CN116835638B - A magnesium oxide partially stabilized zirconium oxide slurry, its preparation method and application - Google Patents
A magnesium oxide partially stabilized zirconium oxide slurry, its preparation method and applicationInfo
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- CN116835638B CN116835638B CN202310726592.4A CN202310726592A CN116835638B CN 116835638 B CN116835638 B CN 116835638B CN 202310726592 A CN202310726592 A CN 202310726592A CN 116835638 B CN116835638 B CN 116835638B
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- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
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- 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
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Abstract
本发明公开一种氧化镁部分稳定氧化锆浆料及其制备方法和应用，称取氧氯化锆晶体溶于去离子水中，加入六水氯化镁形成氯化物混合溶液；向混合溶液中滴加过量的氨水，使氢氧化锆、氢氧化镁沉淀后，离心并反复热水洗涤；干燥并高温煅烧，再加入分散剂和湿磨溶剂球磨；干燥后，筛选合格的粉体配制成水溶液，加入分散剂超声震荡；用氨水调pH，持续搅拌即获得所述浆料。本发明工艺简单，可操作性较强，样品流动性和分散性较好，可以有效地抑制GaSb衬底在研磨过程中因磨粒堆积产生的应力集中而引起的边、角碎裂和裂纹问题，大大提升了GaSb衬底研磨后的表面质量，T2SL红外探测器芯片GaSb衬底研磨后损伤率低。
This invention discloses a magnesium oxide partially stabilized zirconium oxide slurry, its preparation method, and its application. Zirconium oxychloride crystals are dissolved in deionized water, and magnesium chloride hexahydrate is added to form a chloride mixed solution. Excess ammonia is added dropwise to the mixed solution to precipitate zirconium hydroxide and magnesium hydroxide. The precipitate is then centrifuged and repeatedly washed with hot water. The slurry is dried and calcined at high temperature, then ball-milled with a dispersant and wet milling solvent. After drying, qualified powder is screened and prepared into an aqueous solution, which is then ultrasonically vibrated with a dispersant. The pH is adjusted with ammonia, and the mixture is continuously stirred to obtain the slurry. This invention features a simple process, high operability, and good sample flowability and dispersibility. It effectively suppresses edge and corner breakage and cracking problems caused by stress concentration due to abrasive particle accumulation during GaSb substrate grinding, significantly improving the surface quality of the ground GaSb substrate. The T2SL infrared detector chip GaSb substrate shows low damage rate after grinding.
Description
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 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 ultrathin 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 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 abrasive prepared by the method has the problem of poor stability, fluidity and dispersibility of the slurry. 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 steps of dissolving a stabilizer and zirconium salt into a stable transparent solution by using concentrated nitric acid and deionized water respectively, mixing the two solutions according to a certain proportion, regulating the pH value of the mixed solution by using ammonia water, adding excessive precipitant to obtain a precursor, 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 invention 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 invention 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 2·8H2 O) crystal, dissolving in deionized water to prepare saturated solution, filtering to remove insoluble matters and other impurities, adding magnesium chloride hexahydrate (MgCl 2·6H2 O) accounting for 1-10% of the mass fraction of the zirconium oxychloride, and uniformly stirring to form a chloride mixed solution;
(2) Dropwise adding excessive ammonia water (NH 3·H2 O) into the chloride mixed solution obtained in the step (1), magnetically stirring for 3-6 h, standing for 6-24 h to completely precipitate zirconium hydroxide and magnesium hydroxide, centrifuging at 5000-10000 rpm for 5-15 min, repeatedly washing the precipitate with hot water, and repeating the centrifuging operation;
(3) Heating and drying at 60-120 ℃ for 3-12 hours, 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 dispersing agent 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 completely at 80-150 ℃, screening out powder with the size of 1-5 mu m, adding deionized water to enable the powder to account 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 using ammonia water, and continuously mechanically stirring for 6-12 hours 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), filtering by adopting quick filter paper with the aperture size of 80-120 mu m to remove insoluble matters and other impurities;
(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) In the step (4), the powder 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 invention also provides magnesia partially stabilized zirconia slurry prepared by the preparation method.
The invention 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 method for grinding and removing the GaSb substrate comprises the steps of fixing the GaSb substrate to be processed on the bottom of a grinding carrier, adjusting the downward pressure to 150g, placing the grinding carrier on a grinding disc, adjusting the liquid outlet speed of the slurry to be 6ml/min by adopting the slurry, starting the chassis to rotate at a constant speed of 10rpm, and taking down and washing the GaSb substrate after the substrate reaches a preset removal value.
The invention has the beneficial effects that:
According to the invention, 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 (the 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, the slurry is prepared without concentrated nitric acid, the environment is friendly, the sustainable development concept is met, and the method 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 invention, wherein FIG. (a) is a slurry having a volume fraction of 12% abrasive particles prepared in example 1, and FIG. (b) is a slurry having a volume fraction of 12% abrasive particles 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 invention and a conventional alumina slurry;
FIG. 3 is a graph of the surface morphology of a GaSb substrate confocal microscope after mechanical grinding of a magnesia partially stabilized zirconia slurry with a volume fraction of 12% and prepared by adopting the method of examples 1-2, wherein graphs (a) - (c) correspond to example 1, graph (a) are upper left corners of the GaSb substrate, graph (b) are upper edges of the GaSb substrate, graph (c) are centers of the GaSb substrate, graphs (d) - (f) correspond to example 2, graph (d) are lower right corners of the GaSb substrate, graph (e) are lower edges of the GaSb substrate, and graph (f) are centers 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 invention and a conventional alumina slurry.
Detailed Description
The present invention is further illustrated and described below with reference to the following examples, which are but some, but not all, examples of the invention. All other inventions and embodiments, based on this invention and described herein, which would be apparent to one of ordinary skill in the art without undue burden are within the scope of this invention.
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 99.5% zirconium oxychloride (ZrOCl 2·8H2 O) crystal by mass percent, dissolving in deionized water to prepare saturated solution, filtering insoluble substances and other impurities on quick filter paper with the pore size of 80-120 mu m, adding analytically pure magnesium chloride hexahydrate (MgCl 2·6H2 O) according to 2.5wt.% of zirconium oxychloride, and uniformly stirring to form a chloride mixed solution;
(2) And (3) dropwise adding excessive ammonia water (NH 3·H2 O) into the mixed solution, magnetically stirring for 6h, and standing for 12h to completely precipitate zirconium hydroxide and magnesium hydroxide. And then, carrying out centrifugal treatment, wherein the rotating speed is 8000rpm, the time is 10min, and repeatedly washing the filter paper on the slow filter paper with the aperture size of 1-3 mu m for 15 times by using 70 ℃ hot water after the completion. Finally repeating the centrifugal operation for one time;
(3) Dried in an oven at 100 ℃ for 12 hours and then calcined in a resistance furnace at 1650 ℃ to a 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) The ball-milled Mg-PSZ was taken out from the ball mill, dried at 100℃to completion, and screened with a high-precision electroformed screen having a pore size of 5 μm and a pitch 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), as can be seen from the SEM image of the magnesia partially stabilized zirconia slurry of example 1, the slurry abrasive particles prepared in this example are amorphous powder particles, and after being screened by an electroforming screen having a pore size of 5 μm, the particle size is mostly concentrated in 1 to 5 μm, and no obvious 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 99.5% zirconium oxychloride (ZrOCl 2·8H2 O) crystal by mass percent, dissolving in deionized water to prepare saturated solution, filtering insoluble substances and other impurities on quick filter paper with the pore size of 80-120 mu m, adding analytically pure magnesium chloride hexahydrate (MgCl 2·6H2 O) according to 2.5wt.% of zirconium oxychloride, and uniformly stirring to form a chloride mixed solution;
(2) And (3) dropwise adding excessive ammonia water (NH 3·H2 O) into the mixed solution, magnetically stirring for 6h, and standing for 12h to completely precipitate zirconium hydroxide and magnesium hydroxide. And then, carrying out centrifugal treatment, wherein the rotating speed is 8000rpm, the time is 10min, and repeatedly washing the filter paper on the slow filter paper with the aperture size of 1-3 mu m for 15 times by using 70 ℃ hot water after the completion. Finally repeating the centrifugal operation for one time;
(3) Dried in an oven at 100 ℃ for 12 hours and then calcined in a resistance furnace at 1650 ℃ to a 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) The ball-milled Mg-PSZ was taken out from the ball mill, dried at 100℃to completion, and screened with a high-precision electroformed screen having a pore size of 3 μm and a pitch 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), as can be seen from the SEM image of the magnesia partially stabilized zirconia slurry of example 2, 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 μm, no obvious 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 invention 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 method comprises fixing the GaSb substrate to be processed on the bottom of a grinding carrier by vacuum adsorption, adjusting the adaptive pressing force (150 g), placing the grinding carrier on a grinding disc, adjusting the liquid outlet rates (6 ml/min) of grinding slurries with different abrasive particle volume fractions prepared in the embodiment 1-2, starting the chassis to rotate anticlockwise at a constant speed (10 rpm), and taking down and washing the GaSb substrate after reaching the substrate set removal value.
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 invention, 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 invention 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 is still as high as 13 to 28 μm/min, which is quite considerable. 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. It is noted that while the MRR was slightly reduced with the particle size of the abrasive particles of example 2, the MRR remained at a higher level, reaching 9-24 μm/min.
Claims (3)
1. Use of a magnesia partially stabilized zirconia slurry for abrasive removal of GaSb substrates, characterized in that the magnesia partially stabilized zirconia slurry preparation method comprises 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 hours, standing for 6-24 hours to enable zirconium hydroxide and magnesium hydroxide to be completely precipitated, centrifuging at 5000-10000 rpm for 5-15 minutes, repeatedly washing the precipitate with hot water, and repeating the centrifuging operation;
(3) Heating and drying at 60-120 ℃ for 3-12 hours, 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 dispersing agent and wet grinding solvent, and wet grinding for 8-24 hours;
(4) Taking out the magnesium oxide partially stabilized zirconia powder subjected to ball milling from a ball mill, drying the powder completely at 80-150 ℃, screening out powder with the size of 1-5 mu m, adding deionized water to enable the powder to account 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, wherein the powder accounts for 12% of the volume fraction of the mixed solution;
(5) Adjusting the pH value of the mixed solution to 8-10 by ammonia water, and continuously mechanically stirring for 6-12 hours to obtain the magnesia partially stabilized zirconia slurry;
also included are one or more of the following S1-S12:
s1, selecting zirconium oxychloride crystals with the mass percentage of 99.5-99.9% in the step (1);
S2, filtering the insoluble matters and other impurities by adopting quick filter paper with the aperture size of 80-120 mu m in the step (1);
s3, the temperature of the hot water in the step (2) is 60-70 ℃;
S4, 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;
s5, the wet grinding solvent in the step 3 is absolute ethyl alcohol or high-purity water;
S6, the ball mill in the step 3 is a superfine ball mill;
s7, calcining in the step (3) in a resistance furnace;
s8, the addition amount of the wet grinding solvent is 50% of the mass of the powder;
S9, the dispersing agent in the step (4) is selected from AD8098 or ethylene glycol;
S10, screening powder by adopting a high-precision electroforming screen in the step (4);
s11, performing the steps (1) - (5) in a clean environment with thousands of grades or more;
S12, the powder in the step (4) accounts for 8% -12% of the volume fraction of the mixed solution.
2. The use according to claim 1, wherein the magnesia partially stabilized zirconia slurry is mechanically stirred well before use in the abrasive removal of GaSb substrates.
3. The method for grinding and removing the GaSb substrate according to claim 1, wherein the method for grinding and removing the GaSb substrate comprises the steps of fixing the GaSb substrate to be processed on the bottom of a grinding carrier, adjusting the downward pressure to 150 g, placing the grinding carrier on a grinding disc, adjusting the liquid outlet rate of the slurry to 6 ml/min by using the slurry according to claim 1, starting the chassis 10 to rpm to rotate at a constant speed, and taking down and washing the GaSb substrate after the substrate reaches a set removing value.
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