CN118772843B - A multi-layer core-shell structure polishing abrasive, polishing liquid, preparation method and application - Google Patents
A multi-layer core-shell structure polishing abrasive, polishing liquid, preparation method and application Download PDFInfo
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- CN118772843B CN118772843B CN202411271315.XA CN202411271315A CN118772843B CN 118772843 B CN118772843 B CN 118772843B CN 202411271315 A CN202411271315 A CN 202411271315A CN 118772843 B CN118772843 B CN 118772843B
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
- C09K3/1445—Composite particles, e.g. coated particles the coating consisting exclusively of metals
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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
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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Abstract
The invention relates to a polishing abrasive material with a multilayer core-shell structure, a polishing liquid, a preparation method and application. The polishing solution comprises, by weight, 1-30 parts of a multi-layer core-shell structure polishing abrasive, 1-20 parts of a pH regulator, 0.1-10 parts of a dispersing agent, 0.1-10 parts of a dispersing auxiliary agent and 20-70 parts of deionized water. The multi-layer core-shell structure polishing abrasive is prepared by adopting the modes of impregnation, oxygen atmosphere calcination and concentrated sulfuric acid activation, metal salt is combined with the polishing abrasive through chelation of a chelating agent by the impregnation, the abrasive can be oxidized by the oxygen atmosphere, the dispersibility of the abrasive is improved, the chelating agent can be removed in the high-temperature calcination process, the loading capacity of the metal salt is improved, the core-shell structure after the concentrated sulfuric acid activation is correspondingly loosened, more catalytic sites are exposed, and the multi-layer core-shell structure is obtained through repeated wrapping.
Description
Technical Field
The invention belongs to the polishing solution technology, and particularly relates to a polishing abrasive with a multilayer core-shell structure, a polishing solution, a preparation method and application.
Background
Silicon carbide (SiC), which is a third generation semiconductor material, has two distinct characteristics, high hardness and chemical inertness. Because the hardness of the SiC material is high, the Mohs hardness of the silicon carbide is 9.2, and the silicon carbide is difficult to finely process by a common abrasive, the silicon carbide is mechanically polished at present by using a polishing solution containing diamond micro powder, and the diamond micro powder has a morphology with clear edges and corners and irregularities, has the Mohs hardness of 10 and is the hardest substance in the nature.
The diamond micro powder polishing solution is selected to have higher polishing efficiency, but after mechanical polishing, a plurality of scratches with different depths are observed on the surface of the silicon carbide wafer under a microscope due to irregular shape and high hardness of the diamond abrasive, which indicates that the damaged layer on the surface is deeper, and the damaged layer generated by mechanical polishing is difficult to completely remove in the subsequent chemical mechanical polishing.
However, the acid (pH <7, especially pH < 4) silicon carbide chemical mechanical polishing solution of the alpha-Al 2O3 abrasive with hardness which is inferior to that of silicon carbide is used, and the corners of the alpha-Al 2O3 abrasive are easily passivated by hard SiC, so that the polishing efficiency is rapidly attenuated with time, and the SiC removal rate is low.
Disclosure of Invention
The invention solves the technical problems of low SiC removal rate and serious scratch existing in the existing polishing solution in different degrees, and provides a polishing abrasive with a multilayer core-shell structure, the polishing solution, a preparation method and application.
In view of the technical problems in the prior art, the invention designs a polishing abrasive with a multilayer core-shell structure, polishing liquid, a preparation method and application.
It should be noted that, in the present invention, unless otherwise specified, reference to a specific meaning of "comprising" in the definition and description of compositions includes both open "comprising", "comprising" and the like and closed "consisting of.
In order to solve the technical problems, the invention adopts the following scheme:
[ first technical means ]
The preparation method of the polishing abrasive with the multilayer core-shell structure comprises the following steps:
step 1, preparing a metal-abrasive single-layer core-shell structured abrasive;
Step 1.1, immersing a polishing abrasive in a mixed solution of a metal salt solution, a chelating agent and a background solvent, and filtering after the impregnation is finished to obtain an abrasive precursor with a metal-abrasive single-layer core-shell structure;
Step 1.2, the precursor obtained in the step 1.1 is calcined at a high temperature in an oxygen atmosphere to obtain the core-shell structured abrasive with catalytic properties;
Step 1.3, placing the abrasive obtained in the step 1.2 in concentrated sulfuric acid, activating the metal-abrasive single-layer core-shell structure abrasive with catalytic properties under water bath heating, and cleaning after activation to obtain the metal-abrasive single-layer core-shell structure abrasive;
step2, preparing an abrasive with a metal-abrasive multilayer core-shell structure;
Taking the metal-abrasive material single-layer core-shell structured abrasive material prepared in the step 1 as polishing abrasive material, soaking the polishing abrasive material into a mixed solution of a metal salt solution, a chelating agent and a background solvent, filtering after soaking, calcining at a high temperature in an oxygen atmosphere, and activating with concentrated sulfuric acid to obtain the abrasive material with the metal-abrasive material double-layer core-shell structure;
And (3) repeating the operation of the step (1) again for the abrasive with the metal-abrasive double-layer core-shell structure to obtain the abrasive with the metal-abrasive multi-layer core-shell structure.
Further, the mass ratio of the polishing abrasive, the metal salt solution, the chelating agent and the background solvent is 2.5-10:0.5-2:20-30:20-70;
Preferably, the mass ratio of the polishing abrasive to the metal salt solution is 4:1-6:1.
Further, the polishing abrasive is one or more of aluminum oxide, silicon oxide and cerium oxide;
the metal elements in the metal salt solution are one or more of nickel, cobalt, iron, palladium, copper and zinc, and the salt in the metal salt solution is one or more of nitrate, hydrochloride and sulfate;
the chelating agent is one or more of valine, methionine, phenylalanine, threonine and glutamic acid;
The background solvent is one or more of ethanol, methanol, acetone, dimethylformamide and dimethylacetamide.
Further, in the step 1.1, the soaking time is 2-24 hours;
In the step 1.2, the flow rate of the oxygen is 0.1-1L/min;
In the step 1.2, the high-temperature calcination temperature is 350-1000 ℃ and the calcination time is 5-20h;
In the step 1.3, the temperature of water bath heating is 40-85 ℃ and the time is 1-4h.
Further, the particle size range of the metal-abrasive single-layer core-shell structured abrasive in the step 1 is 10-150nm,
The grain diameter range of the metal-abrasive material multilayer core-shell structure abrasive material in the step 2 is 20-160nm.
In the present invention, the mass ratio of the metal salt solution, the chelating agent to the background solvent may preferably be 1:25:65, and the mass ratio of the polishing abrasive to the metal salt solution may preferably be 5:1.
In the present invention, the polishing abrasive is preferably alumina;
the metal element in the metal salt solution is preferably palladium, and the salt solution in the metal salt solution is preferably nitrate;
The chelating agent is preferably glutamic acid;
The background solvent is preferably ethanol.
The metal salt solution is a mixed solution of metal salt and deionized water, and the mass ratio of the metal salt to the deionized water is 10-20:80-100, preferably 15-18:80-90.
In the present invention, the particle size range of the metal-abrasive single-layer core-shell structured abrasive described in step 1 is preferably 55 to 75nm.
The grain diameter range of the metal-abrasive material multi-layer core-shell structure abrasive material in the step 2 is preferably 60-80nm, and the grain diameter of the multi-layer core-shell structure abrasive material is larger than that of the single-layer core-shell structure abrasive material.
In the present invention, the impregnation time in step 1.1 is preferably 12 hours.
In step 1.2, the flow rate of oxygen is preferably 0.6L/min.
In step 1.2, the high temperature calcination is preferably at 600 to 1000 ℃, more preferably at 800 ℃, and the calcination time is preferably 8 to 14 hours, more preferably 12 hours.
In step 1.3, the temperature of the water bath heating is preferably 60 ℃, and the heating time is preferably 2h.
Further, the single-layer core-shell structured abrasive obtained in the step 1 is washed and filtered by deionized water, and then is dried, wherein the drying temperature is 50-70 ℃, preferably 60 ℃, and the drying time is 5-8 hours, preferably 7 hours.
The cleaning, filtering and drying treatment are carried out after each activation treatment.
The preparation method of the polishing abrasive with the multilayer core-shell structure has the unique advantages that:
firstly, the oxygen atmosphere can oxidize the abrasive material to generate oxygen-containing groups on the surface of the abrasive material, which is favorable for the synergistic effect of the polishing abrasive material and a dispersing agent in the polishing liquid and improves the dispersibility of the abrasive material;
Secondly, chelating agents can be removed in the high-temperature calcination process, so that metal salts are wrapped in the abrasive, and the loading capacity of the metal salts is improved by utilizing the advantage of large specific surface area of the polished abrasive;
Thirdly, the core-shell structure after the activation of the concentrated sulfuric acid is correspondingly loose, so that the surface of the core-shell structure is provided with more hydroxyl groups, more catalytic sites can be exposed, the dispersibility of the abrasive can be improved in a polishing procedure, and the metal salt-polishing abrasive-metal salt-polishing abrasive alternating multi-layer core-shell structure polishing abrasive is obtained through repeated wrapping.
In general, the invention prepares the polishing abrasive with a multi-layer core-shell structure by means of impregnation, oxygen atmosphere calcination and concentrated sulfuric acid activation, and the impregnation enables the metal salt to be combined with the polishing abrasive through chelation of a chelating agent.
The activation step of the invention has special significance:
The metal salt in the invention serves as a 'core' in the core-shell structure and has a catalytic effect.
The activation step is a special treatment step of the core-shell structure under a polishing system, and is not involved in the preparation of a general catalyst. The main reason is that in a general catalytic system, the problems of recycling of the catalyst and the like are required to be related, so that the structural stability of the catalyst needs to be considered and emphasized, and the activated core-shell structure is correspondingly loose and does not meet the practical application requirements of the existing catalyst.
In the polishing system, the catalytic performance of the core with the core-shell structure and the activated loose structure are utilized, so that more catalytic sites can be exposed, and the dispersibility of the abrasive can be improved in the polishing process.
[ Second technical means ]
The polishing abrasive with the multilayer core-shell structure is prepared by the preparation method.
The invention has the unique advantages of adopting a specific multi-layer core-shell structure:
In the polishing process, the metal salt as a "core" in the core-shell structure is dispersed with the dispersion of the polishing abrasive, and the polishing abrasive (shell) breaks up during polishing to expose the core-shell abrasive therein. The invention is a multi-layer core-shell structure, can expose more active sites, strengthen the catalysis effect, effectively prevent the problem of embedding the active sites of the core and effectively reduce scratches generated in the polishing process.
[ Third technical means ]
The polishing solution comprises the polishing abrasive with the multilayer core-shell structure, and comprises the following components in parts by weight:
1-30 parts of a polishing abrasive with a multilayer core-shell structure;
1-20 parts of pH regulator;
0.1-10 parts of dispersing agent;
0.1-10 parts of dispersing auxiliary;
And 20-70 parts of deionized water.
The pH regulator is an alkaline regulator, wherein the alkaline regulator is an organic base, and the organic base is one or more of diethanolamine, triisopropanolamine and triethanolamine;
The dispersing agent is an aqueous dispersing agent, wherein the aqueous dispersing agent is one or more of sodium polyacrylate, sodium dodecyl benzene sulfonate and sodium dodecyl sulfonate;
the dispersing auxiliary is one or more of aminopropylamine dioleate, octadecylamine sodium acetate, metoclopramide N4-sulfonate and 2-hydroxyethyl sulfonic acid dimethylamine.
In the invention, in order to further optimize the performance of the polishing solution, the components of the polishing solution can be preferably selected from 10-25 parts of a polishing abrasive with a multilayer core-shell structure, 3-10 parts of a pH regulator, 1-5 parts of a dispersing agent, 5-10 parts of a dispersing agent auxiliary agent and 30-50 parts of deionized water.
In the present invention, the pH adjuster is preferably triethanolamine;
the dispersant is preferably sodium dodecyl sulfonate;
The dispersing aid is preferably methoprene N4-sulfonate.
In the present invention, the pH of the prepared polishing liquid is 7 to 9, and the pH may be further preferably 8 to 9.
[ Fourth technical means ]
The preparation method of the polishing solution comprises the following steps:
Firstly weighing the components according to the proportion, fully mixing and stirring all the components except the polishing abrasive with the multi-layer core-shell structure to obtain a mixed solution, and finally adding the polishing abrasive with the multi-layer core-shell structure into the mixed solution and stirring uniformly to obtain the polishing solution.
Further, stirring for 30-90min at 30-100r/min before adding the polishing abrasive with the multilayer core-shell structure;
The multilayer core-shell structured polishing abrasive may be stirred for 45-80min, preferably at 45-80 r/min.
Further, adding the polishing abrasive with the multi-layer core-shell structure, and stirring for 10-50min at 30-100 r/min;
after adding the polishing abrasive with a multi-layer core-shell structure, stirring can be preferably carried out at 45-80r/min for 15-45min.
[ Fifth technical means ]
The polishing process of the polishing solution comprises the following steps:
step 1, diluting polishing solution by 2-5 times;
Step 2, setting ultraviolet light to irradiate the surface of the substrate with the wavelength of 100-400nm;
Step 3, setting the rotating speed of the polishing machine to be 50-100r/min and the pressure to be 15-30kg, dripping the polishing solution to the surface of the substrate at 5-200mL/min, and polishing for 10-800min;
In the polishing process of the present invention, the substrate is sapphire, silicon carbide or gallium nitride.
In the polishing process, the polishing solution used for the surface of sapphire, silicon carbide or gallium nitride in unit area is 3-5 mL.
[ Sixth technical means ]
The polishing solution of the polishing abrasive with the multilayer core-shell structure is applied to the polishing fields of silicon carbide, sapphire and gallium nitride.
The invention provides a polishing abrasive material with a multilayer core-shell structure, polishing solution, a preparation method and application, and the polishing abrasive material has the following beneficial effects:
1. The invention prepares the polishing abrasive with the multi-layer core-shell structure by adopting the modes of dipping, oxygen atmosphere calcination and concentrated sulfuric acid activation, the dipping enables the metal salt to be combined with the polishing abrasive through the chelation of the chelating agent, the oxygen atmosphere can oxidize the abrasive to improve the dispersibility of the abrasive, the chelating agent can be removed in the high-temperature calcination process to improve the loading capacity of the metal salt, the core-shell structure after the concentrated sulfuric acid activation can be correspondingly loosened, the surface of the core-shell structure can be provided with more hydroxyl groups, more catalytic sites can be exposed, the dispersibility of the abrasive can be improved in the polishing process, and the polishing abrasive with the multi-layer core-shell structure can be obtained through repeated wrapping.
2. The preparation method comprises the steps of taking polishing abrasive as a shell and wrapping metal salt as a core to obtain metal-abrasive assembled balls, taking the metal-abrasive assembled balls as the shell, forming a shell layer outside the metal salt added in the step 2 (the shell layer is formed by assembling a plurality of metal-abrasive assembled balls), finally forming the abrasive with a multi-layer core-shell structure, adopting the abrasive with the multi-layer core-shell structure with a specific structure, crushing the shell layer of the outer layer in the polishing process to generate a plurality of metal-abrasive assembled balls, dispersing along with the dispersion of the polishing abrasive, and because each metal-abrasive assembled ball can absorb energy under the irradiation of ultraviolet light, electrons on a valence band are transited to a conduction band, leaving a positively charged cavity on an original valence band, thereby exposing more active sites, strengthening the catalysis effect, and simultaneously, the cavity can react with OH-on the surface of other abrasive to generate OH free radicals with high oxidizing property, oxidizing the silicon carbide surface, so that the hardness is reduced, scratches are effectively reduced, and the problem of embedding active sites of the core is effectively prevented.
3. The invention improves the dispersibility of the abrasive by adding the dispersing agent auxiliary agent and the dispersing agent, ensures that the surface quality of the polished substrate is better, simultaneously can well maintain the pH stability, ensures that the pH in the polishing process is maintained in an alkaline range, and ensures that the polishing solution can be kept stable and the polishing rate is stable.
4. The activation step of the present invention is advantageous in polishing systems, and can expose more catalytic sites, and can also improve the dispersibility of the abrasive during the polishing process.
Drawings
FIG. 1 is a photograph showing the surface of silicon carbide after polishing with the polishing solution of example 1 of the present invention;
FIG. 2 is a photograph showing the surface of silicon carbide after polishing by the polishing liquid of comparative example 1 of the present invention.
Detailed Description
The invention is further described with reference to specific examples and figures:
The invention relates to a preparation method of a polishing abrasive with a multi-group multi-layer core-shell structure, which comprises the following steps:
Step 1, preparing a metal-abrasive single-layer core-shell structured abrasive
Step 1.1, immersing a polishing abrasive in a mixed solution of a metal salt solution, a chelating agent and a background solvent for 12 hours, washing and filtering with deionized water, and drying in an oven at 60 ℃ for 7 hours to obtain an abrasive precursor with a metal-abrasive single-layer core-shell structure;
Calcining the precursor obtained in the step 1.1 at a high temperature of 800 ℃ in an oxygen atmosphere, wherein the flow of oxygen is 0.6L/min, and calcining for 12 hours to obtain the core-shell structured abrasive with catalytic properties;
Step 1.3, placing the abrasive obtained in the step 1.2 in concentrated sulfuric acid, heating in a water bath at 60 ℃ for 2 hours, washing and filtering deionized water, drying in an oven at 60 ℃ for 7 hours to obtain the metal-abrasive single-layer core-shell structured abrasive with catalytic properties;
Step 2, preparing the abrasive with the metal-abrasive multi-layer core-shell structure
Immersing the single-layer nuclear abrasive material prepared in the step 1 in a mixed solution of a metal salt solution, a chelating agent and a background solvent for 12 hours, washing and filtering with deionized water, and drying in an oven at 60 ℃ for 7 hours to obtain an abrasive precursor with a metal-abrasive material double-layer nuclear shell structure;
Then calcining the precursor at a high temperature of 800 ℃ in an oxygen atmosphere, wherein the flow rate of oxygen is 0.6L/min, and calcining for 12 hours to obtain the core-shell structured abrasive with catalytic properties;
Placing the core-shell structured abrasive with the catalytic property into concentrated sulfuric acid, heating in a water bath at 60 ℃ for 2 hours, washing and filtering deionized water, and drying in an oven at 60 ℃ for 7 hours to obtain the metal-abrasive double-layer core-shell structured abrasive with the catalytic property;
And 3, repeating the operation of the step 1 on the abrasive with the metal-abrasive double-layer core-shell structure to obtain the abrasive with the metal-abrasive three-layer core-shell structure.
The preparation method of the metal salt solution in the step 1-3 comprises the step of dissolving 18 parts of metal salt in 82 parts of deionized water to obtain the metal salt solution.
TABLE 1 polishing abrasive 1-abrasive 5 of multilayer core-shell structure
The preparation method of the polishing abrasive with the single-layer core-shell structure comprises the following steps:
Step 1, preparing a metal-abrasive single-layer core-shell structured abrasive
As abrasive 1.
Abrasive 7 differs from abrasive 1 in that concentrated sulfuric acid is not used for activation.
The preparation method of the polishing solution comprises the following steps:
Weighing all the components according to the proportion, stirring all the components except the polishing abrasive with the multi-layer core-shell structure for 60min at 60r/min, adding the polishing abrasive with the multi-layer core-shell structure into the solution, and continuously stirring for 35 min at 60r/min to obtain the polishing solution containing the polishing abrasive.
Table 2 examples 1-5 of polishing solutions
Table 3 comparative examples 1-4 of polishing solutions
Performance 1 Material Removal Rate (MRR)
The test method comprises measuring substrate quality before and after polishing, and indirectly calculating the thickness of the removed silicon carbide layer according to density and substrate area. The method has the greatest characteristics of simple measurement and capability of rapidly obtaining the removal rate. The evaluation of the material removal rate in the examples and comparative examples of the present application is as follows:
MRR=△m/(ρSt)
Wherein Deltam is the mass change before and after polishing silicon carbide, ρ is the silicon carbide density, S is the area of the silicon carbide wafer, and t is the polishing time.
Performance 2 surface roughness (Ra)
The testing method comprises the steps of measuring the surface roughness of the polished silicon carbide chip by using a surface roughness measuring instrument, observing the surface scratch degree, and the testing result is shown in figures 1-2.
Table 4 test data
As can be seen from Table 4, the Material Removal Rate (MRR) ranges from 5.0 to 6.1 μm/h and the surface roughness (Ra) ranges from 0.13 to 0.25nm.
Comparative example the Material Removal Rate (MRR) ranged from 4.6 to 5.4 μm/h and the surface roughness (Ra) ranged from 0.26 to 0.51nm.
Compared with the comparative example, the embodiment of the invention improves the material removal rate, reduces the surface roughness, and can also prove the severity of the scratch of the silicon carbide surface, and the larger the roughness is, the rougher and the unsmooth of the surface are, so that the polishing solution of the embodiment of the invention has the effect of low scratch.
In comparative example 1, the alumina abrasive is extremely liable to agglomerate in the solution, resulting in insufficient dispersibility of the abrasive in the solution, and thus poor polishing effect on the substrate, low material removal rate, and corresponding scratch.
In comparative example 2, the abrasive 6 with a single-layer core-shell structure is adopted, so that fewer active sites are exposed in the polishing process, the catalysis effect is weakened, the problem of embedding the active sites of the core with the core-shell structure cannot be well solved, and the surface roughness is high.
In comparative example 3, the abrasive 7, which is not activated by concentrated sulfuric acid, is not activated, has no active group, has enhanced chemical inertness of the shell, cannot be further modified, is not easy to form a multi-layer structure, and has low removal rate and high surface roughness.
In comparative example 4, the dispersion was not good enough and the pH of the solution was not well stabilized during polishing, and the polishing rate was fluctuated, i.e., the polishing rate was faster at the early stage and the polishing rate was lower after a period of use.
The polishing effect of the present invention will be further described with reference to the accompanying drawings:
FIG. 1 is a photograph showing the surface of silicon carbide after polishing by the polishing liquid of example 1 of the present invention, and FIG. 2 is a photograph showing the surface of silicon carbide after polishing by the polishing liquid of comparative example 1 of the present invention.
As can be seen from fig. 1 and fig. 2, the surface of fig. 2 has more scratches, which proves that the silicon carbide treated with the polishing solution of comparative example 1 has scratches, whereas fig. 1 does not observe significant scratches, which proves that the polishing solution of example 1 of the present invention has low scratch performance.
The invention prepares the multi-layer core-shell structure polishing abrasive by adopting the modes of dipping, oxygen atmosphere calcination and concentrated sulfuric acid activation, the dipping enables the metal salt to be combined with the polishing abrasive through the chelation of the chelating agent, the oxygen atmosphere can oxidize the abrasive to improve the dispersibility of the abrasive, the chelating agent can be removed in the high-temperature calcination process to improve the loading capacity of the metal salt, the core-shell structure after the concentrated sulfuric acid activation can be correspondingly loosened, the surface of the core-shell structure can be provided with more hydroxyl groups, more catalytic sites can be exposed, the dispersibility of the abrasive can be improved in the polishing process, and the multi-layer core-shell structure can be obtained through repeated wrapping.
While the present invention has been described above by way of example with reference to the embodiments and the accompanying drawings, it is apparent that the implementation of the present invention is not limited by the above manner, and it is within the scope of the present invention to apply the inventive concept and technical solution to other situations as long as various improvements are adopted by the inventive concept and technical solution, or without any improvement.
Claims (8)
1. The polishing solution is characterized by comprising a multi-layer core-shell structure polishing abrasive, and comprises the following components in parts by weight:
1-30 parts of a polishing abrasive with a multilayer core-shell structure;
1-20 parts of pH regulator;
0.1-10 parts of dispersing agent;
0.1-10 parts of dispersing auxiliary;
20-70 parts of deionized water;
the preparation method of the polishing abrasive with the multilayer core-shell structure comprises the following steps:
step 1, preparing a metal-abrasive single-layer core-shell structured abrasive;
Step 1.1, immersing a polishing abrasive in a mixed solution of a metal salt solution, a chelating agent and a background solvent, and filtering after the impregnation is finished to obtain an abrasive precursor with a metal-abrasive single-layer core-shell structure;
Step 1.2, the precursor obtained in the step 1.1 is calcined at a high temperature in an oxygen atmosphere to obtain the core-shell structured abrasive with catalytic properties;
Step 1.3, placing the abrasive obtained in the step 1.2 in concentrated sulfuric acid, activating the metal-abrasive single-layer core-shell structure abrasive with catalytic properties under water bath heating, and cleaning after activation to obtain the metal-abrasive single-layer core-shell structure abrasive;
step2, preparing an abrasive with a metal-abrasive multilayer core-shell structure;
and (3) taking the metal-abrasive single-layer core-shell structured abrasive prepared in the step (1) as a polishing abrasive, and repeating the operation of the step (1) at least twice to obtain the multi-layer metal-abrasive core-shell structured abrasive.
2. The polishing liquid according to claim 1, wherein:
The specific operation of preparing the metal-abrasive material with the multi-layer core-shell structure in the step 2 is as follows:
Taking the metal-abrasive material single-layer core-shell structured abrasive material prepared in the step 1 as polishing abrasive material, soaking the polishing abrasive material into a mixed solution of a metal salt solution, a chelating agent and a background solvent, filtering after soaking, calcining at a high temperature in an oxygen atmosphere, and activating with concentrated sulfuric acid to obtain the abrasive material with the metal-abrasive material double-layer core-shell structure;
And (3) repeating the operation of the step (1) again for the abrasive with the metal-abrasive double-layer core-shell structure to obtain the abrasive with the metal-abrasive multi-layer core-shell structure.
3. The polishing liquid according to claim 2, wherein:
The mass ratio of the metal salt solution to the chelating agent to the background solvent is 0.5-2:20-30:20-70;
The mass ratio of the polishing abrasive to the metal salt solution is 4:1-6:1.
4. The polishing liquid according to claim 2, wherein:
The metal elements in the metal salt solution are one or more of nickel, cobalt, iron, palladium, copper and zinc, and the salt in the metal salt solution is one or more of nitrate, hydrochloride and sulfate.
5. The polishing liquid according to claim 1, wherein:
The pH regulator is an alkaline regulator;
The alkaline regulator is an organic base, and the organic base is one or more of diethanolamine, triisopropanolamine and triethanolamine;
The dispersing agent is an aqueous dispersing agent, wherein the aqueous dispersing agent is one or more of sodium polyacrylate, sodium dodecyl benzene sulfonate and sodium dodecyl sulfonate;
the dispersing auxiliary is one or more of aminopropylamine dioleate, octadecylamine sodium acetate, metoclopramide N4-sulfonate and 2-hydroxyethyl sulfonic acid dimethylamine.
6. A method for producing the polishing liquid according to any one of claims 1 to 5, comprising the steps of:
Firstly weighing the components according to the proportion, fully mixing and stirring all the components except the polishing abrasive with the multi-layer core-shell structure to obtain a mixed solution, and finally adding the polishing abrasive with the multi-layer core-shell structure into the mixed solution and stirring uniformly to obtain the polishing solution.
7. A polishing process of the polishing liquid according to any one of claims 1 to 5, comprising the steps of:
step 1, diluting polishing solution by 2-5 times;
Step 2, setting ultraviolet light to irradiate the surface of the substrate with the wavelength of 100-400nm;
Step 3, setting the rotating speed of the polishing machine to be 50-100r/min and the pressure to be 15-30kg, dripping the polishing solution to the surface of the substrate at the speed of 5-200mL/min, and polishing for 10-800min.
8. Use of the polishing liquid according to any one of claims 1 to 5 in the field of silicon carbide, sapphire and gallium nitride polishing.
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