CN111673632A - Preparation method of nano-grade zirconium oxide grinding medium - Google Patents
Preparation method of nano-grade zirconium oxide grinding medium Download PDFInfo
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- CN111673632A CN111673632A CN202010576257.7A CN202010576257A CN111673632A CN 111673632 A CN111673632 A CN 111673632A CN 202010576257 A CN202010576257 A CN 202010576257A CN 111673632 A CN111673632 A CN 111673632A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
- B24D18/009—Tools not otherwise provided for
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
- B24D18/0009—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using moulds or presses
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/34—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties
- B24D3/346—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties utilised during polishing, or grinding operation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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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
- C09K3/1409—Abrasive particles per se
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/612—Machining
Abstract
A preparation method of a nano-grade zirconia grinding medium comprises the following steps: selection of 3Y-ZrO2Taking the composite powder as a raw material; reacting 3Y-ZrO2Sending the composite powder into a grinding machine to be ground into slurry with the particle size of 90nm, and then discharging the slurry outwards; adjusting the solid content of the slurry to 65-75%, and adjusting the viscosity of the slurry; the high-voltage electrostatic generator is used for generating static electricity, the anode and the cathode of the high-voltage electrostatic generator are respectively connected with the metal titration disc and the metal reaction kettle, and the slurry is sent to the metal titrationFilling reaction liquid in a metal reaction kettle to ensure that the slurry has positive charges and the reaction liquid has negative charges; the slurry is dripped from the metal titration disc to the reaction kettle by the attraction of positive and negative charges for reaction and forming to form titration microbeads; drying and sintering the titration microbeads to form spherical cores; selecting 500-600 mesh ball cores for frosting treatment; rolling and molding the frosted ball core to 0.1mm of microbeads by a wet method; the finished product of the nano-grinding zirconium beads is prepared by airing, drying, binder removal, sintering, polishing and screening the ball blank. The zirconia beads prepared by the method have the characteristics of compact and uniform internal structure, good wear resistance and high grinding efficiency.
Description
Technical Field
The invention belongs to the technical field of ceramic materials in inorganic nonmetallic materials, and particularly relates to a preparation method of a nano-grade zirconia grinding medium.
Background
The zirconia grinding medium has high density, high strength and toughness, excellent wear resistance and high grinding efficiency, can prevent material pollution, is especially suitable for wet grinding and dispersing, and is widely applied to the industrial fields of ceramics, magnetic materials, coatings, printing ink, medicines, foods and the like. For example: high-grade automobile paint, mobile phone paint, ink-jet ink, high-grade cosmetics and the like.
With the progress of modern technology level, the execution standard of the chemical industry is higher and higher, and the grinding fineness of many industries is required to be in a nanometer level, so the requirement on the grinding medium is higher and higher. At present, the nano-grade zirconia beads on the market are mainly imported from Japan and Korean, the price is very expensive, the selling price of one kilogram can reach ten thousand yuan, and the zirconium beads produced in China can only be ground to the submicron grade at most. The beads prepared by the traditional wet rolling forming method have the defects of heart rotting phenomenon, insufficient density and poor wear resistance in the internal structure. The nanometer zirconia beads prepared by the titration forming process have flat roundness and lower grinding efficiency.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a nano-grade zirconia grinding medium, and the obtained zirconia beads have compact and uniform internal structure, good wear resistance and high grinding efficiency.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a nano-grade zirconia grinding medium comprises the following steps:
selection of 3Y-ZrO2Taking the composite powder as a raw material;
reacting 3Y-ZrO2Sending the composite powder into a grinding machine to be ground into slurry with the particle size of 90nm, and then discharging the slurry outwards;
adjusting the solid content of the slurry to 65-75%, and adjusting the viscosity of the slurry;
generating static electricity by using a high-voltage static electricity generator, respectively connecting the anode and the cathode of the high-voltage static electricity generator with a metal titration disc and a metal reaction kettle, feeding slurry into the metal titration disc, and filling reaction liquid in the metal reaction kettle to ensure that the slurry has positive charges and the reaction liquid has negative charges; the slurry is dripped from the metal titration disc to the reaction kettle by the attraction of positive and negative charges for reaction and forming to form titration microbeads;
drying and sintering the titration microbeads to form spherical cores;
selecting 500-600 mesh ball cores for frosting treatment;
rolling and molding the frosted ball core to 0.1mm of microbeads by a wet method;
the finished product of the nano-grinding zirconium beads is prepared by airing, drying, binder removal, sintering, polishing and screening the ball blank.
The 3Y-ZrO2The composite powder is prepared by the following steps:
the molar ratio of 94: zirconium oxychloride ZrOCl of 62Yttrium chloride YCl3And 50% concentration of urea CO (NH)2)2The mixed aqueous solution is used as a reaction precursor;
heating in a high-pressure reactor to decompose OH-ions from urea to form Zr (OH)4-Y(OH)3A mixture solution;
then the oxidation reaction is continued in the high-pressure reaction kettle to generate Y2O3-ZrO2Separating, washing and drying to prepare 3Y-ZrO2And (3) compounding powder.
When the viscosity of the slurry is adjusted, 0.05% -0.1% of sodium carboxymethyl cellulose is added for adjustment.
When the wet rolling molding is carried out, firstly, 500-sand 600-mesh spherical cores are placed in a zirconium-aluminum grinding tank, and 100-sand 400-mesh calcined alumina powder is added for dry grinding;
and then, adding the granulation powder below a 500-mesh sieve into the frosted spherical cores with the surface provided with the burrs, and rolling and molding the mixture to form the microbeads with the diameter of 0.1mm by a wet method.
The high-voltage electrostatic device is a 12000V high-voltage electrostatic generator.
The zirconium oxychloride ZrOCl2Yttrium chloride YCl3And urea CO (NH)2)2When the mixed aqueous solution is treated in the high-pressure reaction kettle, the temperature of the high-pressure reaction kettle is kept at 200-350 ℃, and the pressure is kept at 10-15 Mpa.
The invention adopts 3Y-ZrO2The composite powder is used as a raw material, and the nano-micron zirconium beads prepared by the high-voltage electrostatic titration forming process are sintered and ground to prepare spherical cores with approximate sizes and smoothness. And then the prepared ball core is subjected to wet rolling molding to prepare the superfine microspheres with compact internal structure, high grinding efficiency and good wear resistance.
Detailed Description
The following detailed description of the invention is provided to enable further understanding of the nature and technical means of the invention, as well as the specific objects and functions attained by the invention.
The invention discloses a preparation method of a nano-grade zirconia grinding medium, which comprises the following steps:
selection of 3Y-ZrO2The composite powder is used as raw material. The 3Y-ZrO is prepared by a hydrothermal method2The composite powder material specifically comprises: the molar ratio of 94: zirconium oxychloride ZrOCl of 62Yttrium chloride YCl3And urea CO (NH)2)2The mixed aqueous solution is used as a reaction precursor; heating in a high-pressure reactor to decompose OH-ions from urea to form Zr (OH)4-Y(OH)3A mixture solution; then continuously reacting in a high-pressure reaction kettle to generate Y2O3-ZrO2Separating, washing and drying to prepare 3Y-ZrO2And (3) compounding powder.
Reacting 3Y-ZrO2Sending the composite powder into a grinder to be ground into slurry with the particle size of 90nm, and then discharging the slurry outwards.
Adjusting the solid content of the slurry to 65-75%, adjusting the viscosity of the slurry, and adding sodium carboxymethyl cellulose into the slurry, wherein the amount of the added sodium carboxymethyl cellulose is 0.05-0.1% of the slurry.
Generating static electricity by using a 12000V high-voltage static electricity generator, respectively connecting the anode and the cathode of the high-voltage static electricity generator with a metal titration disc and a metal reaction kettle, wherein the metal titration disc is positively charged, the metal reaction kettle is negatively charged, slurry is fed into the metal titration disc to enable the slurry to be positively charged, and reaction liquid is filled in the metal reaction kettle to enable the reaction liquid to be negatively charged; and the slurry is quickly dripped from the metal titration disc to the reaction kettle for reaction and forming by utilizing the attraction of positive and negative charges to form the titration micro-beads.
And drying and sintering the titration micro-beads to form a spherical core.
Selecting 500-sand 600-mesh spherical cores, placing the spherical cores in a zirconium-aluminum grinding tank, and adding 100-sand 400-mesh calcined alumina powder for dry grinding treatment.
And then, adding the granulation powder below a 500-mesh sieve into the frosted spherical cores with the surface provided with the burrs, and rolling and molding the mixture to form the microbeads with the diameter of 0.1mm by a wet method.
The nano-grinding zirconium beads with compact and uniform internal structure, good wear resistance and high grinding efficiency are prepared by airing, drying, binder removal, sintering, polishing and screening the ball blank.
The zirconium oxychloride ZrOCl2Yttrium chloride YCl3And urea CO (NH)2)2When the mixed aqueous solution is treated in the high-pressure reaction kettle, the temperature of the high-pressure reaction kettle is kept at 200-350 ℃, and the pressure is kept at 10-15Mpa, so that the whole reaction process is ensured to be effectively carried out.
Although the present invention has been described in detail with reference to the embodiments, it will be apparent to those skilled in the art that modifications, equivalents, improvements, and the like can be made in the technical solutions of the foregoing embodiments or in some of the technical features of the foregoing embodiments, but those modifications, equivalents, improvements, and the like are all within the spirit and principle of the present invention.
Claims (6)
1. A preparation method of a nano-grade zirconia grinding medium comprises the following steps:
selection of 3Y-ZrO2Taking the composite powder as a raw material;
reacting 3Y-ZrO2Sending the composite powder into a grinding machine to be ground into slurry with the particle size of 90nm, and then discharging the slurry outwards;
adjusting the solid content of the slurry to 65-75%, and adjusting the viscosity of the slurry;
generating static electricity by using a high-voltage static electricity generator, respectively connecting the anode and the cathode of the high-voltage static electricity generator with a metal titration disc and a metal reaction kettle, feeding slurry into the metal titration disc, and filling reaction liquid in the metal reaction kettle to ensure that the slurry has positive charges and the reaction liquid has negative charges; the slurry is dripped from the metal titration disc to the reaction kettle by the attraction of positive and negative charges for reaction and forming to form titration microbeads;
drying and sintering the titration microbeads to form spherical cores;
selecting 500-600 mesh ball cores for frosting treatment;
rolling and molding the frosted ball core to 0.1mm of microbeads by a wet method;
the finished product of the nano-grinding zirconium beads is prepared by airing, drying, binder removal, sintering, polishing and screening the ball blank.
2. The method of preparing nanoscale zirconia grinding media as in claim 1, wherein the 3Y-ZrO is2The composite powder is prepared by the following steps:
the molar ratio of 94: zirconium oxychloride ZrOCl of 62Yttrium chloride YCl3And 50% concentration of urea CO (NH)2)2The mixed aqueous solution is used as a reaction precursor;
heating in a high-pressure reactor to decompose OH-ions from urea to form Zr (OH)4-Y(OH)3A mixture solution;
then continue at highOxidation reaction in the pressure reactor to produce Y2O3-ZrO2Separating, washing and drying to prepare 3Y-ZrO2And (3) compounding powder.
3. The method of claim 2, wherein the adjusting the viscosity of the slurry is performed by adding 0.05% to 0.1% sodium carboxymethylcellulose.
4. The method for preparing nano-scale zirconia grinding medium according to claim 3, wherein when the wet rolling molding is performed, the 500-sand 600-mesh ball core is placed in a zirconia-alumina grinding tank, and the 100-sand 400-mesh calcined alumina powder is added for dry grinding;
and then, adding the granulation powder below a 500-mesh sieve into the frosted spherical cores with the surface provided with the burrs, and rolling and molding the mixture to form the microbeads with the diameter of 0.1mm by a wet method.
5. The method of claim 4, wherein the high voltage electrostatic device is a 12000V high voltage electrostatic generator.
6. The method of claim 5, wherein the zirconium oxychloride ZrOCl2Yttrium chloride YCl3And urea CO (NH)2)2When the mixed aqueous solution is treated in the high-pressure reaction kettle, the temperature of the high-pressure reaction kettle is kept at 200-350 ℃, and the pressure is kept at 10-15 Mpa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608148A (en) * | 2020-12-19 | 2021-04-06 | 安徽致磨新材料科技有限公司 | Zirconium silicate grinding medium and preparation method thereof |
| CN114181628A (en) * | 2021-11-01 | 2022-03-15 | 深圳艾利佳材料科技有限公司 | Low-cost porous titanium alloy metallographic polishing reagent and polishing process |
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| US4719091A (en) * | 1986-07-01 | 1988-01-12 | Corning Glass Works | Preparation of mono-sized zirconia powders by forced hydrolysis |
| KR910011361A (en) * | 1989-12-30 | 1991-08-07 | 정명식 | Method for producing alumina-zirconia composite with excellent sinterability and mechanical properties |
| CN101037337A (en) * | 2007-04-27 | 2007-09-19 | 淄博启明星新材料有限公司 | Preparation method of micro crystal wearable ceramic ball |
| CN108673707A (en) * | 2018-05-10 | 2018-10-19 | 河源帝诺新材料有限公司 | A kind of zirconium oxide microballon high-pressure electrostatic attraction titration former |
| CN110240195A (en) * | 2019-07-09 | 2019-09-17 | 中国科学院广州地球化学研究所 | A kind of preparation method of monoclinic zirconia nanometer product |
| CN110835263A (en) * | 2019-10-31 | 2020-02-25 | 中国船舶重工集团公司第七二五研究所 | Method for preparing zirconia ceramic microspheres |
-
2020
- 2020-06-22 CN CN202010576257.7A patent/CN111673632A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4719091A (en) * | 1986-07-01 | 1988-01-12 | Corning Glass Works | Preparation of mono-sized zirconia powders by forced hydrolysis |
| KR910011361A (en) * | 1989-12-30 | 1991-08-07 | 정명식 | Method for producing alumina-zirconia composite with excellent sinterability and mechanical properties |
| CN101037337A (en) * | 2007-04-27 | 2007-09-19 | 淄博启明星新材料有限公司 | Preparation method of micro crystal wearable ceramic ball |
| CN108673707A (en) * | 2018-05-10 | 2018-10-19 | 河源帝诺新材料有限公司 | A kind of zirconium oxide microballon high-pressure electrostatic attraction titration former |
| CN110240195A (en) * | 2019-07-09 | 2019-09-17 | 中国科学院广州地球化学研究所 | A kind of preparation method of monoclinic zirconia nanometer product |
| CN110835263A (en) * | 2019-10-31 | 2020-02-25 | 中国船舶重工集团公司第七二五研究所 | Method for preparing zirconia ceramic microspheres |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608148A (en) * | 2020-12-19 | 2021-04-06 | 安徽致磨新材料科技有限公司 | Zirconium silicate grinding medium and preparation method thereof |
| CN114181628A (en) * | 2021-11-01 | 2022-03-15 | 深圳艾利佳材料科技有限公司 | Low-cost porous titanium alloy metallographic polishing reagent and polishing process |
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