIUM.
Preferred in above technical scheme, described oxygenant is at least one in clorox, SPC-D, Sodium peroxoborate, Peracetic Acid and potassium per(oxy)borate.
Preferred in above technical scheme, described tensio-active agent is at least one in polyoxyethylene octylphenol ether, alkylphenol polyoxyethylene, sodium polyacrylate and Sodium dodecylbenzene sulfonate.
Preferred in above technical scheme, described wetting Agent for Printing Inks is at least one in glycerol, Xylitol, sorbyl alcohol, polyvinyl alcohol, Walocel MT 20.000PV and Natvosol.
Preferred in above technical scheme, described PH conditioning agent is at least one in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH and methyl triethylammonium hydroxide.
C of the present invention to sapphire polishing liquid, wherein: the softer zone of oxidation that wafer surface can be formed because of chemical action by silicon sol is ground off by machinery to be removed with adsorption; Help rumbling compound to improve quality transfering rate, strengthen C to the average rate of cutting of sapphire surfacing, reduce plane of crystal roughness; Complexing agent is mainly used in the metal ion in the whole polishing system of complexing, reduces the pollution of foreign ion; Wafer surface can be oxidized to softer zone of oxidation by oxygenant in polishing process, is conducive to abrasive grains in polishing fluid of the present invention and, to the worn effect of wafer, improves polishing efficiency; Utilize the dispersion stabilization of silicon sol in tensio-active agent raising system, and form physical adsorption with reaction product, be convenient to cleaning and remove; Utilize wetting Agent for Printing Inks to reduce Yin Wendu in CMP (Chemical Mechanical Polishing) process to raise and the moisture evaporation that causes, and then greatly reduce the crystallization in polishing process; PH adjusting agent adopts the organic bases of not metal ion to have triple role: a, can reduce the pollution of metal ion to wafer; B, for regulating polishing fluid system pH value, make sol system more stable; C, the chemical action that can strengthen in CMP (Chemical Mechanical Polishing) process, improve chemically machinery polished efficiency.
Apply C of the present invention and carry out polishing to sapphire polishing liquid, the ratio of being watered is 1:1, thousand sapphire sheet consumptions are 50-54 kilogram, clear frequency is 28-32 days, surfaceness is less than 0.3nm, average apparent yield is 82%-85%, and average rate of cutting is 2.0-2.3 μm/h, meets C requirement for rate of cutting and yield in sapphire glossing processing procedure completely.
The second object of the present invention is to provide a kind of above-mentioned C to the preparation method of sapphire polishing liquid, comprises the following steps:
Step one: silicon sol is carried out twice filtration by 500 order deep bed filter, removes impurity wherein;
Concentration after above-mentioned filtration is that the silicon sol of 35%-45% adds with the flow velocity of 0.1-0.4L/min while stirring and helps rumbling compound and complexing agent by step 2: control the rotating speed of retort between 60-120rpm, and every 5min reversion once;
Step 3: continue to add oxygenant and tensio-active agent and wetting Agent for Printing Inks with the flow velocity of 0.1-0.4L/min in retort, and regulate the pH value of mixed solution to 9-10 by pH adjusting agent, obtain C to sapphire polishing liquid.
Preparation method of the present invention has that processing step is simplified, processing parameter easily controls and the advantage of applicable scale operation.
Except object described above, feature and advantage, the present invention also has other object, feature and advantage.Below with reference to specific embodiment, the present invention is further detailed explanation.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in detail, but the multitude of different ways that the present invention can limit according to claim and cover is implemented.
Embodiment 1:
A kind of novel sapphire C, to polishing fluid, is made up of the raw material of following parts by weight:
Silicon sol 92 parts, help rumbling compound 0.3 part, complexing agent 0.5 part, 0.08 part, oxygenant, 0.5 part, tensio-active agent, wetting Agent for Printing Inks 5 parts, pH adjusting agent 0.5 part and deionized water 1.62 parts.
The particle diameter of described silicon sol is 50nm, and its concentration is 40%.
The described rumbling compound that helps adopts Repone K, potassiumiodide and Sodium Fluoride obtained according to the mixing of 1:1:1 weight proportion.
Described complexing agent adopts diethylenetriamine and dihydroxy ethyl quadrol to obtain according to the mixing of 2:1 weight proportion.
Described oxygenant adopts clorox, Sodium peroxoborate, Peracetic Acid and potassium per(oxy)borate obtained according to the weight proportion mixing of 1:2:2:1.
Described tensio-active agent adopts polyoxyethylene octylphenol ether, sodium polyacrylate, Sodium dodecylbenzene sulfonate obtained according to the weight proportion mixing of 1:1:2.
Described wetting Agent for Printing Inks adopts glycerol, polyvinyl alcohol, Natvosol obtained according to the weight proportion mixing of 1:1:2.
Above-mentioned C, to the preparation method of sapphire polishing liquid, comprises the following steps:
Step one: silicon sol is carried out twice filtration by 500 order deep bed filter, removes impurity wherein;
Concentration after above-mentioned filtration is that the silicon sol of 35%-45% adds with the flow velocity of 0.1-0.4L/min while stirring and helps rumbling compound and complexing agent by step 2: control the rotating speed of retort between 60-120rpm, and every 5min reversion once;
Step 3: continue to add oxygenant, tensio-active agent and wetting Agent for Printing Inks with the flow velocity of 0.1-0.4L/min in retort, and regulate the pH value of mixed solution to 9-10 by pH adjusting agent, obtain C to sapphire polishing liquid.
Provide the sapphire C for preparing through the embodiment of the present invention 1 data to the average yield of the glass surface after polishing fluid polishing, roughness Ra and average rate of cutting below, the polishing condition of above-mentioned experimentation is as follows:
The two-sided precision polisher of polishing machine: CJ
Polished wafer: C is to sapphire two cun of sheets
Polished wafer sheet number: 105pcs
Polishing pad: urethane fluting damping cloth
Unit polish pressure: 0.24kg
Twin polishing speed ratio: 16.5:33:8.4:4.7
Polishing time: 240min
Polishing fluid flow: 500-800ml/min
After polishing, ultrasonic cleaning, drying are carried out to polishing sapphire wafer, then measure the thickness of wafer.The thickness difference measuring sapphire wafer with thickness tester asks rate of cutting, measures, average and obtain average rate of cutting all polished wafers; With roughness tester, all polished wafers are measured, average and obtain wafer surface roughness.
The results detailed in following table 1, as known from Table 1: when adopting the present embodiment C to carry out polishing to sapphire polishing liquid, crystallization is few, clear frequency becomes one month from an original week, thousand consumptions are necessarily saved, its apparent yield also can reach 85%, and its surfaceness is less than 0.3nm, and product performance are stablized, production cost is lower, pollution-free, easily reclaim.
The service condition of table 1 Application Example 1 gained C to sapphire polishing liquid and the performance of products obtained therefrom
Following examples 2-embodiment 7 adopts the preparation method identical with embodiment 1, and each raw material composition is as shown in table 2, table 3, table 4, table 5, table 6, table 7 and table 8.
Each raw material composition cartogram (in mass fraction) of table 2 embodiment 2-embodiment 7
Table 3 embodiment 2-embodiment 7 adopt the kind and percentage composition cartogram that help rumbling compound
| Parameter embodiment | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Sodium-chlor | 30 | 100 | - | - | - | |
| Repone K | - | 10 | - | - | - | 30 |
| Sodium iodide | 30 | 40 | - | 50 | 10 | 20 |
| Potassiumiodide | 40 | 10 | - | 50 | - | 20 |
| Sodium Fluoride | - | 40 | - | - | 80 | 30 |
| Potassium monofluoride | - | - | - | - | 10 | - |
Table 4 embodiment 2-embodiment 7 adopt kind and the percentage composition cartogram of complexing agent
| Parameter embodiment | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Diethanolamine | 50 | 20 | - | - | - | 10 |
| Diethylenetriamine | - | 80 | - | - | 20 | 10 |
| Quadrol | - | - | 10 | 50 | - | 20 |
| Hydroxyethylethylene diamine | 50 | - | 10 | 50 | - | 20 |
| EDETATE SODIUM | - | - | 80 | - | 80 | 40 |
Table 5 embodiment 2-embodiment 7 adopt kind and the percentage composition cartogram of oxygenant
| Parameter embodiment | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Clorox | - | - | 20 | - | 50 | - |
| SPC-D | - | 10 | 30 | - | - | 70 |
| Sodium peroxoborate | 30 | 50 | - | 50 | 20 | - |
| Peracetic Acid | 70 | - | 50 | 50 | - | 20 |
| Potassium per(oxy)borate | - | 40 | - | - | 30 | 10 |
Table 6 embodiment 2-embodiment 7 adopt kind and the percentage composition cartogram of tensio-active agent
Table 7 embodiment 2-embodiment 7 adopt kind and the percentage composition cartogram of wetting Agent for Printing Inks
| Parameter embodiment | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Glycerol | - | 50 | - | 15 | - | 35 |
| Xylitol | 60 | - | 10 | 45 | 20 | - |
| Sorbyl alcohol | 10 | 40 | - | - | - | |
| Polyvinyl alcohol | 10 | - | 20 | - | 45 | 20 |
| Walocel MT 20.000PV | 10 | 30 | ||||
| Natvosol | 10 | 50 | 30 | 40 | 35 | 15 |
Table 8 embodiment 2-embodiment 7 adopt kind and the percentage composition cartogram of pH adjusting agent
| Parameter embodiment | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Tetramethylammonium hydroxide | - | 50 | - | - | 30 | - |
| Tetraethyl ammonium hydroxide | - | - | 40 | - | 50 | 50 |
| TPAOH | 45 | 50 | - | 50 | 20 | - |
| TBAH | 25 | - | 60 | 50 | - | 22 |
| Methyl triethylammonium hydroxide | 30 | - | - | - | - | 28 |
Embodiment 2-embodiment 7 adopts polishing process its correlation circumstance identical with embodiment 1 to refer to table 9.
The service condition of table 9 application implementation 2-embodiment 7C to sapphire polishing liquid and the performance of products obtained therefrom
Consolidated statement 1 and table 9 can obtain: adopt C of the present invention to carry out polishing to sapphire polishing liquid, the ratio of being watered is 1:1, thousand sapphire sheet consumptions are 52 kilograms, and clear frequency is 28-32 days, and surfaceness is less than 0.3nm, average apparent yield is 82%-85%, average rate of cutting is 2.0-2.3 μm/h, and meet C requirement for rate of cutting and yield in sapphire glossing processing procedure completely, product performance are stablized, production cost is lower, pollution-free, easily reclaim.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a C is to sapphire polishing liquid, it is characterized in that, comprise following component with its raw material of weight parts: silicon sol 90-95 part, help rumbling compound 0.2-2 part, complexing agent 0.5-1 part, oxygenant 0.08-1 part, tensio-active agent 0.5-1 part, wetting Agent for Printing Inks 3-6 part, pH adjusting agent 0.5-2 part and water 1.0-3.2 part.
2. C according to claim 1 is to sapphire polishing liquid, it is characterized in that, the particle diameter of described silicon sol is 50-80 nanometer, and its concentration is 35%-45%; The colloid proterties of described silicon sol is spherical, and its Mohs' hardness is 7.
3. C according to claim 1 is to sapphire polishing liquid, it is characterized in that, described in help rumbling compound to be at least one in sodium-chlor, Repone K, sodium iodide, potassiumiodide, Sodium Fluoride and Potassium monofluoride.
4. C according to claim 1 is to sapphire polishing liquid, it is characterized in that, described complexing agent is at least one in diethanolamine, diethylenetriamine, quadrol, hydroxyethylethylene diamine and EDETATE SODIUM.
5. C according to claim 1 is to sapphire polishing liquid, it is characterized in that, described oxygenant is at least one in clorox, SPC-D, Sodium peroxoborate, Peracetic Acid and potassium per(oxy)borate.
6. C according to claim 1 is to sapphire polishing liquid, it is characterized in that, described tensio-active agent is at least one in polyoxyethylene octylphenol ether, alkylphenol polyoxyethylene, sodium polyacrylate and Sodium dodecylbenzene sulfonate.
7. C according to claim 1 is to sapphire polishing liquid, it is characterized in that, described wetting Agent for Printing Inks is at least one in glycerol, Xylitol, sorbyl alcohol, polyvinyl alcohol, Walocel MT 20.000PV and Natvosol.
8. C according to claim 1 is to sapphire polishing liquid, it is characterized in that, described PH conditioning agent is at least one in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH and methyl triethylammonium hydroxide.
9. the C as described in claim 1-8 any one, to a preparation method for sapphire polishing liquid, is characterized in that: comprise the following steps:
Step one: silicon sol is carried out twice filtration by 500 order deep bed filter, removes impurity wherein;
Concentration after above-mentioned filtration is that the silicon sol of 35%-45% adds with the flow velocity of 0.1-0.4L/min while stirring and helps rumbling compound and complexing agent by step 2: control the rotating speed of retort between 60-120rpm, and every 5min reversion once;
Step 3: continue to add oxygenant, tensio-active agent and wetting Agent for Printing Inks with the flow velocity of 0.1-0.4L/min in retort, and regulate the pH value of mixed solution to 9-10 by pH adjusting agent, obtain C to sapphire polishing liquid.
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| CN114015360A (en) * | 2021-11-23 | 2022-02-08 | 浙江奥首材料科技有限公司 | Water-based full-suspension diamond polishing solution for sapphire, preparation method and application thereof |
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