CN113185920A - Chemical mechanical polishing solution for lithium niobate crystal - Google Patents
Chemical mechanical polishing solution for lithium niobate crystal Download PDFInfo
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- CN113185920A CN113185920A CN202110466472.6A CN202110466472A CN113185920A CN 113185920 A CN113185920 A CN 113185920A CN 202110466472 A CN202110466472 A CN 202110466472A CN 113185920 A CN113185920 A CN 113185920A
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- lithium niobate
- polishing solution
- chemical mechanical
- mechanical polishing
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- 238000005498 polishing Methods 0.000 title claims abstract description 46
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000000126 substance Substances 0.000 title claims abstract description 36
- 239000013078 crystal Substances 0.000 title claims abstract description 17
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 27
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 10
- 230000002925 chemical effect Effects 0.000 abstract description 3
- 238000003754 machining Methods 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 abstract description 2
- 239000002344 surface layer Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 230000003746 surface roughness Effects 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 229910003334 KNbO3 Inorganic materials 0.000 description 1
- 229910003327 LiNbO3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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Classifications
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention provides a lithium niobate crystal chemical mechanical polishing solution, and belongs to the technical field of precision/ultraprecision machining. The pH value of the lithium niobate chemical mechanical polishing solution is 9.5-10, and the lithium niobate chemical mechanical polishing solution comprises two parts of solute and solvent. Wherein the solvent is deionized water. The solute comprises the following components in percentage by mass based on 100 percent of the total mass fraction of the solute: 10-20 wt% of silica sol, 1-2 wt% of potassium hydroxide, 0.02-0.05 wt% of surfactant and the balance of pH regulator, and all the substances are uniformly mixed in deionized water by ultrasonic. The chemical mechanical polishing solution provided by the invention has moderate corrosion effect, and can obtain an ultra-smooth and nondestructive lithium niobate surface on the premise of ensuring the chemical effect of the polishing solution; the graphene oxide can promote the surface layer of the workpiece to be oxidized and form a softening layer, so that the polishing efficiency of the surface of the workpiece is accelerated, and the polishing time is shortened.
Description
Technical Field
The invention belongs to the technical field of precision/ultra-precision machining, and relates to a novel polishing solution for chemical mechanical polishing of lithium niobate crystals.
Background
Lithium niobate crystal (molecular formula LiNbO)3LN for short) is a multifunctional material integrating several functions of piezoelectric effect, electrooptical effect, nonlinear optical effect, photorefractive effect, photovoltaic effect and acousto-optic effect into one body. Preparing a high-frequency device by utilizing a piezoelectric effect; preparing high-quality optical waveguide and periodic polarization crystal by using optical performance; realizing light frequency conversion and quantum entanglement state photon generation by utilizing a nonlinear optical effect; holographic storage, a spatial light modulator and the like are realized by utilizing a light refraction effect; the acoustic surface filter is prepared by using acoustic properties. Lithium niobate materials play an important role in different fields, and enjoy the reputation of "optical silicon" in the optoelectronic era.
With the continuous development of the fields of mobile communication technology (5G), integrated photonics, quantum optics and the like, the requirements on the quality of a substrate material are stricter and stricter, particularly the flatness, the surface roughness and the surface morphology. When the surface quality of the lithium niobate material is poor, the lithium niobate sheet has high scattering loss, and the performance of components is influenced. Therefore, higher requirements are put on the polishing technology in the fields of precision and ultra-precision machining. Chemical Mechanical Polishing (CMP) is a process that can achieve a flat, scratch-free, and contaminant-free surface, and utilizes the Chemical action of a Polishing solution and the Mechanical action of abrasive particles to adjust experimental parameters so that the Chemical action and the Mechanical action reach a balance point, thereby obtaining a high-quality material surface with high efficiency and achieving precise and ultra-precise processing.
Patent CN 102010659B proposes a lithium niobate chemical mechanical polishing solution prepared by a negative pressure stirring preparation method, which is convenient for transportation and storage, but the preparation method is performed under a negative pressure state, and the preparation environment is relatively complex. Patent CN 101857775B proposes a lithium niobate chemical mechanical polishing solution prepared by using silica sol of silica as mother liquor, which can realize ultra-precision processing of lithium niobate wafer under corresponding polishing process conditions, but the roughness of the obtained lithium niobate crystal is 0.8574nm, and the lithium niobate crystal still has high scattering loss at this time.
Therefore, there is a need for a polishing solution that can rapidly obtain a low surface roughness, ultra-smooth, and damage-free lithium niobate crystal surface.
Disclosure of Invention
Aiming at the problems of the existing polishing solution, the invention provides a novel lithium niobate chemical mechanical polishing solution which can effectively improve the polishing efficiency while obtaining an ultra-smooth and nondestructive lithium niobate crystal.
The technical scheme adopted by the invention for solving the problems is as follows:
the lithium niobate crystal chemical mechanical polishing solution has the pH value of 9.5-10 and comprises two parts, namely a solute and a solvent.
The solvent is deionized water.
The solute comprises the following components in percentage by mass based on 100 percent of the total mass fraction of the solute: 10-20 wt% of silica sol, 1-2 wt% of potassium hydroxide, 0.02-0.05 wt% of surfactant and a proper amount of pH regulator, and all the substances are uniformly mixed in deionized water by ultrasonic.
Furthermore, the silica sol has a particle size of 20-50nm, and the mass fraction of the silica abrasive in the silica sol is 10-20%.
Further, the potassium hydroxide is used for adjusting the pH value of the polishing solution, and the potassium hydroxide and the lithium niobate react with each other as follows: LiNbO3+KOH→LiOH+KNbO3To generate water-soluble niobate and accelerate the polishing efficiency of lithium niobate.
Furthermore, the surfactant is graphene oxide, and under the composite action of the graphene oxide and other components of the polishing solution, the surfactant and the surface of the lithium niobate crystal are subjected to chemical action, so that the surface of a workpiece is softened, the removal rate of the material is improved, and the surface quality is improved.
Further, the pH regulator comprises phosphoric acid, acetic acid, oxalic acid, citric acid and the like, and the pH regulator not only has the function of regulating the pH, but also can be used as a complexing agent to be present in the polishing solution.
The novel lithium niobate chemical mechanical polishing solution can be prepared according to a conventional method, for example, the components are added into deionized water according to a ratio and a designated sequence of deionized water, silica sol, potassium hydroxide, a pH regulator and graphene oxide, and the polishing solution can be obtained by ultrasonic dispersion for about 30 minutes.
The beneficial effects of the invention are as follows:
the lithium niobate chemical mechanical polishing solution has moderate corrosion effect, and can reach a balance point of mechanical effect and chemical effect on the premise of ensuring the chemical effect of the polishing solution, so that an ultra-smooth and nondestructive lithium niobate surface is obtained.
The graphene oxide in the lithium niobate chemical mechanical polishing solution can promote the surface layer of the workpiece to be oxidized and form a softening layer, and the polishing efficiency of the surface of the workpiece is accelerated.
The lithium niobate chemical mechanical polishing solution disclosed by the invention can reduce the surface roughness to 0.1-0.5 nm under the same experimental conditions, and meanwhile, can shorten the polishing time and improve the polishing efficiency.
Drawings
FIG. 1 is a surface topography map of example 1;
FIG. 2 is a surface topography map of example 2.
Detailed Description
The present invention will be further described with reference to specific embodiments, which are only a part of the embodiments of the present invention and not all embodiments. The specific embodiments and descriptions of the present invention are provided for illustration only and not for the purpose of limiting the scope of the invention.
The prepared lithium niobate chemical mechanical polishing solution is used for a lithium niobate polishing experiment.
The surface roughness of the polished lithium niobate was measured using a white light interferometer manufactured by ZYGO, usa, and the surface morphology of the lithium niobate was observed using an ultra-deep-field microscope of keyence.
The surface roughness after polishing of lithium niobate in the following examples is shown in Table 1
Example 1
The solvent is deionized water.
The solute comprises the following components in percentage by mass based on 100 percent of the total mass fraction of the solute: 10 wt% of silica sol, 2 wt% of potassium hydroxide, 0.02 wt% of surfactant and a proper amount of pH regulator, and all the substances are uniformly mixed in deionized water by ultrasonic.
The lithium niobate chemical mechanical polishing solution described in this embodiment is prepared by the following steps:
adding 10 wt% of silica sol and 2 wt% of potassium hydroxide into deionized water according to the weight ratio for primary stirring;
adding a pH regulator citric acid to regulate the pH to about 10.5;
adding 0.02 wt% of graphene oxide;
continuously adding a pH regulator citric acid to regulate the pH to 10;
and (3) putting the mixed liquid in a water bath, performing ultrasonic treatment for 30 minutes, and stirring until the mixed liquid is uniformly mixed.
Example 2
The solvent is deionized water.
The solute comprises the following components in percentage by mass based on 100 percent of the total mass fraction of the solute: 10 wt% of silica sol, 1 wt% of potassium hydroxide, 0.02 wt% of surfactant and a proper amount of pH regulator, and all the substances are uniformly mixed in deionized water by ultrasonic.
The lithium niobate chemical mechanical polishing solution described in this embodiment is prepared by the following steps:
adding 10 wt% of silica sol and 1 wt% of potassium hydroxide into deionized water according to the weight ratio for primary stirring;
adding a pH regulator citric acid to regulate the pH to about 10;
adding 0.02 wt% of graphene oxide;
continuously adding a pH regulator citric acid to regulate the pH to about 9.5;
and (3) putting the mixed liquid in a water bath, performing ultrasonic treatment for 30 minutes, and stirring until the mixed liquid is uniformly mixed.
Example 3
The solvent is deionized water.
The solute comprises the following components in percentage by mass based on 100 percent of the total mass fraction of the solute: 15 wt% of silica sol, 2 wt% of potassium hydroxide, 0.05 wt% of surfactant and a proper amount of pH regulator, and all the substances are uniformly mixed in deionized water by ultrasonic.
The lithium niobate chemical mechanical polishing solution described in this embodiment is prepared by the following steps:
adding 15 wt% of silica sol and 2 wt% of potassium hydroxide into deionized water according to the weight ratio for preliminary stirring;
adding oxalic acid as pH regulator to regulate pH to about 10.5;
adding 0.05 wt% of graphene oxide;
continuously adding a pH regulator oxalic acid to regulate the pH to 10;
and (3) putting the mixed liquid in a water bath, performing ultrasonic treatment for 30 minutes, and stirring until the mixed liquid is uniformly mixed.
Example 4
The solvent is deionized water.
The solute comprises the following components in percentage by mass based on 100 percent of the total mass fraction of the solute: 20 wt% of silica sol, 1 wt% of potassium hydroxide, 0.05 wt% of surfactant and a proper amount of pH regulator, and all the substances are uniformly mixed in deionized water by ultrasonic.
The lithium niobate chemical mechanical polishing solution described in this embodiment is prepared by the following steps:
adding 20 wt% of silica sol and 1 wt% of potassium hydroxide into deionized water according to the weight ratio for primary stirring;
adding a pH regulator citric acid to regulate the pH to about 10;
adding 0.05 wt% of graphene oxide;
continuously adding a pH regulator citric acid to regulate the pH to 9.7;
and (3) putting the mixed liquid in a water bath, performing ultrasonic treatment for 30 minutes, and stirring until the mixed liquid is uniformly mixed.
Table 1 table of effects of examples
The above-mentioned embodiments only express the embodiments of the present invention, but not should be understood as the limitation of the scope of the invention patent, it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the concept of the present invention, and these all fall into the protection scope of the present invention.
Claims (5)
1. The chemical mechanical polishing solution for the lithium niobate crystal is characterized by having a pH value of 9.5-10 and comprising a solute and a solvent;
the solvent is deionized water;
the solute comprises the following components in percentage by mass based on 100 percent of the total mass fraction of the solute: 10-20 wt% of silica sol, 1-2 wt% of potassium hydroxide, 0.02-0.05 wt% of surfactant and the balance of pH regulator, and all the substances are uniformly mixed in deionized water by ultrasonic.
2. The lithium niobate crystal chemical mechanical polishing solution according to claim 1, wherein the silica abrasive in the silica sol has a particle size of 20 to 50nm, and the mass fraction of the silica abrasive in the silica sol is 10 to 20%.
3. The chemical mechanical polishing solution for lithium niobate crystals according to claim 1 or 2, wherein the surfactant is graphene oxide.
4. The chemical mechanical polishing solution for lithium niobate crystals according to claim 1 or 2, wherein the pH adjusting agent comprises phosphoric acid, acetic acid, oxalic acid or citric acid.
5. The chemical mechanical polishing solution for lithium niobate crystals according to claim 3, wherein the pH regulator comprises phosphoric acid, acetic acid, oxalic acid or citric acid.
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| CN202110466472.6A CN113185920A (en) | 2021-04-28 | 2021-04-28 | Chemical mechanical polishing solution for lithium niobate crystal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113787450A (en) * | 2021-09-07 | 2021-12-14 | 大连理工大学 | Preparation method of super-smooth surface of FeCrAl material |
| CN114085616A (en) * | 2021-09-27 | 2022-02-25 | 河北工业大学 | Lithium tantalate material chemical mechanical polishing solution based on silicon dioxide nano abrasive and preparation method thereof |
| CN115353807A (en) * | 2022-08-19 | 2022-11-18 | 山东大学深圳研究院 | Chemical mechanical polishing solution for preparing high-aspect-ratio lithium niobate waveguide |
-
2021
- 2021-04-28 CN CN202110466472.6A patent/CN113185920A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113787450A (en) * | 2021-09-07 | 2021-12-14 | 大连理工大学 | Preparation method of super-smooth surface of FeCrAl material |
| CN113787450B (en) * | 2021-09-07 | 2022-11-15 | 大连理工大学 | Preparation method of super-smooth surface of FeCrAl material |
| CN114085616A (en) * | 2021-09-27 | 2022-02-25 | 河北工业大学 | Lithium tantalate material chemical mechanical polishing solution based on silicon dioxide nano abrasive and preparation method thereof |
| CN115353807A (en) * | 2022-08-19 | 2022-11-18 | 山东大学深圳研究院 | Chemical mechanical polishing solution for preparing high-aspect-ratio lithium niobate waveguide |
| CN115353807B (en) * | 2022-08-19 | 2023-07-21 | 山东大学深圳研究院 | Chemical mechanical polishing solution for preparing high aspect ratio lithium niobate waveguide |
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Application publication date: 20210730 |