CN112126357A - Polishing solution for gallium nitride substrate material - Google Patents
Polishing solution for gallium nitride substrate material Download PDFInfo
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- CN112126357A CN112126357A CN202011008767.0A CN202011008767A CN112126357A CN 112126357 A CN112126357 A CN 112126357A CN 202011008767 A CN202011008767 A CN 202011008767A CN 112126357 A CN112126357 A CN 112126357A
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
Abstract
The embodiment of the invention discloses polishing solution for a gallium nitride substrate material, which comprises polishing particles, a corrosive, an oxidant, an ordered catalyst, a dispersion stabilizer and water, wherein the polishing particles comprise the following components in percentage by weight: 10-50 wt% of polishing particles; 0.1-20 wt% of a corrosive agent; 0.01-10 wt% of an oxidant; 0.0001-10 wt% of ordered catalyst; 0.01-10 wt% of a dispersion stabilizer; the balance of water. The ordered catalyst is added into the polishing solution, is prepared by a synthesis and modification method, has a special structure, electronic arrangement and surface groups on the surface, and can be orderly adsorbed on the surface of gallium nitride during polishing, so that the removal rate of the polishing solution is improved.
Description
Technical Field
The invention relates to the technical field of semiconductor material polishing, in particular to polishing solution for a gallium nitride substrate material.
Background
Gallium nitride (GaN) has potential application prospects in the aspects of photoelectric devices such as blue and ultraviolet light emitting diodes, laser diodes and the like. Currently, most commercial GaN-based devices are prepared by growing epitaxial thin films on substrates such as sapphire and silicon carbide. However, the higher dislocation density in the heteroepitaxial layer is due to the larger lattice and thermal mismatch between the GaN epitaxial layer and the substrate. Therefore, there is an urgent need to produce atomically smooth, damage-free GaN surfaces. Since GaN has very high hardness and strong chemical resistance and is difficult to process, its chemical mechanical polishing efficiency cannot meet the increasing industrial demand.
In the early stage of research, alumina particles with high hardness were used for polishing to improve the efficiency, but the removal rate was as close as 50nm/h, and the surface quality was also poor (Journal of electrochemical Society 155(2008): 113-. The research team carries out a series of researches (Tribology International 110(2017)441- & 450, Applied Surface Science 338(2015):85-91) on the ultra-fine Surface polishing of gallium nitride, and in order to improve the polishing efficiency, the research team proposes to adopt a catalyst to assist in polishing the gallium nitride (patent: 201510156564.9), but the catalytic performance of the catalyst cannot reach the best due to the agglomeration of the catalyst and the ineffective adsorption of the catalyst on the Surface of the gallium nitride.
Disclosure of Invention
The technical problem to be solved by the embodiments of the present invention is to provide a polishing solution for a gallium nitride substrate material, which can be orderly and stably adsorbed on gallium nitride, and can exert the catalytic performance of a catalyst to the maximum extent, and has high polishing efficiency.
In order to solve the technical problem, an embodiment of the present invention provides a polishing solution for a gallium nitride substrate material, including polishing particles, a corrosive agent, an oxidant, an ordered catalyst, a dispersion stabilizer and water, wherein the polishing solution comprises the following components by weight:
10 to 50wt% of polishing particles
0.1-20 wt% of corrosive agent
0.01 to 10wt% of an oxidizing agent
0.0001-10 wt% of ordered catalyst
0.01 to 10wt% of a dispersion stabilizer
The balance of water.
Further, the polishing particles are one or more of silicon oxide, cerium oxide, diamond, silicon carbide, boron nitride, zirconium oxide and iron oxide, and the particle size distribution range is 0.01-20 microns.
Further, the corrosive agent comprises an acidic corrosive agent and a basic corrosive agent.
Further, the acid corrosive agent comprises one or more of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, boric acid, sulfuric acid, phosphoric acid, acid potassium carbonate, sodium salt, citric acid, salicylic acid, glycolic acid, oxalic acid, malic acid, lactic acid and amino acid.
Further, the alkaline etchant includes one or more of potassium hydroxide, sodium hydroxide, ammonia, methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, isopropanolamine, aminopropanol, tetraethyleneamine, ethylenediamine, ethanolamine, diethanolamine, triethanolamine, hydroxylamine, diethyltriamine, triethylenetetramine, hydroxyethylethylenediamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine.
Further, the oxidizing agent includes one or more of hypochlorous acid, sodium hypochlorite, potassium hypochlorite, ammonium hypochlorite, perchloric acid, sodium perchlorate, potassium perchlorate, hypobromous acid, sodium hypobromite, perbromic acid, sodium hypoiodite, iodic acid, sodium iodate, potassium iodate, periodic acid, sodium periodate, potassium periodate, hydrogen peroxide, sodium peroxide, potassium peroxide, sodium nitrate, sodium nitrite, potassium nitrate, aluminum nitrate, iron nitrate, sodium percarbonate, potassium percarbonate, sodium persulfate, peroxodisulfuric acid, sodium peroxodisulfate, ammonium peroxodisulfate, peracetic acid or perbenzoic acid, urea peroxide.
Further, the stabilizing dispersant is hydroxyl alcohol, and comprises one or more of ethylene glycol, propylene glycol, butanediol, hexanediol, diethylene glycol, triethylene glycol, tetraethylene glycol, polyethylene glycol, polypropylene glycol, polyvinyl alcohol and glycerol.
Furthermore, the ordered catalyst is a compound with one or more of the characteristics of large specific surface area, high surface energy, porosity, multiple catalytic centers, regular active site distribution, stable structure, good dispersibility and multiple functional groups.
Further, the ordered catalyst is prepared by one or more of simple metal substances, oxides, salts, carbon, diatomite, graphite, graphene, montmorillonite, vermiculite and kaolin through synthesis treatment and modification treatment.
Further, the synthesis treatment comprises one or more of a solid phase grinding method, a thermal evaporation method, an ion sputtering method, a vacuum evaporation method, a plasma evaporation method, electron beam evaporation, a chemical vapor deposition method, a coprecipitation method, a hydrolysis precipitation method, a hydrothermal and solvothermal method, a microemulsion method, a solvent evaporation method and a template method; the modification treatment comprises one or more of surface organic coating, precipitation reaction coating, mechanochemistry, intercalation modification, organic physics/chemical coating, mechanochemistry/organic coating and inorganic precipitation reaction/organic coating.
The invention has the beneficial effects that: the ordered catalyst is added into the polishing solution, is prepared by a synthesis and modification method, has a special structure, electronic arrangement and surface groups on the surface, and can be orderly adsorbed on the surface of gallium nitride during polishing, so that the removal rate of the polishing solution is improved.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application can be combined with each other without conflict, and the present invention is further described in detail with reference to the accompanying tables and specific examples.
If directional indications (such as up, down, left, right, front, and rear … …) are provided in the embodiment of the present invention, the directional indications are only used to explain the relative positional relationship between the components, the movement situation, and the like in a specific posture, and if the specific posture is changed, the directional indications are changed accordingly.
In addition, the descriptions related to "first", "second", etc. in the present invention are only used for descriptive purposes and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature.
The polishing solution for the gallium nitride substrate material of the embodiment of the invention comprises polishing particles, a corrosive, an oxidant, an ordered catalyst, a dispersion stabilizer and water.
As an implementation mode, the ordered catalyst is a compound which has one or more of the characteristics of large specific surface area, high surface energy, porosity, multiple catalytic centers, regular active site distribution, stable structure, good dispersibility and multiple functional groups.
As an embodiment, the ordered catalyst is prepared by one or more of simple metal, oxide, salt, carbon, diatomite, graphite, graphene, montmorillonite, vermiculite and kaolin through synthesis treatment and modification treatment. The elementary metal is one or more of iron, nickel, titanium, aluminum, cobalt, molybdenum, copper, gold, silver, palladium, platinum, tungsten, tantalum, ruthenium, tin, vanadium and manganese, and the elementary substance can also be used as a reactant to generate a new ordered catalyst after modification or synthesis.
As an embodiment, the synthesis treatment includes treatment using one or more of a solid phase milling method, a thermal evaporation method, an ion sputtering method, a vacuum evaporation method, a plasma evaporation method, electron beam evaporation, a chemical vapor deposition method, a coprecipitation method, a hydrolytic precipitation method, a hydrothermal and solvothermal method, a microemulsion method, a solvent evaporation method, a template method; the modification treatment comprises one or more of surface organic coating, precipitation reaction coating, mechanochemistry, intercalation modification, organic physics/chemical coating, mechanochemistry/organic coating and inorganic precipitation reaction/organic coating.
The following examples after polishing, the gallium nitride surface was washed and dried with a cleaning agent and deionized water, and then the removal rate and surface quality of the thick film were measured. The removal rate of polishing (MRR) was calculated from the change in wafer weight before and after overpolishing measured with a precision electronic balance with a precision of 0.01mg, and the removal rate was calculated as the ratio of the removal thickness to the polishing time after conversion of the removal weight. The removal rate was determined by measuring the difference in thickness between the wafer before and after polishing with a thickness gauge, surface defects (scratches, pits) were observed with an optical microscope, the surface roughness Ra was measured with an atomic force microscope, the probe radius was 10nm, the vertical resolution was 0.01nm, the scanning frequency was 1.5Hz, and the scanning range was 1X 1 μm2. The polishing performance of each example and comparative document 1 is shown in table 1.
Example one
Under the condition of continuous stirring, polishing particles, a corrosive agent, an oxidant, an ordered catalyst and a dispersion stabilizer are sequentially added into deionized water and continuously stirred until the polishing particles, the corrosive agent, the oxidant, the ordered catalyst and the dispersion stabilizer are completely dissolved. The polishing solution comprises the following components in percentage by weight: 30 wt% of polishing particles (0.1 micron silicon oxide particles), 5 wt% of corrosive (sodium hydroxide), 10wt% of oxidant (hydrogen peroxide), 5 wt% of iron-based ordered catalyst (prepared by a precipitation method) and 0.1 wt% of dispersion stabilizer (glycerol). After polishing, the gallium nitride is cleaned and dried. The removal rate was determined by measuring the difference in thickness between the wafers before and after polishing with a thickness gauge, and surface defects (scratches, pits) were observed with an optical microscope, and the surface roughness Ra was measured with an atomic force microscope, and the results are shown in table 1.
Example two
Under the condition of continuous stirring, polishing particles, a corrosive agent, an oxidant, an ordered catalyst and a dispersion stabilizer are sequentially added into deionized water and continuously stirred until the polishing particles, the corrosive agent, the oxidant, the ordered catalyst and the dispersion stabilizer are completely dissolved. The polishing solution comprises the following components in percentage by weight: 50wt% of polishing particles (0.01 micron cerium oxide particles), 20wt% of corrosive (ammonia water), 5 wt% of oxidant (sodium hypochlorite), 0.0001 wt% of nickel-based ordered catalyst (prepared by coprecipitation method), and 5 wt% of dispersion stabilizer (hexanediol). After polishing, the gallium nitride is cleaned and dried. The removal rate was determined by measuring the difference in thickness between the wafers before and after polishing with a thickness gauge, and surface defects (scratches, pits) were observed with an optical microscope, and the surface roughness Ra was measured with an atomic force microscope, and the results are shown in table 1.
EXAMPLE III
Under the condition of continuous stirring, polishing particles, a corrosive agent, an oxidant, an ordered catalyst and a dispersion stabilizer are sequentially added into deionized water and continuously stirred until the polishing particles, the corrosive agent, the oxidant, the ordered catalyst and the dispersion stabilizer are completely dissolved. The polishing solution comprises the following components in percentage by weight: 20wt% of polishing particles (1 micron silicon carbide particles), 10wt% of corrosive agent (oxalic acid), 1 wt% of oxidizing agent (sodium persulfate), 0.01 wt% of cobalt-based ordered catalyst (prepared by a template method) and 5 wt% of dispersion stabilizer (ethanol). After polishing, the gallium nitride is cleaned and dried. The removal rate was determined by measuring the difference in thickness between the wafers before and after polishing with a thickness gauge, and surface defects (scratches, pits) were observed with an optical microscope, and the surface roughness Ra was measured with an atomic force microscope, and the results are shown in table 1.
Example four
Under the condition of continuous stirring, polishing particles, a corrosive agent, an oxidant, an ordered catalyst and a dispersion stabilizer are sequentially added into deionized water and continuously stirred until the polishing particles, the corrosive agent, the oxidant, the ordered catalyst and the dispersion stabilizer are completely dissolved. The polishing solution comprises the following components in percentage by weight: 1 wt% of polishing particles (20 micron aluminum oxide particles), 1 wt% of corrosive (hydrochloric acid), 5 wt% of oxidizing agent (potassium permanganate), 0.001 wt% of tantalum-based ordered catalyst (prepared by a template method) and 10wt% of dispersion stabilizer (ethylene glycol). After polishing, the gallium nitride is cleaned and dried. The removal rate was determined by measuring the difference in thickness between the wafers before and after polishing with a thickness gauge, and surface defects (scratches, pits) were observed with an optical microscope, and the surface roughness Ra was measured with an atomic force microscope, and the results are shown in table 1.
EXAMPLE five
Under the condition of continuous stirring, polishing particles, a corrosive agent, an oxidant, an ordered catalyst and a dispersion stabilizer are sequentially added into deionized water and continuously stirred until the polishing particles, the corrosive agent, the oxidant, the ordered catalyst and the dispersion stabilizer are completely dissolved. The polishing solution comprises the following components in percentage by weight: 0.1 wt% of polishing particles (10-micron iron oxide particles), 5 wt% of corrosive agent (malic acid), 0.01 wt% of oxidizing agent (perchloric acid), 10wt% of carbon-based ordered catalyst (prepared by organic coating method), and 10wt% of dispersion stabilizer (ethanol). After polishing, the gallium nitride is cleaned and dried. The removal rate was determined by measuring the difference in thickness between the wafers before and after polishing with a thickness gauge, and surface defects (scratches, pits) were observed with an optical microscope, and the surface roughness Ra was measured with an atomic force microscope, and the results are shown in table 1.
Reference 1 uses the application No.: 201510156564.9 patent publication:
under the condition of continuous stirring, polishing particles, a corrosive agent, an oxidant and a dispersion stabilizer are sequentially added into deionized water and are continuously stirred until the particles are completely dissolved. The polishing solution comprises the following components in percentage by weight: 0.1 wt% of polishing particles (10-micron iron oxide particles), 5 wt% of corrosive agent (malic acid), 0.01 wt% of oxidizing agent (perchloric acid), 10wt% of carbon-based ordered catalyst (prepared by organic coating method), and 10wt% of dispersion stabilizer (ethanol). After polishing, the gallium nitride is cleaned and dried. The removal rate was determined by measuring the difference in thickness between the wafers before and after polishing with a thickness gauge, and surface defects (scratches, pits) were observed with an optical microscope, and the surface roughness Ra was measured with an atomic force microscope, and the results are shown in table 1.
TABLE 1
| Examples | Removal Rate (nm/h) | Surface roughness (Ra) | Condition of surface defect |
| Example one | 80 | 0.01nm | No defect and no scratch |
| Example two | 90 | 0.03nm | No defect and no scratch |
| EXAMPLE III | 96 | 0.02nm | No defect and no scratch |
| Example four | 100 | 0.27nm | No defect and no scratch |
| EXAMPLE five | 120 | 0.01nm | No defect and no scratch |
| Reference 1 | 53 | 0.15nm | No defect and no scratch |
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The polishing solution for the gallium nitride substrate material is characterized by comprising polishing particles, a corrosive agent, an oxidant, an ordered catalyst, a dispersion stabilizer and water, wherein the polishing particles comprise the following components in percentage by weight:
10 to 50wt% of polishing particles
0.1-20 wt% of corrosive agent
0.01 to 10wt% of an oxidizing agent
0.0001-10 wt% of ordered catalyst
0.01 to 10wt% of a dispersion stabilizer
The balance of water.
2. The polishing slurry for a gallium nitride substrate material according to claim 1, wherein the polishing particles are one or more of silicon oxide, cerium oxide, diamond, silicon carbide, boron nitride, zirconium oxide, and iron oxide, and have a particle size distribution in the range of 0.01 to 20 μm.
3. The polishing slurry for a gallium nitride substrate material according to claim 1, wherein the etchant comprises an acidic etchant and an alkaline etchant.
4. The polishing solution for a gallium nitride substrate material according to claim 3, wherein the acidic etchant includes one or more of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, boric acid, sulfuric acid, phosphoric acid, acid potassium carbonate, sodium salt, citric acid, salicylic acid, glycolic acid, oxalic acid, malic acid, lactic acid, and amino acid.
5. The polishing solution for a gallium nitride substrate material according to claim 3, wherein the alkaline etchant comprises one or more of potassium hydroxide, sodium hydroxide, ammonia, methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, isopropanolamine, aminopropanol, tetraethyleneamine, ethylenediamine, ethanolamine, diethanolamine, triethanolamine, hydroxylamine, diethyltriamine, triethylenetetramine, hydroxyethylethylenediamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine.
6. The polishing solution for a gallium nitride substrate material according to claim 1, wherein the oxidizing agent comprises one or more of hypochlorous acid, sodium hypochlorite, potassium hypochlorite, ammonium hypochlorite, perchloric acid, sodium perchlorate, potassium perchlorate, hypobromous acid, sodium hypobromite, perbromic acid, sodium perbromite, hypoiodic acid, sodium hypoiodite, iodic acid, sodium iodate, potassium iodate, periodic acid, sodium periodate, potassium periodate, hydrogen peroxide, sodium peroxide, potassium peroxide, sodium nitrate, sodium nitrite, potassium nitrate, aluminum nitrate, ferric nitrate, sodium percarbonate, potassium percarbonate, sodium persulfate, peroxydisulfate, sodium peroxydisulfate, ammonium peroxydisulfate, peracetic acid or perbenzoic acid, and urea peroxide.
7. The polishing solution for gallium nitride substrate material according to claim 1, wherein the stabilizing dispersant is a hydroxyl alcohol comprising one or more of ethylene glycol, propylene glycol, butylene glycol, hexylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, polyethylene glycol, polypropylene glycol, polyvinyl alcohol, and glycerol.
8. The polishing solution for gallium nitride substrate material according to claim 1, wherein the ordered catalyst is a composite having one or more of features of large specific surface area, high surface energy, porosity, multiple catalytic centers, regular active site distribution, stable structure, good dispersibility, and multiple functional groups.
9. The polishing solution for gallium nitride substrate material according to claim 8, wherein the ordered catalyst is prepared by synthesizing and modifying one or more of simple metal, oxide, salt, carbon, diatomaceous earth, graphite, graphene, montmorillonite, vermiculite and kaolin.
10. The polishing solution for gallium nitride substrate material according to claim 9, wherein the synthetic treatment comprises treatment with one or more of a solid phase milling method, a thermal evaporation method, an ion sputtering method, a vacuum evaporation method, a plasma evaporation method, an electron beam evaporation method, a chemical vapor deposition method, a coprecipitation method, a hydrolytic precipitation method, a hydrothermal and solvothermal method, a microemulsion method, a solvent evaporation method, a template method; the modification treatment comprises one or more of surface organic coating, precipitation reaction coating, mechanochemistry, intercalation modification, organic physics/chemical coating, mechanochemistry/organic coating and inorganic precipitation reaction/organic coating.
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| CN113372821A (en) * | 2021-06-09 | 2021-09-10 | 广东富行洗涤剂科技有限公司 | Glass polishing solution capable of improving yield and reducing consumption and preparation method thereof |
| CN115011255A (en) * | 2022-06-27 | 2022-09-06 | 中国地质大学（北京） | High-precision polishing agent of monocrystalline diamond added with nano metal and preparation method thereof |
| CN115212920A (en) * | 2022-07-11 | 2022-10-21 | 浙江奥首材料科技有限公司 | Chitosan-based dispersion catalyst, semiconductor material polishing solution containing chitosan-based dispersion catalyst, and preparation method and application of semiconductor material polishing solution |
| RU2782566C1 (en) * | 2021-12-21 | 2022-10-31 | Общество с ограниченной ответственностью "AEM Технолоджис" (ООО "АЕМТИ") | Composition for chemical-mechanical polishing of the surface of semiconductor materials |
| CN115558427A (en) * | 2022-10-24 | 2023-01-03 | 浙江奥首材料科技有限公司 | Polishing solution based on micro-electrolysis-Fenton oxidation system, preparation method and application thereof |
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| CN115212920A (en) * | 2022-07-11 | 2022-10-21 | 浙江奥首材料科技有限公司 | Chitosan-based dispersion catalyst, semiconductor material polishing solution containing chitosan-based dispersion catalyst, and preparation method and application of semiconductor material polishing solution |
| CN115212920B (en) * | 2022-07-11 | 2023-08-15 | 浙江奥首材料科技有限公司 | Chitosan-based dispersion catalyst, semiconductor material polishing solution containing chitosan-based dispersion catalyst, preparation method and application of chitosan-based dispersion catalyst |
| CN115558427A (en) * | 2022-10-24 | 2023-01-03 | 浙江奥首材料科技有限公司 | Polishing solution based on micro-electrolysis-Fenton oxidation system, preparation method and application thereof |
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