CN116835638A - Magnesia partially stabilized zirconia slurry and preparation method and application thereof - Google Patents

Magnesia partially stabilized zirconia slurry and preparation method and application thereof Download PDF

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CN116835638A
CN116835638A CN202310726592.4A CN202310726592A CN116835638A CN 116835638 A CN116835638 A CN 116835638A CN 202310726592 A CN202310726592 A CN 202310726592A CN 116835638 A CN116835638 A CN 116835638A
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stabilized zirconia
partially stabilized
powder
slurry
magnesia partially
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张凡
何祖东
郭景新
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Zhejiang Chaojing Shengrui Photoelectric Co ltd
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Zhejiang Chaojing Shengrui Photoelectric Co ltd
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/02—Oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/34—Accessories
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B57/00—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
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    • C01—INORGANIC CHEMISTRY
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    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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    • C01F5/06—Magnesia by thermal decomposition of magnesium compounds
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K3/00—Materials not provided for elsewhere
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    • G01—MEASURING; TESTING
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    • G01J1/42—Photometry, e.g. photographic exposure meter using electric radiation detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/10—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors
    • H—ELECTRICITY
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    • 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
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Abstract

The application discloses a magnesia partially stabilized zirconia slurry, a preparation method and application thereof, wherein zirconium oxychloride crystal is weighed and dissolved in deionized water, and magnesium chloride hexahydrate is added to form a chloride mixed solution; dropwise adding excessive ammonia water into the mixed solution to precipitate zirconium hydroxide and magnesium hydroxide, centrifuging and repeatedly washing with hot water; drying and calcining at high temperature, and adding a dispersing agent and a wet grinding solvent for ball milling; after drying, screening qualified powder to prepare an aqueous solution, and adding a dispersing agent for ultrasonic vibration; regulating pH with ammonia water, and continuously stirring to obtain the slurry. The method has the advantages of simple process, strong operability, good sample fluidity and dispersibility, and capability of effectively inhibiting the problems of edge and corner chipping and cracking caused by stress concentration generated by abrasive particle accumulation in the grinding process of the GaSb substrate, greatly improving the surface quality of the ground GaSb substrate and reducing the damage rate of the ground GaSb substrate of the T2SL infrared detector chip.

Description

Magnesia partially stabilized zirconia slurry and preparation method and application thereof
Technical Field
The application relates to the technical field of preparation of semiconductor materials, in particular to magnesia partially-stabilized zirconia slurry, and a preparation method and application thereof.
Background
Antimonide II type superlattice (T2 SL) has the advantages of adjustable energy band, wide wavelength coverage range, high detection rate, good large-area uniformity and the like due to the two-type energy band structure, and is an ideal material of the third-generation infrared detector after HgCdTe materials and QWIP materials. The antimonide II type superlattice infrared detector is used as a back incidence device, under a refrigeration environment, a GaSb monocrystal substrate with the thickness of hundreds of micrometers can cause low infrared transmittance, and in a low-temperature cyclic test process, cracks and fragments of the GaSb substrate can be generated due to the difference of thermal expansion coefficients of materials, the consistency of the materials is affected, and the performance of the device is reduced, so that the preparation of the ultra-thin high-quality GaSb substrate is very important.
The surface quality index of the GaSb substrate after grinding and polishing mainly comprises damage, defects, surface roughness, surface particles, residues and the like, wherein the damage (including cracks, chipping and the like) can greatly influence the consistency of chip materials, and the performance of the device is greatly reduced. It is noted that, a simple mechanical polishing process is one of the effective means for removing a large amount of GaSb substrate, and the friction force applied to the GaSb substrate is large, the average removal rate (MRR) is fast, and the method is a main process for affecting the surface quality of the GaSb substrate.
At present, products mainly used for grinding and removing GaSb substrates in the markets at home and abroad are alumina aqueous solution grinding materials, abrasive grain alumina is often smelted by adopting an electric arc furnace Gao Wenlao, then is processed, finely crushed and hydraulically graded into corundum micropowder with different particle diameters, and finally, the corundum micropowder is prepared into a single aqueous solution grinding material according to a certain abrasive grain volume ratio. However, the abrasives prepared by this method have problems of poor slurry stability, fluidity and dispersibility. During the grinding process, the alumina abrasive grains are easy to agglomerate and sink to the grinding disc, and the occurrence probability of stress concentration of the GaSb substrate is increased greatly, so that the substrate edge, the corner fracture and the crack are caused, and the problems are fatal to tens of thousands of chips.
Zirconia is used as a novel abrasive, and has higher hardness and density, good toughness and wear resistance. The preparation method of the zirconia powder comprises an electric melting method and a chemical method, wherein the chemical method is divided into a hydrolysis precipitation method, a hydrothermal method, a sol-gel method and a coprecipitation method, and the three methods have the problems of complex process, high energy consumption, severe reaction conditions, environmental pollution and the like. The Chinese patent application (application number CN 201310300328.0) discloses a low-temperature synthesis method of agglomeration-free fully-stable cubic phase nano zirconia powder, which comprises the following production processes: firstly, respectively dissolving a stabilizer and zirconium salt by using concentrated nitric acid and deionized water to form a stable transparent solution, mixing the two solutions according to a certain proportion, regulating the pH value of the mixed solution by using ammonia water, then adding excessive precipitant to obtain a precursor, and drying and grinding for later use. And then mixing the powder with molten salt, drying and calcining, and finally washing with deionized water and drying to obtain the stable cubic phase nano zirconia powder. In the production process, the method has higher requirements on the granularity and shape of the powder, the calcination temperature is low, the whole process is insufficient for producing the powder with larger grain size, the higher average grinding rate of the GaSb substrate is not ensured, and the production efficiency is reduced. In addition, the adoption of concentrated nitric acid to dissolve zirconium salt can cause environmental pollution problem, which is unfavorable for sustainable development.
Disclosure of Invention
Aiming at the problems in the prior art, the application provides a preparation method of magnesia partially stabilized zirconia slurry, which has good repeatability and strong operability, and the GaSb substrate after being ground by adopting the slurry prepared by the application has low damage rate and is suitable for the requirement of advanced production of T2SL infrared detector chips. Specifically, the preparation method of the magnesia partially stabilized zirconia slurry comprises the following steps:
(1) Weighing zirconium oxychloride (ZrOCl) 2 ·8H 2 O) the crystal is dissolved in deionized water to prepare saturated solution, after insoluble matters and other impurities are removed by filtration, 1 to 10 percent of magnesium chloride hexahydrate (MgCl) is added according to the mass percent of zirconium oxychloride 2 ·6H 2 O), stirring uniformly to form a chloride mixed solution; in the application, magnesium is added as a stabilizer of zirconia particles;
(2) Dropwise adding excessive ammonia water (NH) into the chloride mixed solution in the step (1) 3 ·H 2 O), magnetically stirring for 3-6 h, and standing for 6-24 h to completely precipitate zirconium hydroxide and magnesium hydroxide; then, centrifuging for 5-15 min at a rotation speed of 5000-10000 rpm, repeatedly washing the precipitate with hot water, and repeating the centrifugation operation again;
(3) Heating and drying for 3-12 h at 60-120 ℃, and calcining at 1500-1800 ℃ to obtain magnesia partially stabilized zirconia powder; after cooling completely, putting the magnesia partially stabilized zirconia powder into a ball mill, adding 0.01-0.15 wt.% of polyacrylic acid dispersant and wet grinding solvent, and wet grinding for 8-24 hours;
(4) Taking out the magnesia partially stabilized zirconia powder after ball milling from a ball mill, drying the magnesia partially stabilized zirconia powder completely at 80-150 ℃, screening out powder with the size of 1-5 mu m, adding deionized water to ensure that the powder accounts for 8-20% of the volume fraction of the mixed solution, uniformly stirring, adding 0.05-3.00 wt.% of dispersing agent, and carrying out ultrasonic vibration for 30-90 min;
(5) And regulating the pH value of the mixed solution to 8-10 by ammonia water, and continuously mechanically stirring for 6-12 h to obtain the magnesia partially stabilized zirconia slurry.
Further, the method further comprises one or more of the following (1) - (12):
(1) The zirconium oxychloride crystal with the mass percentage of 99.5-99.9% is selected in the step (1);
(2) In the step (1), the insoluble matters and other impurities are removed by adopting rapid filter paper with the aperture size of 80-120 mu m;
(3) The temperature of the hot water in the step (2) is 60-70 ℃;
(4) Repeatedly washing the slow filter paper with the aperture size of 1-3 mu m with hot water for 7-15 times in the step (2);
(5) The wet grinding solvent in the step (3) is absolute ethyl alcohol or high-purity water;
(6) The ball mill in the step (3) is a superfine ball mill;
(7) In the step (3), calcining treatment is carried out in a resistance furnace;
(8) The addition amount of the wet grinding solvent is 50% of the mass of the powder;
(9) The dispersant in the step (4) is selected from AD8098 or ethylene glycol;
(10) Screening the powder by adopting a high-precision electroforming screen in the step (4);
(11) The steps (1) - (5) are carried out in a clean environment of thousands or more;
(12) The powder in the step (4) accounts for 8% -12% of the volume fraction of the mixed solution, and preferably the powder accounts for 12% of the volume fraction of the mixed solution.
The application also provides magnesia partially stabilized zirconia slurry prepared by the preparation method.
The application also provides an application of the magnesia partially stabilized zirconia slurry obtained by adopting the preparation method, wherein the application is used for grinding and removing the GaSb substrate.
Specifically, the magnesia partially stabilized zirconia slurry is mechanically stirred uniformly before being used for grinding and removing the GaSb substrate. The grinding and removing method comprises the following steps: fixing the GaSb substrate to be processed on the bottom of a grinding carrier, adjusting the downward pressure to 150g, and placing the grinding carrier on a grinding disc; by adopting the slurry, the liquid outlet speed of the slurry is adjusted to be 6ml/min, and the chassis is started to rotate at a constant speed of 10 rpm; and after the set removal value of the substrate is reached, taking down the GaSb substrate and washing the GaSb substrate.
The application has the beneficial effects that:
according to the application, the grinding powder with excellent dispersibility is prepared by wet grinding of the polyacrylic acid, the dispersing agent is added into the aqueous solution of the grinding powder, and the pH value is regulated to 8-10, so that the fluidity and the dispersibility of the slurry are greatly improved, the problems of edge and corner chipping and cracking caused by stress concentration generated by abrasive particle accumulation in the grinding process of the GaSb substrate can be effectively inhibited, and the surface quality of the ground GaSb substrate is greatly improved. In addition, the powder has high calcination temperature (calcination temperature is more than 1500 ℃), the crystal volume obtained by crystal growth is larger, and micron-sized grinding particles are obtained through ball milling and particle size screening, so that the high-level average grinding rate of the GaSb substrate in the grinding process is ensured, and the method is environment-friendly without using concentrated nitric acid to prepare slurry, meets the concept of sustainable development, and is suitable for the requirement of advanced production of T2SL infrared detector chips.
Drawings
FIG. 1 is an SEM image of a magnesia partially stabilized zirconia slurry of the application; wherein figure (a) is a slurry of 12% abrasive particles volume fraction prepared in example 1 and figure (b) is a slurry of 12% abrasive particles volume fraction prepared in example 2;
FIG. 2 is a schematic illustration of a single drop self-leveling comparison of a magnesia partially stabilized zirconia slurry having a volume fraction of 12% abrasive particles prepared in examples 1-2 of the present application and a conventional alumina slurry;
FIG. 3 is a graph of surface morphology under a GaSb substrate confocal microscope at 5 x magnification of a partially stabilized zirconia slurry of magnesia having a volume fraction of 12% with abrasive particles prepared in examples 1-2 of the present application; wherein figures (a) - (c) correspond to example 1, figure (a) being the top left corner of the GaSb substrate, figure (b) being the top edge of the GaSb substrate, figure (c) being the center of the GaSb substrate; fig. (d) - (f) correspond to example 2, fig. (d) is the lower right corner of the GaSb substrate, fig. (e) is the lower edge of the GaSb substrate, and fig. (f) is the center of the GaSb substrate;
FIG. 4 is a graph showing the damage rate and average removal rate of GaSb substrate after mechanical polishing of the magnesia partially stabilized zirconia slurry of examples 1-2 of the present application and a conventional alumina slurry.
Detailed Description
The present application is further illustrated and described below with reference to the following examples, which are but some, but not all, examples of the application. All other applications and embodiments, based on this application and described herein, which would be apparent to one of ordinary skill in the art without undue burden are within the scope of this application.
The experimental methods used in the following examples are conventional methods unless otherwise specified.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Example 1, a magnesia partially stabilized zirconia slurry
The preparation method comprises the following steps:
(1) Weighing zirconium oxychloride (ZrOCl) with the mass percentage of 99.5 percent 2 ·8H 2 O) the crystal is dissolved in deionized water to prepare saturated solution, insoluble substances and other impurities are filtered on a quick filter paper with the pore size of 80-120 mu m, and then analytically pure magnesium chloride hexahydrate (MgCl) is added according to 2.5wt.% of zirconium oxychloride 2 ·6H 2 O), stirring uniformly to form a chloride mixed solution;
(2) To the mixed solution, an excessive amount of aqueous ammonia (NH) 3 ·H 2 O), magnetically stirring for 6h, and standing for 12h to completely precipitate zirconium hydroxide and magnesium hydroxide. Subsequently, centrifugation was performed at 8000rpm for 10min, and after completion, washing was repeated 15 times with hot water at 70℃on a slow filter paper having a pore size of 1 to 3. Mu.m. Finally repeating the centrifugal operation for one time;
(3) Drying in an oven at 100deg.C for 12h, and calcining in a resistance furnace at 1650deg.C to obtain magnesium oxide partially stabilized zirconia (Mg-PSZ) powder. After cooling completely, the magnesia partially stabilized zirconia (Mg-PSZ) powder was put into a superfine ball mill, 0.015wt.% of polyacrylic acid (PAA) dispersant and 50wt.% of absolute ethanol were added, and wet-milled for 24 hours;
(4) Taking out the ball-milled Mg-PSZ from the ball mill, drying completely at 100 ℃, and screening by using a high-precision electroformed screen with the aperture size of 5 mu m and the interval of 15 mu m. Screening qualified powder, adding the qualified powder into deionized water, stirring uniformly with the powder accounting for 8%, 12%, 16% and 20% of the volume fraction (the volume fraction of abrasive particles) of the mixed solution, adding 1.5wt.% of dispersing agent AD8098 by weight of the powder, and carrying out ultrasonic vibration for 30min;
(5) And regulating the pH value of the mixed solution to 9 by ammonia water, and continuously mechanically stirring for 12 hours to obtain the Mg-PSZ grinding slurry. The prepared grinding slurry is stored in a cool and ventilated ultra-clean environment, the storage time is not suitable to be too long, and the grinding slurry is mechanically and uniformly stirred before use.
As shown in FIG. 1 (a), it can be seen from the SEM image of the partially stabilized zirconia slurry of example 1 that the slurry abrasive particles prepared in this example are amorphous powder particles, and after screening by an electroforming screen having a pore size of 5 μm, the particle size is mostly concentrated in 1 to 5. Mu.m, and no significant agglomeration phenomenon occurs, and the overall particle dispersibility is good. As shown in FIG. 2, the single drop self-leveling comparison experiment of the magnesia partially stabilized zirconia slurry and the conventional alumina slurry in example 1 shows that the sample prepared by the method has larger single drop flow area, better fluidity, smaller wetting angle, better wettability and better dispersibility compared with the conventional alumina slurry.
Example 2, a magnesia partially stabilized zirconia slurry
The preparation method comprises the following steps:
(1) Weighing zirconium oxychloride (ZrOCl) with the mass percentage of 99.5 percent 2 ·8H 2 O) the crystal is dissolved in deionized water to prepare saturated solution, insoluble substances and other impurities are filtered on a quick filter paper with the pore size of 80-120 mu m, and then analytically pure magnesium chloride hexahydrate (MgCl) is added according to 2.5wt.% of zirconium oxychloride 2 ·6H 2 O), stirring uniformly to form a chloride mixed solution;
(2) To the mixed solution, an excessive amount of aqueous ammonia (NH) 3 ·H 2 O), magnetically stirring for 6h, and standing for 12h to completely precipitate zirconium hydroxide and magnesium hydroxide. Subsequently, a centrifugation step is performedAnd (3) repeatedly washing the filter paper with water at 70 ℃ for 15 times on slow filter paper with the aperture size of 1-3 mu m after the completion of the rotation speed of 8000rpm for 10 min. Finally repeating the centrifugal operation for one time;
(3) Drying in an oven at 100deg.C for 12h, and calcining in a resistance furnace at 1650deg.C to obtain magnesium oxide partially stabilized zirconia (Mg-PSZ) powder. After cooling completely, the magnesia partially stabilized zirconia (Mg-PSZ) powder was put into a superfine ball mill, 0.015wt.% of polyacrylic acid (PAA) dispersant and 50wt.% of absolute ethanol were added, and wet-milled for 24 hours;
(4) Taking out the ball-milled Mg-PSZ from the ball mill, drying completely at 100 ℃, and screening by using a high-precision electroformed screen with the aperture size of 3 mu m and the interval of 15 mu m. Screening qualified powder, adding the qualified powder into deionized water, stirring uniformly with the powder accounting for 8%, 12%, 16% and 20% of the volume fraction (the volume fraction of abrasive particles) of the mixed solution, adding 1.5wt.% of dispersing agent AD8098 by weight of the powder, and carrying out ultrasonic vibration for 30min;
(5) And regulating the pH value of the mixed solution to 9 by ammonia water, and continuously mechanically stirring for 12 hours to obtain the Mg-PSZ grinding slurry. The prepared grinding slurry is stored in a cool and ventilated ultra-clean environment, the storage time is not suitable to be too long, and the grinding slurry is mechanically and uniformly stirred before use.
As shown in FIG. 1 (b), it can be seen from the SEM image of the partially stabilized zirconia slurry of example 2 that the slurry abrasive particles prepared in this example are amorphous powder particles, and after screening by an electroforming screen having a pore size of 3 μm, the particle size is mostly concentrated in 1 to 3. Mu.m, no significant agglomeration phenomenon occurs, and the overall particle dispersibility is good. As shown in fig. 2, the single drop self-leveling comparison experiment of the magnesia partially stabilized zirconia slurry and the conventional alumina slurry in example 2 shows that the sample prepared by the method has larger single drop flow area, better fluidity, smaller wetting angle, better wettability and better dispersibility compared with the conventional alumina slurry.
Example 3 application Effect verification of magnesia partially stabilized zirconia slurry prepared according to the application in GaSb substrate grinding removal
The magnesia partially stabilized zirconia slurry prepared in examples 1-2 with a volume fraction of 12% abrasive particles was used for GaSb substrate grinding, as compared to conventional alumina slurries. The specific grinding method is as follows: the GaSb substrate to be processed is fixed at the bottom of a grinding carrier by utilizing vacuum adsorption, and the grinding carrier is placed on a grinding disc after the adjustment of the adaptive downward pressure (150 g); adjusting the liquid outlet rates (6 ml/min) of the grinding slurries with different abrasive particle volume fractions prepared in the examples 1-2, and starting the chassis to rotate anticlockwise at a constant speed (10 rpm); and after the set removal value of the substrate is reached, taking down the GaSb substrate and washing the GaSb substrate.
As shown in FIG. 3, when the surface morphology of the GaSb substrate is mechanically ground by using a confocal microscope to observe the magnesia partially stabilized zirconia slurry with the abrasive particle volume fraction of 12% prepared in the embodiment 1-2 of the application, the surface of the GaSb substrate is uniform, no obvious scratches are generated, and no obvious damage and damage to edges and corners are generated.
As shown in fig. 4, it can be seen from the GaSb substrate surface damage rate curve and the average removal rate (MRR) curve of the magnesia partially stabilized zirconia slurry after mechanical grinding with the conventional alumina slurry that the GaSb substrate surface damage rate (the ratio of scratches, sharp damage at edges and corners and damage) corresponding to example 1-2 is lower overall, and is superior to the conventional alumina slurry because the magnesia partially stabilized zirconia slurry has better dispersibility and fluidity than the conventional alumina slurry. As such, the MRR for examples 1-2 of the present application is lower than conventional alumina slurries because less slurry accumulates on the abrasive disk, resulting in reduced mechanical grinding friction, at the same abrasive volume fraction. However, even so, the removal rate corresponding to example 1 was still as high as 13 to 28. Mu.m/min, which was quite remarkable. In contrast, the further decrease in the particle size of the abrasive particles of example 2 further reduced the mechanical polishing friction again, further suppressed the problem of stress concentration during the GaSb substrate polishing removal process, and therefore the corresponding substrate surface damage rate was slightly decreased. Notably, while the MRR corresponding to example 2 was slightly reduced as the particle size of the abrasive particles was reduced, it remained at a higher level, reaching 9-24 μm/min.

Claims (7)

1. A method for preparing a magnesia partially stabilized zirconia slurry, the method comprising the steps of:
(1) Weighing zirconium oxychloride crystal, dissolving in deionized water to prepare saturated solution, filtering to remove insoluble matters and other impurities, adding magnesium chloride hexahydrate according to the mass fraction of 1% -10% of zirconium oxychloride, and uniformly stirring to form chloride mixed solution;
(2) Dropwise adding excessive ammonia water into the chloride mixed solution obtained in the step (1), magnetically stirring for 3-6 h, and standing for 6-24 h to completely precipitate zirconium hydroxide and magnesium hydroxide; then, centrifuging for 5-15 min at a rotation speed of 5000-10000 rpm, repeatedly washing the precipitate with hot water, and repeating the centrifugation operation again;
(3) Heating and drying for 3-12 h at 60-120 ℃, and calcining at 1500-1800 ℃ to obtain magnesia partially stabilized zirconia powder; after cooling completely, putting the magnesia partially stabilized zirconia powder into a ball mill, adding 0.01-0.15 wt.% of polyacrylic acid dispersant and wet grinding solvent, and wet grinding for 8-24 hours;
(4) Taking out the magnesia partially stabilized zirconia powder after ball milling from a ball mill, drying the magnesia partially stabilized zirconia powder completely at 80-150 ℃, screening out powder with the size of 1-5 mu m, adding deionized water to ensure that the powder accounts for 8-20% of the volume fraction of the mixed solution, uniformly stirring, adding 0.05-3.00 wt.% of dispersing agent, and carrying out ultrasonic vibration for 30-90 min;
(5) And regulating the pH value of the mixed solution to 8-10 by ammonia water, and continuously mechanically stirring for 6-12 h to obtain the magnesia partially stabilized zirconia slurry.
2. The method for producing a magnesia partially stabilized zirconia slurry according to claim 1, wherein the method further comprises one or more of the following (1) to (12):
(1) The zirconium oxychloride crystal with the mass percentage of 99.5-99.9% is selected in the step (1);
(2) In the step (1), the insoluble matters and other impurities are removed by adopting rapid filter paper with the aperture size of 80-120 mu m;
(3) The temperature of the hot water in the step (2) is 60-70 ℃;
(4) Repeatedly washing the slow filter paper with the aperture size of 1-3 mu m with hot water for 7-15 times in the step (2);
(5) The wet grinding solvent in the step (3) is absolute ethyl alcohol or high-purity water;
(6) The ball mill in the step (3) is a superfine ball mill;
(7) In the step (3), calcining treatment is carried out in a resistance furnace;
(8) The addition amount of the wet grinding solvent is 50% of the mass of the powder;
(9) The dispersant in the step (4) is selected from AD8098 or ethylene glycol;
(10) Screening the powder by adopting a high-precision electroforming screen in the step (4);
(11) The steps (1) - (5) are carried out in a clean environment of thousands or more;
(12) The powder in the step (4) accounts for 8-12% of the volume fraction of the mixed solution.
3. The method for producing a magnesia partially stabilized zirconia slurry according to claim 2, wherein the powder in the step (4) is 12% by volume of the mixed solution.
4. A magnesia partially stabilized zirconia slurry prepared by the process of any one of claims 1 to 3.
5. The use of a magnesia partially stabilized zirconia slurry according to claim 4, wherein the use is for abrasive removal of GaSb substrates.
6. The use according to claim 5, wherein the magnesia partially stabilized zirconia slurry is mechanically stirred well before use in the abrasive removal of GaSb substrates.
7. The use according to claim 5, wherein the method of abrasive removal comprises: fixing the GaSb substrate to be processed on the bottom of a grinding carrier, adjusting the downward pressure to 150g, and placing the grinding carrier on a grinding disc; adopting the slurry as claimed in claim 4, adjusting the liquid outlet rate of the slurry to 6ml/min, and starting the chassis to rotate at a constant speed of 10 rpm; and after the set removal value of the substrate is reached, taking down the GaSb substrate and washing the GaSb substrate.
CN202310726592.4A 2023-06-19 2023-06-19 Magnesia partially stabilized zirconia slurry and preparation method and application thereof Pending CN116835638A (en)

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