CN116283242A - Preparation method of metal-ceramic composite grinding medium with adjustable density - Google Patents
Preparation method of metal-ceramic composite grinding medium with adjustable density Download PDFInfo
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- CN116283242A CN116283242A CN202310394184.3A CN202310394184A CN116283242A CN 116283242 A CN116283242 A CN 116283242A CN 202310394184 A CN202310394184 A CN 202310394184A CN 116283242 A CN116283242 A CN 116283242A
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- 238000000227 grinding Methods 0.000 title claims abstract description 47
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 239000000919 ceramic Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000004005 microsphere Substances 0.000 claims abstract description 48
- 238000001354 calcination Methods 0.000 claims abstract description 40
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 29
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 21
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000010431 corundum Substances 0.000 claims abstract description 15
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 15
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 13
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 13
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 13
- 239000005642 Oleic acid Substances 0.000 claims abstract description 13
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 13
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 13
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 13
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 13
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000002002 slurry Substances 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 25
- 239000012153 distilled water Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 17
- 238000003825 pressing Methods 0.000 claims description 16
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 10
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000012716 precipitator Substances 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 description 19
- 238000005299 abrasion Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 239000004927 clay Substances 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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- 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
- C04B35/10—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 aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/20—Disintegrating members
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
- C01F7/308—Thermal decomposition of nitrates
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention relates to the technical field of grinding media, and discloses a preparation method of a metal-ceramic composite grinding medium with adjustable density, which uses urea as a precipitator, oleic acid as a surfactant, aluminum nitrate is subjected to hydrothermal reaction and calcination to generate micro-nano alumina microspheres, and then the micro-nano alumina microspheres are sintered with gadolinium nitrate and a sintering aid to obtain gadolinium doped alumina microspheres, wherein gadolinium is doped into crystal lattices of alumina, so that the bonding strength of crystal interfaces of the alumina is improved, and the strength and hardness of the alumina microspheres are improved. Gadolinium doped alumina microsphere is used as main component of grinding medium and nano zirconia, and is compounded with corundum, kaolin, calcium carbonate and nano silica, and the metal-ceramic composite grinding medium with adjustable density is obtained by optimizing and adjusting proportion, the raw materials are cheap and easy to obtain, the cost is low, and the composite grinding medium has the advantages of high hardness, low wear rate and adjustable density.
Description
Technical Field
The invention relates to the technical field of grinding media, in particular to a preparation method of a metal-ceramic composite grinding medium with adjustable density.
Background
The alumina has strong high temperature resistance, excellent wear resistance, good corrosion resistance, low price and easy obtainment, can be used as a grinding medium, can be widely applied to the fields of building industry, metallurgy industry, printing ink coating and the like, and has the advantages of high hardness, high strength, low abrasion and adjustable density in order to meet the requirements of industrial production, the development of the high-hardness and high-wear-resistance alumina grinding medium is a research hot spot, and the patent CN115340369B 'ternary complex-phase wear-resistant ceramic ball and the preparation method thereof' discloses a ternary complex-phase wear-resistant ceramic ball prepared by taking alumina, zirconium silicate, nano-zirconia, talcum, lanthanum oxide and the like as raw materials.
Patent CN107312499B discloses a metal and ceramic composite grinding medium for a ball mill and a preparation method thereof, and discloses the metal and ceramic composite grinding medium which comprises a metal core and an outer ceramic layer coated on the outer peripheral surface of the metal core, wherein the metal and the ceramic are combined together to achieve the aim of changing the density of a grinding body, and the wear resistance of the grinding body is improved under the condition of not reducing the grinding efficiency. The invention aims to prepare a metal-ceramic composite grinding medium with high hardness, low wear rate and adjustable density by taking micro-nano alumina microspheres, gadolinium nitrate, nano zirconia, corundum and the like as raw materials.
Disclosure of Invention
(one) solving the technical problems
The invention provides a preparation method of a metal-ceramic composite grinding medium with high hardness, low wear rate and adjustable density.
(II) technical scheme
A preparation method of a metal-ceramic composite grinding medium with adjustable density comprises the following steps:
(1) Adding aluminum nitrate and urea into distilled water, stirring and dissolving, adding ethanol and surfactant oleic acid, transferring the solution into a hydrothermal reaction kettle, carrying out heat preservation reaction, filtering the solution after the reaction, washing with deionized water, and finally placing the materials into a tubular furnace, and calcining in an air atmosphere to obtain micro-nano alumina microspheres;
(2) Adding micro-nano alumina microspheres, gadolinium nitrate, a sintering aid and ethanol into a ball mill for ball milling, then drying ball milling slurry, placing the materials into a cold isostatic press for pressing until the materials are pressed, and finally placing the materials into a tubular furnace for sintering in air atmosphere to obtain gadolinium doped alumina microspheres;
(3) Adding zirconium oxychloride into a sodium hydroxide solution, adding cetyltrimethylammonium bromide, heating the solution to 60-90 ℃ for reaction for 6-18h, filtering after the reaction, washing the solution to neutrality by deionized water, then placing the product into a tube furnace, calcining the product in an air atmosphere, and controlling the calcining temperature to 800-1000 ℃ for 2-3h to obtain the nano zirconium oxide.
(4) Adding gadolinium doped alumina microsphere, nanometer zirconia, corundum, kaolin, calcium carbonate, nanometer silica and distilled water into a ball mill for ball milling, drying ball milling slurry, placing the ball milling slurry into a cold isostatic press for pressing to be spherical, placing the ball milling slurry into a tubular furnace for calcining in air atmosphere, and controlling the calcining temperature to 1250-1400 ℃ for 2-3 hours to obtain the metal-ceramic composite grinding medium with adjustable density.
Preferably, the weight ratio of the aluminum nitrate, the urea and the oleic acid in the step (1) is 100:120-180:400-750.
Preferably, the temperature of the heat preservation reaction in the step (1) is 180-210 ℃ and the time is 3-8h.
Preferably, the calcination temperature in the step (1) is 600-800 ℃ and the time is 3-5h.
Preferably, the weight ratio of the micro-nano alumina microspheres, gadolinium nitrate and sintering aid in the step (2) is 97-99.5:0.2-1.5:0.3-1.5.
Preferably, the sintering aid in (2) comprises calcium oxide, magnesium oxide, manganese dioxide or titanium dioxide.
Preferably, the sintering temperature in the step (2) is 1350-1600 ℃ and the time is 3-6h.
Preferably, the pH of the sodium hydroxide solution in (2) is 9-10.
Preferably, the weight ratio of the zirconium oxychloride to the cetyltrimethylammonium bromide in the step (3) is 100:150-320.
Preferably, the weight ratio of gadolinium doped alumina microsphere, nano zirconia, corundum, kaolin, calcium carbonate and nano silica in the step (4) is 40-75:5-12:10-18:4-10:12-20:4-10.
(III) beneficial technical effects
Urea is used as a precipitator, oleic acid is used as a surfactant, aluminum nitrate is subjected to hydrothermal reaction and calcination to generate micro-nano aluminum oxide microspheres, and then the micro-nano aluminum oxide microspheres are sintered with gadolinium nitrate and a sintering aid to obtain gadolinium doped aluminum oxide microspheres, gadolinium is doped into crystal lattices of aluminum oxide, the bonding strength of crystal interfaces of aluminum oxide is improved, and the strength and hardness of the aluminum oxide microspheres are improved. Gadolinium doped alumina microsphere and nano zirconia are used as main components of the grinding medium, corundum, kaolin, calcium carbonate and nano silica are compounded, and the metal-ceramic composite grinding medium with adjustable density is obtained by optimizing and adjusting the proportion, so that the raw materials are cheap and easy to obtain, the cost is low, and the composite grinding medium has the advantages of high hardness, low wear rate and adjustable density.
Drawings
FIG. 1 is a scanning electron microscope image of gadolinium doped alumina microspheres.
Fig. 2 is a scanning electron microscope image of nano zirconia.
Detailed Description
Example 1
(1) Adding 0.2g of aluminum nitrate and 0.24g of urea into distilled water, stirring and dissolving, adding ethanol and 0.8g of surfactant oleic acid, transferring the solution into a hydrothermal reaction kettle, reacting at 200 ℃ for 3 hours while maintaining the temperature, filtering the solution after the reaction, washing with deionized water, finally placing the materials into a tubular furnace, calcining in air atmosphere, controlling the temperature to 800 ℃ and the time to 3 hours, and obtaining the micro-nano alumina microspheres.
(2) 199g of micro-nano alumina microspheres, 0.4g of gadolinium nitrate, 0.6g of sintering aid calcium oxide and ethanol are added into a ball mill for ball milling, then ball milling slurry is dried, the materials are placed into a cold isostatic press for pressing until reaching, finally the materials are placed into a tubular furnace for sintering in air atmosphere, the temperature is controlled to 1600 ℃, and the time is 3 hours, so that the gadolinium-doped alumina microspheres are obtained.
(3) Adding 2g of zirconium oxychloride into a sodium hydroxide solution with the pH value of 10, then adding 4.6g of cetyltrimethylammonium bromide, heating the solution to 80 ℃ for reaction for 12 hours, filtering after the reaction, washing deionized water to be neutral, then placing the product into a tubular furnace for calcination in an air atmosphere, and controlling the calcination temperature to 800 ℃ for 3 hours to obtain the nano zirconium oxide.
(4) 550g of gadolinium doped alumina microsphere, 50g of nano zirconia, 120g of corundum, 40g of kaolin, 120g of calcium carbonate, 40g of nano silica and distilled water are added into a ball mill for ball milling, then the ball milling slurry is dried and then is placed into a cold isostatic press for pressing to be spherical, finally, the ball milling slurry is placed into a tubular furnace for calcination in air atmosphere, the temperature is controlled to be 1400 ℃, and the time is 2 hours, so that the metal-ceramic composite grinding medium with adjustable density is obtained.
Example 2
(1) Adding 0.2g of aluminum nitrate and 0.3g of urea into distilled water, stirring and dissolving, adding ethanol and 1g of surfactant oleic acid, transferring the solution into a hydrothermal reaction kettle, reacting at 210 ℃ for 3 hours under heat preservation, filtering the solution after the reaction, washing with deionized water, finally placing the materials into a tubular furnace, calcining in air atmosphere, controlling the temperature to 700 ℃ and the time to 4 hours, and obtaining the micro-nano alumina microspheres.
(2) Adding 197.5g of micro-nano alumina microspheres, 1g of gadolinium nitrate, 1.5g of sintering aid magnesium oxide and ethanol into a ball mill for ball milling, then drying ball milling slurry, placing the materials into a cold isostatic press for pressing until reaching, finally placing the materials into a tubular furnace for sintering in air atmosphere, controlling the temperature to 1600 ℃ and the time to 4 hours, and obtaining the gadolinium doped alumina microspheres.
(3) Adding 2g of zirconium oxychloride into a sodium hydroxide solution with the pH value of 10, adding 3g of cetyltrimethylammonium bromide, heating the solution to 60 ℃ for reaction for 12 hours, filtering after the reaction, washing deionized water to be neutral, placing the product into a tube furnace, calcining in an air atmosphere, and controlling the calcining temperature to 900 ℃ for 3 hours to obtain the nano zirconium oxide.
(4) Adding 500g of gadolinium doped alumina microspheres, 120g of nano zirconia, 120g of corundum, 40g of kaolin clay, 150g of calcium carbonate, 50g of nano silica and distilled water into a ball mill for ball milling, drying the ball milling slurry, placing the ball milling slurry into a cold isostatic press for pressing to be spherical, placing the ball milling slurry into a tubular furnace, calcining the ball milling slurry in an air atmosphere, and controlling the temperature to be 1400 ℃ and the time to be 2 hours to obtain the metal-ceramic composite grinding medium with adjustable density.
Example 3
(1) Adding 0.2g of aluminum nitrate and 0.36g of urea into distilled water, stirring and dissolving, adding ethanol and 1.5g of surfactant oleic acid, transferring the solution into a hydrothermal reaction kettle, reacting at 210 ℃ for 3 hours while maintaining the temperature, filtering the solution after the reaction, washing with deionized water, finally placing the materials into a tubular furnace, calcining in air atmosphere, controlling the temperature to 800 ℃ and the time to 3 hours, and obtaining the micro-nano alumina microspheres.
(2) Adding 195.5g of micro-nano alumina microspheres, 2g of gadolinium nitrate, 2.5g of sintering aid titanium dioxide and ethanol into a ball mill for ball milling, then drying ball milling slurry, placing the materials into a cold isostatic press for pressing until reaching, finally placing the materials into a tubular furnace for sintering in air atmosphere, controlling the temperature to 1500 ℃ and the time to 6 hours, and obtaining the gadolinium doped alumina microspheres.
(3) Adding 2g of zirconium oxychloride into a sodium hydroxide solution with the pH value of 10, then adding 5.5g of cetyltrimethylammonium bromide, heating the solution to 80 ℃ for reaction for 6 hours, filtering after the reaction, washing deionized water to be neutral, then placing the product into a tubular furnace for calcining in an air atmosphere, and controlling the calcining temperature to 1000 ℃ for 3 hours to obtain the nano zirconium oxide.
(4) 750g of gadolinium doped alumina microsphere, 120g of nano zirconia, 120g of corundum, 100g of kaolin, 200g of calcium carbonate, 100g of nano silica and distilled water are added into a ball mill for ball milling, then the ball milling slurry is dried and then is placed into a cold isostatic press for pressing to be spherical, finally, the ball milling slurry is placed into a tubular furnace for calcination in air atmosphere, the temperature is controlled to be 1400 ℃, and the time is 3 hours, so that the metal-ceramic composite grinding medium with adjustable density is obtained.
Example 4
(1) Adding 0.2g of aluminum nitrate and 0.36g of urea into distilled water, stirring and dissolving, adding ethanol and 1.2g of surfactant oleic acid, transferring the solution into a hydrothermal reaction kettle, reacting at 180 ℃ for 5 hours while maintaining the temperature, filtering the solution after the reaction, washing with deionized water, finally placing the materials into a tubular furnace, calcining in air atmosphere, controlling the temperature to 750 ℃ and the time to 5 hours, and obtaining the micro-nano alumina microspheres.
(2) Adding 194g of micro-nano alumina microspheres, 3g of gadolinium nitrate, 3g of sintering aid manganese dioxide and ethanol into a ball mill for ball milling, then drying ball milling slurry, placing the materials into a cold isostatic press for pressing to a certain temperature, finally placing the materials into a tube furnace for sintering in air atmosphere, controlling the temperature to 1600 ℃ and the time to 6 hours, and obtaining the gadolinium doped alumina microspheres.
(3) Adding 2g of zirconium oxychloride into a sodium hydroxide solution with the pH value of 10, then adding 3g of cetyltrimethylammonium bromide, heating the solution to 60 ℃ for reaction for 18 hours, filtering after the reaction, washing deionized water to be neutral, then placing the product into a tube furnace for calcining in air atmosphere, controlling the calcining temperature to 900 ℃ and the time to 2 hours, and obtaining the nano zirconium oxide.
(4) 600g of gadolinium doped alumina microsphere, 100g of nano zirconia, 150g of corundum, 80g of kaolin, 150g of calcium carbonate, 50g of nano silica and distilled water are added into a ball mill for ball milling, then the ball milling slurry is dried and then is placed into a cold isostatic press for pressing to be spherical, finally, the ball milling slurry is placed into a tubular furnace for calcination in air atmosphere, the temperature is controlled to be 1400 ℃, and the time is 2 hours, so that the metal-ceramic composite grinding medium with adjustable density is obtained.
Example 5
(1) Adding 0.2g of aluminum nitrate and 0.3g of urea into distilled water, stirring and dissolving, adding ethanol and 0.8g of surfactant oleic acid, transferring the solution into a hydrothermal reaction kettle, reacting at 190 ℃ for 3 hours while maintaining the temperature, filtering the solution after the reaction, washing with deionized water, finally placing the materials into a tubular furnace, calcining in air atmosphere, controlling the temperature to 800 ℃ and the time to 4 hours, and obtaining the micro-nano alumina microspheres.
(2) 198.6g of micro-nano alumina microspheres, 0.4g of gadolinium nitrate, 1g of sintering aid calcium oxide and ethanol are added into a ball mill for ball milling, then ball milling slurry is dried, the materials are placed into a cold isostatic press for pressing until reaching, finally the materials are placed into a tubular furnace for sintering in air atmosphere, the temperature is controlled to be 1500 ℃, and the time is 3 hours, so that the gadolinium-doped alumina microspheres are obtained.
(3) Adding 2g of zirconium oxychloride into a sodium hydroxide solution with the pH value of 9, then adding 6.4g of cetyltrimethylammonium bromide, heating the solution to 60 ℃ for reaction for 12 hours, filtering after the reaction, washing deionized water to be neutral, then placing the product into a tubular furnace for calcining in an air atmosphere, and controlling the calcining temperature to 1000 ℃ for 2 hours to obtain the nano zirconium oxide.
(4) 600g of gadolinium doped alumina microspheres, 55g of nano zirconia, 150g of corundum, 40g of kaolin clay, 100g of calcium carbonate, 60g of nano silica and distilled water are added into a ball mill for ball milling, then the ball milling slurry is dried and then is placed into a cold isostatic press for pressing to be spherical, finally, the ball milling slurry is placed into a tubular furnace for calcination in air atmosphere, the temperature is controlled to be 1300 ℃, and the time is controlled to be 2 hours, so that the metal-ceramic composite grinding medium with adjustable density is obtained.
Comparative example 1
(1) Adding 0.2g of aluminum nitrate and 0.25g of urea into distilled water, stirring and dissolving, adding ethanol and 1.5g of surfactant oleic acid, transferring the solution into a hydrothermal reaction kettle, reacting at 210 ℃ for 3 hours while maintaining the temperature, filtering the solution after the reaction, washing with deionized water, finally placing the materials into a tubular furnace, calcining in air atmosphere, controlling the temperature to 700 ℃ and the time to 5 hours, and obtaining the micro-nano alumina microspheres.
(2) Adding 2g of zirconium oxychloride into a sodium hydroxide solution with the pH value of 10, then adding 3.5g of cetyltrimethylammonium bromide, heating the solution to 90 ℃ for reaction for 18 hours, filtering after the reaction, washing deionized water to be neutral, then placing the product into a tubular furnace for calcining in an air atmosphere, and controlling the calcining temperature to 800 ℃ for 2 hours to obtain the nano zirconium oxide.
(3) 750g of micro-nano alumina microspheres, 80g of nano zirconia, 120g of corundum, 40g of kaolin, 140g of calcium carbonate, 75g of nano silica and distilled water are added into a ball mill for ball milling, then the ball milling slurry is dried and then is placed into a cold isostatic press for pressing to be spherical, finally, the ball milling slurry is placed into a tubular furnace for calcination in air atmosphere, the temperature is controlled to be 1300 ℃, and the time is 3 hours, so that the composite grinding medium is obtained.
Comparative example 2
(1) Adding 0.2g of aluminum nitrate and 0.36g of urea into distilled water, stirring and dissolving, adding ethanol and 1g of surfactant oleic acid, transferring the solution into a hydrothermal reaction kettle, reacting at 200 ℃ for 3 hours under heat preservation, filtering the solution after the reaction, washing with deionized water, finally placing the materials into a tubular furnace, calcining in air atmosphere, controlling the temperature to 650 ℃ and the time to 4 hours, and obtaining the micro-nano alumina microspheres.
(3) 650g of micro-nano alumina microspheres, 120g of corundum, 40g of kaolin, 200g of calcium carbonate, 60g of nano silicon dioxide and distilled water are added into a ball mill for ball milling, then the ball milling slurry is dried and then is placed into a cold isostatic press for pressing to be spherical, finally, the ball milling slurry is placed into a tubular furnace for calcination in air atmosphere, and the temperature is controlled to be 1300 ℃ for 3 hours, thus obtaining the composite grinding medium.
The abrasion resistance of the composite grinding medium is tested by adopting a rolling method, the composite grinding medium is weighed to obtain M, then distilled water is put into a corundum tank, ball milling is carried out in a ball mill, the ball milling time T is regulated and controlled, the composite grinding medium is taken out, the surface residues are washed off and dried, and then the M is obtained by weighing 1 The wear rate was calculated.
Wear rate q= (M-M 1 )/(M·T)×100%。
The density of the composite grinding media was measured by drainage, 5 times per sample, and averaged.
The Rockwell hardness of the composite grinding media was determined using a Rockwell hardness tester.
Density (g/cm) 3 ) | Wear rate (%/h) | Rockwell Hardness (HRA) | |
Example 1 | 3.85 | 0.0382 | 74.5 |
Example 2 | 3.12 | 0.0403 | 73.8 |
Example 3 | 3.62 | 0.0365 | 79.6 |
Example 4 | 3.30 | 0.0346 | 76.9 |
Example 5 | 3.47 | 0.0380 | 76.6 |
Comparative example 1 | 3.53 | 0.0598 | 72.2 |
Comparative example 2 | 3.47 | 0.0560 | 70.7 |
The metal-ceramic composite grinding media prepared in examples 1-4 have the advantages of adjustable density, first abrasion rate, good abrasion resistance and large hardness, the lowest abrasion rate is 0.0346%/h, and the maximum Rockwell hardness is 79.6%.
Claims (10)
1. A preparation method of a metal-ceramic composite grinding medium with adjustable density is characterized by comprising the following steps of: the preparation method comprises the following steps:
(1) Adding aluminum nitrate and urea into distilled water, stirring and dissolving, adding ethanol and surfactant oleic acid, transferring the solution into a hydrothermal reaction kettle, carrying out heat preservation reaction, filtering the solution after the reaction, washing with deionized water, and finally placing the materials into a tubular furnace, and calcining in an air atmosphere to obtain micro-nano alumina microspheres;
(2) Adding micro-nano alumina microspheres, gadolinium nitrate, a sintering aid and ethanol into a ball mill for ball milling, then drying ball milling slurry, placing the materials into a cold isostatic press for pressing until the materials are pressed, and finally placing the materials into a tubular furnace for sintering in air atmosphere to obtain gadolinium doped alumina microspheres;
(3) Adding zirconium oxychloride into a sodium hydroxide solution, adding cetyltrimethylammonium bromide, heating the solution to 60-90 ℃ for reaction for 6-18h, filtering after the reaction, washing deionized water to be neutral, then placing the product into a tubular furnace, calcining in an air atmosphere, controlling the calcining temperature to 800-1000 ℃ and the time to 2-3h, and obtaining nano zirconium oxide;
(4) Adding gadolinium doped alumina microsphere, nanometer zirconia, corundum, kaolin, calcium carbonate, nanometer silica and distilled water into a ball mill for ball milling, drying ball milling slurry, placing the ball milling slurry into a cold isostatic press for pressing to be spherical, placing the ball milling slurry into a tubular furnace for calcining in air atmosphere, and controlling the calcining temperature to 1250-1400 ℃ for 2-3 hours to obtain the metal-ceramic composite grinding medium with adjustable density.
2. The method for preparing a density-adjustable metal-ceramic composite grinding medium according to claim 1, wherein the method comprises the following steps: the weight ratio of the aluminum nitrate to the urea to the oleic acid in the step (1) is 100:120-180:400-750.
3. The method for preparing a density-adjustable metal-ceramic composite grinding medium according to claim 1, wherein the method comprises the following steps: the temperature of the heat preservation reaction in the step (1) is 180-210 ℃ and the time is 3-8h.
4. The method for preparing a density-adjustable metal-ceramic composite grinding medium according to claim 1, wherein the method comprises the following steps: the calcination temperature in the step (1) is 600-800 ℃ and the time is 3-5h.
5. The method for preparing a density-adjustable metal-ceramic composite grinding medium according to claim 1, wherein the method comprises the following steps: the weight ratio of the micro-nano alumina microspheres to the gadolinium nitrate to the sintering aid in the step (2) is 97-99.5:0.2-1.5:0.3-1.5.
6. The method for preparing a density-adjustable metal-ceramic composite grinding medium according to claim 1, wherein the method comprises the following steps: the sintering aid in (2) comprises calcium oxide, magnesium oxide, manganese dioxide or titanium dioxide.
7. The method for preparing a density-adjustable metal-ceramic composite grinding medium according to claim 1, wherein the method comprises the following steps: the sintering temperature in the step (2) is 1350-1600 ℃ and the sintering time is 3-6h.
8. The method for preparing a density-adjustable metal-ceramic composite grinding medium according to claim 1, wherein the method comprises the following steps: the pH of the sodium hydroxide solution in the step (2) is 9-10.
9. The method for preparing a density-adjustable metal-ceramic composite grinding medium according to claim 1, wherein the method comprises the following steps: the weight ratio of the zirconium oxychloride to the cetyltrimethylammonium bromide in the step (3) is 100:150-320.
10. The method for preparing a density-adjustable metal-ceramic composite grinding medium according to claim 1, wherein the method comprises the following steps: the weight ratio of gadolinium doped alumina microsphere, nanometer zirconia, corundum, kaolin, calcium carbonate and nanometer silica in the step (4) is 40-75:5-12:10-18:4-10:12-20:4-10.
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