CN113583573A - Polishing solution for germanium crystal and preparation method thereof - Google Patents
Polishing solution for germanium crystal and preparation method thereof Download PDFInfo
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- CN113583573A CN113583573A CN202111030631.4A CN202111030631A CN113583573A CN 113583573 A CN113583573 A CN 113583573A CN 202111030631 A CN202111030631 A CN 202111030631A CN 113583573 A CN113583573 A CN 113583573A
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- polishing
- germanium
- polishing liquid
- germanium crystal
- organic solvent
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- 238000005498 polishing Methods 0.000 title claims abstract description 92
- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 49
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000013078 crystal Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000003960 organic solvent Substances 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 4
- 230000000996 additive effect Effects 0.000 claims abstract description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 36
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical group CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 33
- 229910003460 diamond Inorganic materials 0.000 claims description 13
- 239000010432 diamond Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- 229910052814 silicon oxide Inorganic materials 0.000 claims 1
- 239000003002 pH adjusting agent Substances 0.000 abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract 1
- 239000011344 liquid material Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 9
- 235000012431 wafers Nutrition 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 description 4
- 150000002191 fatty alcohols Chemical class 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001361 White metal Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 125000000373 fatty alcohol group Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010969 white metal Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
本申请提供一种锗晶体用抛光液。所述抛光液按重量计％，主要由下列原料组成：抛光剂：20％～80％；有机溶剂为：10％～50％；pH值调节剂：1％～30％；余量为去离子水。并提供了一种锗晶体用抛光液的制备方法，包括步骤：步骤一，将抛光剂加去离子水在搅拌条件下加入有机溶剂；步骤二，将pH添加剂加入步骤一中，搅拌均匀后得到抛光液。本申请的锗晶体用抛光液不含有氧化剂，不含重金属离子，对环境无污染。抛光后晶片粗糙度较低，不容易起划痕，抛光液化学试剂简单，是理想的抛光液材料。The present application provides a polishing liquid for germanium crystal. The polishing liquid is mainly composed of the following raw materials in % by weight: polishing agent: 20%-80%; organic solvent: 10%-50%; pH adjusting agent: 1%-30%; the balance is deionized water. Also provided is a method for preparing a polishing solution for germanium crystals, comprising the steps of: step 1, adding a polishing agent to deionized water and adding an organic solvent under stirring conditions; step 2, adding a pH additive to step 1, and stirring uniformly to obtain polishing fluid. The polishing liquid for germanium crystal of the present application contains no oxidizing agent, no heavy metal ions, and no pollution to the environment. After polishing, the roughness of the wafer is low, it is not easy to scratch, and the chemical reagent of the polishing liquid is simple, so it is an ideal polishing liquid material.
Description
Technical Field
The invention relates to the technical field of surface processing, in particular to polishing solution for germanium crystals and a preparation method thereof.
Background
Germanium is an off-white metal, glossy and hard, belongs to the carbon family, has obvious non-metallic properties, has stable chemical properties, and does not react with air or water vapor at normal temperature. The content of germanium in the earth crust is about 0.0007%, which is one of the most dispersed elements in the earth crust, and there is almost no more concentrated germanium ore, which is widely used in the fields of electronics, optics, chemical engineering, biomedicine, energy and other high and new technologies. Germanium as an infrared optical material has the advantages of high infrared refractive index, wide infrared transmission band range, small absorption coefficient, low dispersion rate, easiness in processing, flashing, corrosion and the like, and is particularly suitable for thermal imagers, infrared radars and windows, lenses, prisms and optical filters of other infrared optical devices in military industry and major civil use. The infrared optical application field will be the most important growth point of future germanium demand, and represents the future growth direction of germanium. Polishing of germanium wafers in the infrared processing field is an important part of the processing procedure, and directly influences the optical performance of products. However, after polishing, the wafer has high roughness and is easy to scratch, and the polishing efficiency is low due to the complex chemical reagents of the polishing solution, so that the performance of the polishing solution needs to be further improved.
Disclosure of Invention
In view of the problems in the background art, it is an object of the present disclosure to provide a polishing liquid for germanium crystals and a method for preparing the same. The germanium crystal polished by the polishing solution has low wafer roughness, is not easy to scratch and has no pollution to the environment.
In order to achieve the above object, in a first aspect of the present application, there is provided a polishing liquid for germanium crystal, the polishing liquid mainly consisting of the following raw materials by weight: polishing agent: 20 to 80 percent; the organic solvent is: 10% -50%; pH value regulator: 1% -30%; the balance being deionized water.
In some embodiments, the polishing agent is at least one of silica, alumina, diamond dust.
In some embodiments, the polishing agent has a particle size of 0.1 to 5um and a concentration of 0.1 to 20 g/L.
In some embodiments, the organic solvent is propylene glycol.
In some embodiments, the organic solvent is 99% pure.
In some embodiments, the pH adjusting agent is citric acid.
In some embodiments, the pH adjuster is 99% pure.
In a second aspect of the present application, there is provided a method for preparing a polishing liquid for a germanium crystal, comprising the steps of: the method comprises the following steps: adding a polishing agent into deionized water, and adding an organic solvent under the stirring condition; step two: and (4) adding a pH additive into the step one, and uniformly stirring to obtain the polishing solution.
The beneficial effects of this disclosure are as follows:
the polishing solution for the germanium crystal does not contain an oxidant, does not contain heavy metal ions, and does not pollute the environment. The roughness of the polished wafer is low, the wafer is not easy to scratch, and the chemical reagent of the polishing solution is simple, so the polishing solution is an ideal polishing solution material.
Detailed Description
The polishing liquid for germanium crystals according to the first aspect of the present application, which consists essentially of the following raw materials in% by weight, is explained in detail below: polishing agent: 20 to 80 percent; the organic solvent is: 10% -50%; pH value regulator: 1% -30%; the balance being deionized water.
In the polishing solution raw material for germanium crystals according to the first aspect of the present application, a polishing agent plays a role in polishing the surface of the germanium crystals, the content of the polishing agent ranges from 20% to 80%, the surface of the germanium crystals can be scratched by an excessive content of the polishing agent, and mechanical removal can be reduced by an insufficient content of the polishing agent, so that the polishing efficiency is reduced. The content of the organic solvent is 10-50%, the polishing efficiency is reduced when the content of the organic solvent is too high, and the surface of the germanium crystal is scratched when the content of the organic solvent is too low. The content range of the pH value regulator is 1-30%, the excessive content of the pH value regulator can cause the over-strong acidity and alkalinity and excessively corrode the surface of the polished crystal, the excessive content of the pH value regulator has no auxiliary effect on polishing, and the removal rate is reduced.
In some embodiments, the polishing agent is selected from at least one of silica, alumina, diamond dust.
In some embodiments, the polishing agent particle size is 0.1um to 5 um. The removal rate and the polishing efficiency are reduced when the particle size of the polishing agent is too small; the polishing agent with too large particle size can scratch the surface of the germanium crystal and has too deep scratches.
In some embodiments, the polishing agent has a concentration of 0.1g/L to 20 g/L. The concentration of the polishing agent is more than 20g/L, so that the surface of the germanium crystal can be scratched; when the concentration of the polishing agent is less than 0.1g/L, the removal rate is lowered, and the polishing efficiency is lowered.
In some embodiments, the organic solvent is propylene glycol. The propylene glycol can prevent the suspension from precipitating, improve the stability of the polishing solution and disperse the polishing particles.
In some embodiments, the organic solvent and the pH adjusting agent are both 99% pure. When the purity of the organic solvent and the pH regulator is lower than 99%, many impurities exist, and the polishing effect is influenced.
In some embodiments, the pH adjusting agent is citric acid. The citric acid is weak acid, can not cause serious corrosion to the surface of the crystal, and can effectively improve the quality of the polished surface by matching with the polishing solution.
Next, a description will be given of a method for producing a polishing liquid for a germanium crystal according to a second aspect of the present application, for producing the polishing liquid for a germanium crystal according to the second aspect of the present application, comprising the steps of: step one, adding a polishing agent into an organic solvent under the condition of stirring; and step two, adding the pH additive into the step one, and uniformly stirring to obtain the polishing solution.
In the method for preparing a polishing solution for germanium crystals according to the second aspect of the present application, the addition of the organic solvent under stirring in the first step facilitates better dispersion of the polishing agent in the organic solvent.
The present application is further illustrated below with reference to examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present application.
Example 1
The polishing solution for germanium crystals in the embodiment comprises the following raw materials in percentage by weight:
the content of the diamond powder with the granularity of 0.1um and the concentration of 0.1g/L is 80 percent by weight; propylene glycol content of 99% purity is 10% wt; the citric acid content with the purity of 99 percent is 1 percent by weight; the balance of deionized water;
the preparation method of the polishing solution for the germanium crystal comprises the following steps:
step one, adding deionized water into diamond powder, and adding propylene glycol under the condition of stirring; and step two, continuously adding the citric acid with the good proportion, and uniformly stirring to obtain the chemical mechanical polishing solution.
Example 2
The polishing solution for germanium crystals in the embodiment comprises the following raw materials in percentage by weight:
the content of the diamond powder with the granularity of 0.3um and the concentration of 0.5g/L is 40 percent by weight; propylene glycol content of 99% purity is 50% wt; the citric acid content with a purity of 99% is 2% wt; the balance of deionized water;
the preparation method of the polishing solution for the germanium crystal comprises the following steps:
step one, adding deionized water into diamond powder, and adding propylene glycol under the condition of stirring; and step two, continuously adding the citric acid, and uniformly stirring to obtain the chemical mechanical polishing solution.
Example 3
The polishing solution for germanium crystals in the embodiment comprises the following raw materials in percentage by weight:
the content of the diamond powder with the granularity of 5um and the concentration of 20g/L is 20 percent by weight; propylene glycol content of 99% purity is 10% wt; the citric acid content with the purity of 99 percent is 10 percent by weight; the balance of deionized water;
the preparation method of the polishing solution for the germanium crystal comprises the following steps:
adding propylene glycol into abrasive diamond powder under the condition of adding deionized water and stirring; and step two, continuously adding the citric acid with the good proportion, and uniformly stirring to obtain the chemical mechanical polishing solution.
Comparative example 1
The polishing solution for germanium crystals in the embodiment comprises the following raw materials in percentage by weight:
the content of the diamond powder with the granularity of 0.1um and the concentration of 0.1g/L is 80 percent by weight; the content of the fatty alcohol polyoxyethylene ether with the purity of 99 percent is 10 percent by weight; the citric acid content with the purity of 99 percent is 1 percent by weight; the balance of deionized water;
the preparation method of the polishing solution for the germanium crystal comprises the following steps:
adding the fatty alcohol polyoxyethylene ether into the diamond powder under the condition of adding deionized water and stirring; and step two, continuously adding the citric acid with the good proportion, and uniformly stirring to obtain the chemical mechanical polishing solution.
Comparative example 2
The polishing solution for germanium crystals in the embodiment comprises the following raw materials in percentage by weight:
the content of the diamond powder with the granularity of 0.1um and the concentration of 0.1g/L is 80 percent by weight; the content of the fatty alcohol polyoxyethylene ether with the purity of 99 percent is 10 percent by weight; the content of hydrochloric acid with the purity of 99 percent is 1 percent by weight; the balance of deionized water;
the preparation method of the polishing solution for the germanium crystal comprises the following steps:
step one, adding deionized water into diamond powder, and adding propylene glycol under the condition of stirring; and step two, continuously adding the proportioned hydrochloric acid, and after uniformly stirring, reducing the polishing efficiency and increasing the size of surface scratches due to the fact that the mechanical friction action occupies a dominant position because the electrochemical reaction, the oxidation of the surface of the wafer and the etching action are weakened.
The polishing solutions of examples 1-3 and comparative examples 1-2 were used to polish flat germanium single crystal wafers 12.6mm in diameter and 2.3mm in thickness. The results are shown in Table 1.
TABLE 1 test results
| Group of | Surface roughness (Ra, unit nm) |
| Comparative example 1 | 27.216 |
| Comparative example 2 | 25.826 |
| Example 1 | 0.516 |
| Example 2 | 0.402 |
| Example 3 | 0.624 |
From the above results, it can be seen from example 1 and comparative example 1 that when the organic solvent in comparative example 1 was replaced with fatty alcohol polyoxyethylene ether, the surface roughness thereof was much greater than that of example 1. It can be seen from example 1 and comparative example 2 that the surface roughness of the germanium single crystal was much greater than that of example 2 of the present application when the pH adjuster in comparative example 2 was replaced with hydrochloric acid.
Claims (8)
1. The polishing solution for germanium crystals is characterized by mainly comprising the following raw materials in percentage by weight:
20 to 80 percent of polishing agent;
10 to 50 percent of organic solvent;
1 to 30 percent of pH value regulator;
the balance being deionized water.
2. The polishing liquid for a germanium crystal according to claim 1,
the polishing agent is at least one of silicon oxide, aluminum oxide and diamond powder.
3. The polishing liquid for a germanium crystal according to claim 1,
the particle size of the polishing agent is 0.1-5 um, and the concentration is 0.1-20 g/L.
4. The polishing liquid for a germanium crystal according to claim 1,
the organic solvent is propylene glycol.
5. The polishing liquid for a germanium crystal according to claim 1,
the purity of the organic solvent is 99%.
6. The polishing liquid for a germanium crystal according to claim 1,
the pH value regulator is citric acid.
7. The polishing liquid for a germanium crystal according to claim 1,
the purity of the pH value regulator is 99%.
8. A method for preparing a polishing liquid for a germanium crystal, which is used for preparing the polishing liquid for a germanium crystal according to any one of claims 1 to 7, and which comprises the steps of:
the method comprises the following steps: adding a polishing agent into deionized water, and adding an organic solvent under the stirring condition;
step two: and (4) adding a pH additive into the step one, and uniformly stirring to obtain the polishing solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111030631.4A CN113583573A (en) | 2021-09-02 | 2021-09-02 | Polishing solution for germanium crystal and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111030631.4A CN113583573A (en) | 2021-09-02 | 2021-09-02 | Polishing solution for germanium crystal and preparation method thereof |
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| CN113583573A true CN113583573A (en) | 2021-11-02 |
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| CN202111030631.4A Pending CN113583573A (en) | 2021-09-02 | 2021-09-02 | Polishing solution for germanium crystal and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113913116A (en) * | 2021-11-11 | 2022-01-11 | 中国电子科技集团公司第二十六研究所 | Polishing solution for polishing germanium single crystal and germanium single crystal polishing method |
| CN114015361A (en) * | 2021-12-03 | 2022-02-08 | 安徽光智科技有限公司 | A kind of polishing liquid for tellurium dioxide and preparation method thereof |
| CN114106701A (en) * | 2021-12-03 | 2022-03-01 | 安徽光智科技有限公司 | Polishing solution for zinc sulfide and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05177536A (en) * | 1991-10-30 | 1993-07-20 | Sumitomo Electric Ind Ltd | Specular polishing method for cdte wafer |
| CN103525314A (en) * | 2013-10-30 | 2014-01-22 | 湖北三翔超硬材料有限公司 | High-efficiency diamond lubricating cooling polishing solution and preparation method and application thereof |
| CN105505227A (en) * | 2015-12-07 | 2016-04-20 | 青岛唐鹏钢结构工程有限公司 | Metal material polishing agent |
-
2021
- 2021-09-02 CN CN202111030631.4A patent/CN113583573A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05177536A (en) * | 1991-10-30 | 1993-07-20 | Sumitomo Electric Ind Ltd | Specular polishing method for cdte wafer |
| CN103525314A (en) * | 2013-10-30 | 2014-01-22 | 湖北三翔超硬材料有限公司 | High-efficiency diamond lubricating cooling polishing solution and preparation method and application thereof |
| CN105505227A (en) * | 2015-12-07 | 2016-04-20 | 青岛唐鹏钢结构工程有限公司 | Metal material polishing agent |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113913116A (en) * | 2021-11-11 | 2022-01-11 | 中国电子科技集团公司第二十六研究所 | Polishing solution for polishing germanium single crystal and germanium single crystal polishing method |
| CN114015361A (en) * | 2021-12-03 | 2022-02-08 | 安徽光智科技有限公司 | A kind of polishing liquid for tellurium dioxide and preparation method thereof |
| CN114106701A (en) * | 2021-12-03 | 2022-03-01 | 安徽光智科技有限公司 | Polishing solution for zinc sulfide and preparation method thereof |
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Application publication date: 20211102 |