CN109913133B - Efficient high-quality chemical mechanical polishing solution for yttrium aluminum garnet crystals - Google Patents
Efficient high-quality chemical mechanical polishing solution for yttrium aluminum garnet crystals Download PDFInfo
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- CN109913133B CN109913133B CN201910250862.2A CN201910250862A CN109913133B CN 109913133 B CN109913133 B CN 109913133B CN 201910250862 A CN201910250862 A CN 201910250862A CN 109913133 B CN109913133 B CN 109913133B
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- chemical mechanical
- mechanical polishing
- polishing solution
- aluminum garnet
- yttrium aluminum
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- 238000005498 polishing Methods 0.000 title claims abstract description 83
- 239000000126 substance Substances 0.000 title claims abstract description 40
- 239000013078 crystal Substances 0.000 title claims abstract description 32
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 title claims abstract description 23
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 14
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 14
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 14
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 13
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims 1
- 230000010355 oscillation Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 10
- 238000012545 processing Methods 0.000 abstract description 7
- 239000000243 solution Substances 0.000 description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
An efficient high-quality chemical mechanical polishing solution for yttrium aluminum garnet crystals, belonging to the field of ultraprecise processing of hard and brittle materials. At room temperature, adding the abrasive zirconia, the sodium silicate and the magnesia into deionized water respectively, and oscillating in ultrasonic equipment for 10 minutes to obtain the chemical mechanical polishing solution. In the chemical mechanical polishing solution, the concentration of zirconium oxide is 0.02-0.12 g/ml, the particle size is 0.02-0.20 mu m, the concentration of sodium silicate is 0.03-0.15 g/ml, and the concentration of magnesium oxide is 1-5 g/L. The yttrium aluminum garnet crystal is polished by the polishing solution, and the yttrium aluminum garnet crystal can obtain higher surface quality and polishing material removal rate.
Description
Technical Field
The invention belongs to the field of ultra-precision processing of hard and brittle materials, relates to preparation of a chemical mechanical polishing solution for a crystal material, and particularly relates to preparation of a chemical mechanical polishing solution for an yttrium aluminum garnet crystal.
Background
With the development of society, lasers have been widely used in various fields such as manufacturing, medical treatment, national defense and the like. The yttrium aluminum garnet crystal is the laser crystal with the most wide application because of the better physical and chemical properties. In order to obtain a better laser beam and a larger laser threshold, the surface and sub-surface quality of the laser wafer plays a crucial role. Defects and damage on the wafer surface can cause laser scattering in the propagation process to cause local energy concentration, and the performance of the laser is greatly reduced.
At present, the processing mode of the yttrium aluminum garnet crystal mainly adopts superfine alumina hard abrasive for mechanical polishing and silica sol for chemical mechanical polishing. Patent CN 103059738A adopts nitric acid, water and emulsified corundum mixed solution to polish YAG crystal, but because aluminium oxide hardness is high, produce dislocation, fine mar and great subsurface damage easily after the crystal processing, the nitric acid seriously corrodes equipment simultaneously, and is great to environmental pollution, and the waste liquid treatment cost is high. The patent CN 108838745A adopts a mixed aqueous solution of zirconium oxide and sodium hydroxide to carry out chemical mechanical polishing on YAG crystals, but the removal rate of the material is low, only 1.99nm/min, and the surface quality is still to be improved. Therefore, the problems of the conventional polishing solutions include: (1) poor surface quality; (2) the removal efficiency is low; (3) it is expensive. The chemical mechanical polishing process is used as the only processing technology capable of realizing global planarization, and the research on novel high-efficiency high-quality chemical mechanical polishing solution is an effective way for solving the problems.
Disclosure of Invention
In order to solve the problems of low chemical mechanical polishing removal rate, limited polishing quality and the like of yttrium aluminum garnet crystals, the invention discloses a novel chemical mechanical polishing solution which comprises deionized water, zirconia abrasive particles, sodium silicate and magnesium oxide. Unlike CN 108838745A, which uses sodium hydroxide as corrosive agent to remove material, the invention uses sodium silicate and magnesium oxide as chemical reaction reagent, and generates uniform softening layer on YAG crystal surface by the action of sodium silicate and magnesium oxide, so as to achieve the balance of chemical action and mechanical action, and the polishing performance is far higher than the polishing effect, and is also far higher than the traditional polishing solution.
The technical scheme adopted by the invention is as follows:
an efficient high-quality chemical mechanical polishing solution for yttrium aluminum garnet crystals is prepared by respectively adding abrasive materials of zirconium oxide, sodium silicate and magnesium oxide into deionized water at room temperature, and oscillating in ultrasonic equipment for 10 minutes to obtain the chemical mechanical polishing solution. In the chemical mechanical polishing solution, the concentration of zirconium oxide is 0.02-0.12 g/ml, the particle size is 0.02-0.20 mu m, the concentration of sodium silicate is 0.03-0.15 g/ml, and the concentration of magnesium oxide is 1-5 g/L.
A high-efficiency high-quality chemical mechanical polishing method of yttrium aluminum garnet crystals comprises the following steps:
firstly, preparing chemical mechanical polishing solution;
at room temperature, adding sodium silicate, magnesium oxide and zirconium oxide as abrasive materials into deionized water respectively, and oscillating in ultrasonic equipment for 10 minutes to obtain the chemical mechanical polishing solution.
Secondly, using the IC1000 polishing pad as a polishing pad for chemical mechanical polishing to trim the polishing pad;
and thirdly, carrying out chemical mechanical polishing on the yttrium aluminum garnet crystal to reach a material removal rate of 34nm/min, and obtaining the YAG crystal surface with the surface roughness of 0.0755nm after processing.
The invention has the following effects and benefits: the novel chemical mechanical polishing solution is adopted to polish the yttrium aluminum garnet crystal, and 1) compared with the traditional polishing solution, the surface roughness of the crystal is greatly reduced, and the defects such as dislocation, scratch, sub-surface damage and the like are greatly reduced; 2) the material removal rate can reach 3 times of that of the traditional chemical mechanical polishing solution under the same process condition; 3) the novel polishing solution is low in cost, does not need a special process for preparation, and does not cause environmental pollution to all components.
Drawings
FIG. 1 is a TEM image of the distribution of abrasive grains in silica sol of a conventional polishing solution;
FIG. 2 is a TEM image of the distribution of zirconia abrasive grains in the novel polishing solution;
FIG. 3 is an atomic force microscope picture of the surface of a yttrium aluminum garnet crystal polished by a conventional silica sol polishing solution;
FIG. 4 is an atomic force microscope photograph of the surface of a yttrium aluminum garnet crystal polished by the novel chemical mechanical polishing solution;
FIG. 5 is a comparison of polishing removal rate and polishing quality between a conventional CMP liquid and a novel CMP liquid.
Detailed Description
The invention aims to improve the surface quality of the polished yttrium aluminum garnet crystal and the removal rate of a chemical mechanical polishing material, explores the influence of different components on the polishing effect, and finally obtains the chemical mechanical polishing solution with excellent performance by optimizing the proportion of different components in the polishing solution. The method specifically comprises the following steps:
1) the zirconium oxide with the grain diameter of 80nm is determined to be selected as the polishing liquid abrasive, and the dispersed grain diameter of the zirconium oxide in the polishing liquid abrasive is shown in figure 1. Sodium silicate and magnesium oxide as chemical reagents, at concentrations of 0.05g/ml and 3g/L, respectively.
2) An aqueous solution containing 8% of zirconia was prepared as polishing solution 1, and a mixed aqueous solution containing 8% of zirconia and 5% of sodium silicate was prepared as polishing solution 2. And respectively polishing the yttrium aluminum garnet wafer subjected to the same grinding pretreatment for 2 hours by using polishing solutions 1 and 2. The surface topography of the polished yttrium aluminum garnet wafer is shown in fig. 2. It can be seen that the yttrium aluminum garnet crystal polished by the polishing solution 2 has a flat surface and no pits, so the sodium silicate has a better acceleration effect on the polishing of the yttrium aluminum garnet crystal.
3) The chemical mechanical polishing removal rate of the yttrium aluminum garnet crystal was measured by changing the concentration of the additive magnesium oxide in the polishing liquid 2. The measurement results are shown in fig. 3. It can be seen that magnesium oxide promotes the polishing removal rate in a certain range, and the polishing removal rate is highest when the concentration is 3 g/L.
4) A conventional commercial silica sol polishing solution was prepared, and the silica sol concentration was 10% as polishing solution 3. Preparing 0.05g/ml sodium silicate, 0.08g/ml 80nm zirconium oxide and 3g/L magnesium oxide aqueous solution, and ultrasonically oscillating for 10min to obtain polishing solution 4.
2) IC1000 was selected as a polishing pad for chemical mechanical polishing, and the polishing pad was dressed by a diamond dresser.
3) And carrying out a chemical mechanical polishing test on YAG crystals by adopting polishing solutions 3 and 4, wherein the polishing pressure is 0.2Mpa, the rotating speed of a polishing disc is 80r/min, and the flow of the polishing solution is 7 ml/min.
Fig. 4 is an afm profile of the polishing solution 3 after polishing, and fig. 5 is an afm profile of the polishing solution 4 after polishing. FIG. 5 is a comparison of polishing performance data for slurries 3 and 4.
The chemical mechanical polishing solution 4 prepared by the method is used for carrying out a chemical mechanical polishing experiment on an IC1000 polishing pad according to specified process parameters, the material removal rate is 34nm/min, and the YAG crystal surface with the surface roughness of 0.0755nm can be obtained after processing. The material removal rate of the process method is 3 times of that of the traditional chemical mechanical polishing, and simultaneously, higher crystal surface quality is obtained.
Claims (2)
1. A high-efficiency high-quality chemical mechanical polishing method for yttrium aluminum garnet crystals is characterized in that the used chemical mechanical polishing solution is as follows: respectively adding abrasive zirconium oxide, sodium silicate and magnesium oxide into deionized water at room temperature, and performing ultrasonic oscillation to obtain a chemical mechanical polishing solution; in the chemical mechanical polishing solution, the concentration of zirconium oxide is 0.02-0.12 g/ml, the particle size is 0.02-0.20 mu m, the concentration of sodium silicate is 0.03-0.15 g/ml, and the concentration of magnesium oxide is 1-5 g/L; and carrying out chemical mechanical polishing on the yttrium aluminum garnet crystal by adopting the chemical mechanical polishing solution.
2. The method of claim 1, wherein the ultrasonic agitation is performed for 10 minutes.
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| CN110358454A (en) * | 2019-07-20 | 2019-10-22 | 大连理工大学 | A kind of general chemistry machine polishing liquor |
| CN113480942B (en) * | 2021-08-06 | 2022-06-07 | 大连理工大学 | Polycrystalline YAG ceramic chemical mechanical polishing solution |
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| CN108559407A (en) * | 2018-06-25 | 2018-09-21 | 安徽全兆光学科技有限公司 | A kind of optics sapphire lapping liquid |
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| US6705926B2 (en) * | 2001-10-24 | 2004-03-16 | Cabot Microelectronics Corporation | Boron-containing polishing system and method |
| GB2478250B (en) * | 2008-12-22 | 2014-09-03 | Kao Corp | Polishing liquid composition for magnetic-disk substrate |
| CN104400624B (en) * | 2014-10-20 | 2016-11-23 | 南京航空航天大学 | The processing method of concretion abrasive chemically mechanical polishing copper |
| CN106479371A (en) * | 2016-08-15 | 2017-03-08 | 惠州市米特仑科技有限公司 | A kind of high precision composite polishing liquid and preparation method thereof |
| CN108838745B (en) * | 2018-06-27 | 2019-08-13 | 大连理工大学 | A kind of efficient chemical mechanical polishing method of yag crystal |
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| CN108559407A (en) * | 2018-06-25 | 2018-09-21 | 安徽全兆光学科技有限公司 | A kind of optics sapphire lapping liquid |
Non-Patent Citations (1)
| Title |
|---|
| 《Preparation of MgO doped colloidal SiO2 abrasive and their chemical mechanical polishing performance on c-, r- and a-plane sapphire substrate》;Da Yin et al.;《Ceramics International》;20180815;第44卷(第12期);第14631-14637页 * |
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