CN111848184A - High-aluminum-content magnesia-alumina spinel transparent ceramic powder and preparation method thereof - Google Patents
High-aluminum-content magnesia-alumina spinel transparent ceramic powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 123
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000000919 ceramic Substances 0.000 title claims abstract description 78
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 61
- 239000011029 spinel Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000012043 crude product Substances 0.000 claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 34
- 239000010439 graphite Substances 0.000 claims abstract description 34
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 33
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 32
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 21
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 16
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical group [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 126
- 239000000395 magnesium oxide Substances 0.000 claims description 63
- 239000002002 slurry Substances 0.000 claims description 50
- 238000007873 sieving Methods 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000011812 mixed powder Substances 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 16
- 238000000498 ball milling Methods 0.000 claims description 14
- 238000001238 wet grinding Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000009837 dry grinding Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000010419 fine particle Substances 0.000 abstract 1
- 229910003023 Mg-Al Inorganic materials 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 229910001873 dinitrogen Inorganic materials 0.000 description 8
- 238000011049 filling Methods 0.000 description 8
- 238000011068 loading method Methods 0.000 description 8
- 230000001681 protective effect Effects 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
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- 239000012071 phase Substances 0.000 description 7
- 238000001513 hot isostatic pressing Methods 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- -1 magnesium aluminate Chemical class 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000003746 solid phase reaction Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 238000001272 pressureless sintering Methods 0.000 description 2
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- 229910017109 AlON Inorganic materials 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
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- 238000000975 co-precipitation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
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- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 108010025899 gelatin film Proteins 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
The invention discloses magnesia-alumina spinel transparent ceramic powder with high aluminum content and a preparation method thereof. The molecular formula of the transparent ceramic powder is MgO. nAl2O3Wherein n is more than or equal to 2.33 and less than or equal to 3.22, and n is Al2O3Molar ratio to MgO. The preparation method comprises the following steps: 1) mixing MgO powder and alpha-Al2O3The method comprises the following steps of pretreating and mixing the powder, placing the powder in a graphite mold, placing the graphite mold in a high-current reaction synthesis device, keeping the pressure of inert gas not more than 0.05MPa, applying high current of 12-15 kA, heating the graphite mold to 1700-1900 ℃ at the heating rate of 100-500 ℃/min, preserving the heat for 5-30 min, cooling the graphite mold at the rate of 30-40 ℃/min to obtain a block crude product, and performing post-treatment to obtain the transparent ceramic powder. The method has the advantages of simple process and high synthesis efficiency, and the obtained transparent ceramic powder has high purity, good dispersibility and uniform and fine particle size, and is suitable for preparing transparent ceramics.
Description
Technical Field
The invention belongs to the technical field of synthesis and preparation of ceramic materials, and particularly relates to magnesia-alumina spinel transparent ceramic powder with high aluminum content and a preparation method thereof.
Background
The magnesium aluminate spinel transparent ceramic material has high melting point, wear resistance, corrosion resistance and excellent electrical insulation performance, has wide light transmission range, covers the region from near ultraviolet to medium infrared light, but has lower mechanical performance compared with sapphire, AlON and other materials, and limits the application field of the material; the magnesium aluminate spinel as a solid solution has the property changed with the stoichiometry, which provides a basis for regulating and controlling the material property by changing the composition technically. When the aluminum oxide enters spinel lattice in a solid solution mode, the lattice constant is reduced, the mechanical property of the spinel lattice is improved, and therefore the magnesia-alumina spinel transparent ceramic is expected to meet the requirements of different application fields on the performance, such as infrared window materials and transparent armors in military use, and high-pressure lamp tubes, light-heat exchangers and the like in civil use.
At present, there are two main methods for preparing magnesia-alumina spinel transparent ceramics, one is a reaction sintering method, also called a one-step method, which generally uses alumina powder and magnesia powder as raw materials, and directly obtains the magnesia-alumina spinel transparent ceramics through reaction sintering after mixing. And the second step is a two-step method, namely, firstly synthesizing single-phase magnesia-alumina spinel transparent ceramic powder by taking alumina powder and magnesia powder as raw materials, and then sintering to obtain the transparent ceramic. Compared with the two methods, the reaction sintering method is more convenient, but the sintering and reaction processes in the method are difficult to control, the problems of second phase, volume expansion and the like are easy to generate, and the high-quality magnesia-alumina spinel transparent ceramic is difficult to prepare. The two-step method does not have the problems and is more beneficial to preparing high-quality magnesia-alumina spinel transparent ceramic with complex shape, but the key problem is to prepare high-performance magnesia-alumina spinel transparent ceramic powder.
Dericoglu et al (Derciglu AF, Boccaccini AR, Dlouhy I, Kagawa Y. Effect of chemical composition on the optical properties and less than biological property of magnetic alumina ceramics [ J]Materials transformations, 2005,46(3): 996-. Through research, when the value of n is 1, the prepared magnesia-alumina spinel scatters lightThe coefficient is the largest. When the value of n is increased, the transmittance is also increased. And when the n value is 2, the fracture toughness is highest and reaches 2.02 MPa.m1/2. Furthermore, Yuan et Al (pressureless/hot isostatic pressing sintering of MgO.1.5 Al2O3 transparent ceramics [ J]Inorganic materials bulletin, 2015, 30 (08): 843-2O3The powder is used as a raw material, MgO.1.5 Al2O3 transparent ceramic powder with high purity and small average grain diameter is synthesized at 1550 ℃, and then pressureless sintering is combined with hot isostatic pressing sintering at 1800 ℃ at 1650 ℃, and the transparent ceramic with the Vickers hardness of 12.75GPa and the transmittance of a visible waveband of 70 percent is prepared. Zhang et Al (He Zhang, Hao Wang, HonggangGu, Xiao Zong, BingTian Tu, Pengyu Xu, et Al. reproduction of MgO.18Al2O3spinel transparentceramics by aqueous gelcasting,presintering and hot isostatic pressing[J]Journal of the European Ceramic Society,2018,46(03):100-2O3The powder is taken as a raw material, single-phase MgO.1.8 Al2O3 transparent ceramic powder is synthesized by utilizing a solid-phase reaction at 1680 ℃, researches show that the powder is easy to combine water molecules in a hydrogen bond form to form a hydration film due to the existence of strong polar hydroxyl on the surface, so that the powder is easy to agglomerate and settle in water, the problem of dispersion of the powder in water is solved by modifying the powder by using stearic acid and a surfactant Tween 80, and the MgO.1.8 Al transparent ceramic powder with the size of 18 x 14 x 11mm and the visible light wave band transmittance of 80 percent is successfully prepared by finally adopting a gel film injection molding mode and a presintering pressureless and hot isostatic pressing sintering mode2O3A transparent ceramic. Guo Sheng Qiang, Wang Hao, Ling Tian, Wang bin, Xupengyu, Wang Min, Fu Zheng, Fine grain MgO.1.44 Al2O3Preparation of transparent ceramics and Performance Studies [ J]Inorganic materials bulletin, 2019, 34 (10): 1067-1071)) in high purity with commercial MgO (99.99 wt%) and α -Al2O3(99.99 wt%) as raw material, and through solid-phase reaction at 1680 deg.C, high-purity fine MgO.16Al is obtained2O3Transparent ceramic powder, then using spark plasma sintering to make formation and pre-densification, then making pressureless sintering to obtain sinteringFinal stage, hot isostatic pressing at 180MPa and 1500 deg.c for 5 hr to prepare fine crystalline MgO.1.44 Al2O3The transparent ceramic has an average crystal grain of 1.9 μm, a Vickers hardness of 13.94GPa, and a transmittance in the visible wavelength band of 70%.
The existing preparation methods for magnesium aluminate spinel transparent ceramic powder mainly comprise a high-temperature solid phase method, a coprecipitation method, a sol-gel method and the like, but the MgO. nAl2O3The transparent ceramic powder has n value in the range of 1-2, and n is>2, the regional spinel transparent ceramic powder is less studied. In order to further improve the performance of the magnesium aluminate spinel transparent ceramic by regulating and controlling the composition, the solid solution range of the magnesium aluminate spinel transparent ceramic needs to be enlarged, so that MgO & nAl with high n value is prepared2O3The transparent ceramic powder is particularly significant, and the prepared high-quality magnesia-alumina spinel transparent ceramic powder is the basis for the subsequent preparation of high-performance magnesia-alumina spinel transparent ceramic.
Disclosure of Invention
The invention aims to provide magnesia-alumina spinel transparent ceramic powder with high aluminum content and a preparation method thereof.
In order to solve the technical problems, the invention provides the following technical scheme:
provides a high aluminum content magnesia alumina spinel transparent ceramic powder, the molecular formula of the transparent ceramic powder is MgO. nAl2O3Wherein n is more than or equal to 2.33 and less than or equal to 3.22, and n is Al2O3Molar ratio to MgO.
According to the scheme, the average grain diameter of the transparent ceramic powder is 200 nm-1 mu m.
The preparation method of the magnesia-alumina spinel transparent ceramic powder with high aluminum content comprises the following steps:
1) with MgO powder and alpha-Al2O3The powder is taken as a raw material, and is ball-milled, dried and sieved after being mixed in proportion to obtain mixed powder;
2) placing the mixed powder obtained in the step 1) in a graphite mold, and then placing the graphite mold in a high-current reaction synthesis device, wherein inert gas with the gas pressure not more than 0.05MPa is filled in the high-current reaction synthesis device; directly applying a large current of 12-15 kA to a graphite mold, heating to 1700-1900 ℃ at a heating rate of 100-500 ℃/min, preserving heat for 5-30 min, and cooling at a rate of 30-40 ℃/min to obtain a block crude product;
3) crushing and screening the massive crude product obtained in the step 2), then performing ball milling twice, performing dry milling and wet milling, and drying and screening after the wet milling is finished to obtain the magnesia-alumina spinel transparent ceramic powder with high aluminum content.
According to the scheme, in the step 1), alpha-Al2O3The average particle size of the powder is below 200 nm; the average particle diameter of the MgO powder is 300nm or less.
According to the scheme, in the step 1), MgO powder and alpha-Al are mixed2O3Adding the powder into absolute ethyl alcohol and alumina balls, then carrying out ball milling for not less than 24 hours to obtain slurry, drying for 10-15 hours at 50-70 ℃, and then sieving with a 100-mesh sieve to obtain mixed powder.
According to the scheme, the volume-to-mass ratio of the absolute ethyl alcohol to the raw material is 400-500 ml:180g, and the mass ratio of the alumina balls to the raw material is 4-5: 1.
According to the scheme, in the step 2), the inert gas is nitrogen or argon.
According to the scheme, in the step 3), the massive crude product obtained in the step 2) is crushed and then sieved by a 50-mesh sieve; adding alumina balls for dry milling for not less than 24h, and adding absolute ethyl alcohol for wet milling for not less than 48 h; drying after ball milling, and then sieving with a 200-mesh sieve to obtain the magnesia-alumina spinel transparent ceramic powder with high aluminum content.
According to the scheme, the mass ratio of the alumina balls to the massive crude products is 5-6: 1; the volume-mass ratio of the absolute ethyl alcohol to the massive crude product is 300-500 ml:180 g.
According to the scheme, the drying conditions are as follows: drying for 10-15 h at 50-70 ℃.
The invention has the following beneficial effects:
1. the invention is based on alpha-Al2O3The high-temperature solid-phase reaction with MgO two phases purifies and activates the surface of the raw material powder under the action of large current, and the high temperature rise rate and temperature are matched to ensure that the raw material powder undergoes rapid solid-phase reaction, thereby greatly improving the conversion rate of the reaction; and the crystal grain growth of the product is greatly inhibited due to the rapid heating and cooling rate and the short reaction time in the synthesis process, the high-aluminum-content magnesia-alumina spinel transparent ceramic powder which is difficult to obtain by the conventional method and has accurate component control can be synthesized, the powder particles are uniform and fine, the process is simple, the preparation speed is high, the preparation can be completed within about 1 hour, the efficiency is high, the energy consumption is low, and the yield is high.
2. In the high-aluminum-content magnesia-alumina spinel transparent ceramic powder provided by the invention, Al2O3The molar ratio of the aluminum powder to MgO is 2.33-3.22, the aluminum content is high, the powder particles are uniform and fine, the average particle size can be below 1 mu m, the dispersibility is good, the purity is high, and the method is suitable for preparing high-performance transparent ceramics.
Description of the drawings:
FIG. 1 is an XRD spectrum of a high aluminum content magnesia alumina spinel transparent ceramic powder prepared in examples 1, 5 and 7 of the present invention.
FIG. 2 is an SEM photograph of a magnesia alumina spinel transparent ceramic powder prepared in example 1 of the present invention.
FIG. 3 is an SEM photograph of a magnesia alumina spinel transparent ceramic powder prepared in example 5 of the present invention.
FIG. 4 is an SEM photograph of a magnesia alumina spinel transparent ceramic powder prepared in example 7 of the present invention.
Detailed Description
The following examples are intended to further illustrate the process features of the present invention and are not intended to limit the invention thereto.
alpha-Al used in the following examples2O3The average particle size of the powder is about 100 nm; the average particle size of the MgO powder is about 180 nm.
Example 1
A transparent ceramic powder of high-Al content Mg-Al spinel with MgO.2133Al molecular formula2O3The preparation method comprises the following steps:
1) firstly, weighing alpha-Al according to the proportion in the molecular formula2O3153.924g of powder and 26.102g of MgO powder are added into 720g of alumina balls and 500ml of absolute ethyl alcohol for ball milling for 24 hours to obtain slurry; taking out the slurry, drying the slurry for 12 hours at 50 ℃ under a vacuum condition, and then sieving the dried slurry with a 100-mesh sieve to obtain mixed powder;
2) loading the mixed powder obtained in the step 1) into a graphite mold, placing the graphite mold in a high-current reaction synthesis device, filling high-purity nitrogen gas of 0.05MPa into the high-current reaction synthesis device as protective gas, directly applying 15kA high current to the graphite mold, keeping the synthesis temperature at 1700 ℃, the heating rate at 500 ℃/min, keeping the temperature for 15min, and cooling at 40 ℃/min to obtain a block crude product;
3) crushing the massive crude product obtained in the step 2) by using agate, and then sieving the crushed massive crude product with a 50-mesh sieve; adding 850g of alumina balls into the sieved powder, carrying out dry grinding for 24h, and then adding 400ml of absolute ethyl alcohol, carrying out wet grinding for 48h, thus obtaining slurry; taking out the slurry, drying for 12h at 50 ℃ under vacuum condition, and sieving with a 200-mesh sieve to obtain the magnesia-alumina spinel transparent ceramic powder with high aluminum content.
XRD of the high aluminum content magnesia alumina spinel transparent ceramic powder prepared in example 1 is shown in FIG. 1, which shows that: the obtained powder has single-phase MgO.2133Al2O3。
FIG. 2 is an SEM of a high aluminum content magnesia alumina spinel transparent ceramic powder showing: the average grain diameter of the powder particles is 200 nm-1 mu m, and the powder particles are uniform, fine and good in dispersibility.
Example 2
A transparent ceramic powder of high-Al content Mg-Al spinel with MgO.2133Al molecular formula2O3The preparation method comprises the following steps:
1) firstly, weighing alpha-Al according to the proportion in the molecular formula2O3153.924g of powder and 26.102g of MgO powder are added into 720g of alumina balls and 500ml of absolute ethyl alcohol for ball milling for 24 hours to obtain slurry; taking out the slurry, drying the slurry for 12 hours at 70 ℃ under a vacuum condition, and then sieving the dried slurry with a 100-mesh sieve to obtain mixed powder;
2) loading the mixed powder obtained in the step 1) into a graphite mold, placing the graphite mold in a high-current reaction synthesis device, filling high-purity nitrogen gas of 0.05MPa into the high-current reaction synthesis device as protective gas, directly applying 13kA high current to the graphite mold, wherein the synthesis temperature is 1800 ℃, the heating rate is 200 ℃/min, the heat preservation is 5min, and the temperature is reduced at the rate of 35 ℃/min to obtain a block crude product;
3) crushing the massive crude product obtained in the step 2) by using agate, and then sieving the crushed massive crude product with a 50-mesh sieve; adding 960g of alumina balls into the sieved powder, carrying out dry grinding for 48h, and then adding 400ml of absolute ethyl alcohol, carrying out wet grinding for 72h, thus obtaining slurry; taking out the slurry, drying at 70 deg.C for 12 hr under vacuum condition, sieving with 200 mesh sieve to obtain MgO.2.33 Al2O3The magnesia-alumina spinel transparent ceramic powder with high aluminum content.
Example 3
A transparent ceramic powder of high-Al content Mg-Al spinel with MgO.2.71 Al molecular formula2O3The preparation method comprises the following steps:
1) firstly, weighing alpha-Al according to the proportion in the molecular formula2O3157.118g of powder and 22.905g of MgO powder are added into 720g of alumina balls and 500ml of absolute ethyl alcohol for ball milling for 24 hours to obtain slurry; taking out the slurry, drying the slurry at 50 ℃ under a vacuum condition, and then sieving the dried slurry with a 100-mesh sieve to obtain mixed powder;
2) loading the mixed powder obtained in the step 1) into a graphite mold, placing the graphite mold in a high-current reaction synthesis device, filling high-purity nitrogen gas of 0.05MPa into the high-current reaction synthesis device as protective gas, directly applying high current of 14kA to the graphite mold, keeping the synthesis temperature at 1750 ℃, increasing the temperature at 400 ℃/min, keeping the temperature for 20min, and cooling at 32 ℃/min to obtain a block crude product;
3) crushing the massive crude product obtained in the step 2) by using agate, and then sieving the crushed massive crude product with a 50-mesh sieve; adding 960g of alumina balls into the sieved powder, carrying out dry grinding for 48h, and then adding 300ml of absolute ethyl alcohol, carrying out wet grinding for 72h, thus obtaining slurry; taking out the slurry, drying at 50 deg.C under vacuum condition, and sieving with 200 mesh sieve to obtain MgO.2.71 Al2O3The magnesia-alumina spinel transparent ceramic powder with high aluminum content.
Example 4
A transparent ceramic powder of high-Al content Mg-Al spinel with MgO.2.71 Al molecular formula2O3The preparation method comprises the following steps:
1) firstly, weighing alpha-Al according to the proportion in the molecular formula2O3157.118g of powder and 22.905g of MgO powder are added into 720g of alumina balls and 500ml of absolute ethyl alcohol for ball milling for 24 hours to obtain slurry; taking out the slurry, drying the slurry at 70 ℃ under a vacuum condition, and then sieving the dried slurry with a 100-mesh sieve to obtain mixed powder;
2) loading the mixed powder obtained in the step 1) into a graphite mold, placing the graphite mold in a high-current reaction synthesis device, filling high-purity nitrogen gas of 0.05MPa into the high-current reaction synthesis device as protective gas, directly applying 12kA high current to the graphite mold, keeping the synthesis temperature at 1825 ℃, the heating rate at 150 ℃/min, keeping the temperature for 10min, and cooling at 36 ℃/min to obtain a block crude product;
3) crushing the massive crude product obtained in the step 2) by using agate, and then sieving the crushed massive crude product with a 50-mesh sieve; adding 960g of alumina balls into the sieved powder, carrying out dry grinding for 48h, and then adding 300ml of absolute ethyl alcohol, carrying out wet grinding for 72h, thus obtaining slurry; taking out the slurry, drying at 70 deg.C under vacuum condition, sieving with 200 mesh sieve to obtain MgO.2.71 Al powder2O3The magnesia-alumina spinel transparent ceramic powder with high aluminum content.
Example 5
A transparent ceramic powder of high-Al content Mg-Al spinel with MgO.295 Al molecular formula2O3The preparation method comprises the following steps:
1) firstly, weighing alpha-Al according to the proportion in the molecular formula2O3158.722g of powder and 21.299g of MgO powder are added into 720g of alumina balls and 500ml of absolute ethyl alcohol for ball milling for 24 hours to obtain slurry; taking out the slurry, drying the slurry at 50 ℃ under a vacuum condition, and then sieving the dried slurry with a 100-mesh sieve to obtain mixed powder;
2) loading the mixed powder obtained in the step 1) into a graphite mold, placing the graphite mold in a high-current reaction synthesis device, filling high-purity nitrogen gas of 0.05MPa into the high-current reaction synthesis device as protective gas, directly applying 13kA high current to the graphite mold, keeping the synthesis temperature at 1780 ℃, the heating rate at 175 ℃/min, keeping the temperature for 25min, and cooling at 34 ℃/min to obtain a block-shaped crude product;
3) crushing the massive crude product obtained in the step 2) by using agate, and then sieving the crushed massive crude product with a 50-mesh sieve; adding 960g of alumina balls into the sieved powder, carrying out dry grinding for 48h, and then adding 300ml of absolute ethyl alcohol, carrying out wet grinding for 72h, thus obtaining slurry; taking out the slurry, drying at 50 ℃ under vacuum condition, and sieving with a 200-mesh sieve to obtain the magnesia-alumina spinel transparent ceramic powder with high aluminum content.
XRD of the high aluminum content magnesia alumina spinel transparent ceramic powder prepared in example 1 is shown in FIG. 1, which shows that: the obtained powder has single-phase MgO.2.95 Al component2O3。
FIG. 3 is an SEM of a high aluminum content magnesia alumina spinel transparent ceramic powder showing: the powder particles are uniform and fine, the average particle size is 200 nm-1 mu m, and the dispersibility is good.
Example 6
A transparent ceramic powder of high-Al content Mg-Al spinel with MgO.295 Al molecular formula2O3The preparation method comprises the following steps:
1) firstly, weighing alpha-Al according to the proportion in the molecular formula2O3158.722g of powder and 21.299g of MgO powder are added into 720g of alumina balls and 500ml of absolute ethyl alcohol for ball milling for 24 hours to obtain slurry; taking out the slurry, drying the slurry at 70 ℃ under a vacuum condition, and then sieving the dried slurry with a 100-mesh sieve to obtain mixed powder;
2) loading the mixed powder obtained in the step 1) into a graphite mold, placing the graphite mold in a high-current reaction synthesis device, filling high-purity nitrogen gas of 0.05MPa into the high-current reaction synthesis device as protective gas, directly applying high current of 14kA to the graphite mold, keeping the synthesis temperature at 1850 ℃, keeping the temperature at 250 ℃/min, keeping the temperature for 10min, and cooling at 38 ℃/min to obtain a block crude product;
3) crushing the massive crude product obtained in the step 2) by using agate, and then sieving the crushed massive crude product with a 50-mesh sieve; adding 960g of alumina balls into the sieved powder, carrying out dry grinding for 48h, and then adding 300ml of absolute ethyl alcohol, carrying out wet grinding for 72h, thus obtaining slurry; taking out the slurry, drying at 70 deg.C under vacuum condition, sieving with 200 mesh sieve to obtain MgO.2.95 Al2O3The magnesia-alumina spinel transparent ceramic powder with high aluminum content.
Example 7
A transparent ceramic powder of high-Al content Mg-Al spinel with MgO.3. 22Al molecular formula2O3The preparation method comprises the following steps:
1) firstly, weighing alpha-Al according to the proportion in the molecular formula2O3160.331g of powder and 19.689g of MgO powder are added into 720g of alumina balls and 500ml of absolute ethyl alcohol for ball milling for 24 hours to obtain slurry; taking out the slurry, drying the slurry at 50 ℃ under a vacuum condition, and then sieving the dried slurry with a 100-mesh sieve to obtain mixed powder;
2) loading the mixed powder obtained in the step 1) into a graphite mold, placing the graphite mold in a high-current reaction synthesis device, filling high-purity nitrogen gas of 0.05MPa into the high-current reaction synthesis device as protective gas, directly applying 13kA high current to the graphite mold, keeping the synthesis temperature at 1800 ℃, the heating rate at 150 ℃/min, keeping the temperature for 25min, and cooling at 35 ℃/min to obtain a block crude product;
3) crushing the massive crude product obtained in the step 2) by using agate, and then sieving the crushed massive crude product with a 50-mesh sieve; adding 960g of alumina balls into the sieved powder, carrying out dry grinding for 48h, and then adding 300ml of absolute ethyl alcohol, carrying out wet grinding for 72h, thus obtaining slurry; taking out the slurry, drying at 50 ℃ under vacuum condition, and sieving with a 200-mesh sieve to obtain the magnesia-alumina spinel transparent ceramic powder with high aluminum content.
XRD of the high aluminum content magnesia alumina spinel transparent ceramic powder prepared in example 1 is shown in FIG. 1, which shows that: the obtained powder has single-phase MgO.3.22 Al2O3。
FIG. 4 is an SEM of a high aluminum content magnesia alumina spinel transparent ceramic powder showing: the powder particles are uniform and fine, the average particle size is 200 nm-1 mu m, and the dispersibility is good.
Example 8
A transparent ceramic powder of high-Al content Mg-Al spinel with MgO.3. 22Al molecular formula2O3The preparation method comprises the following steps:
1) firstly, weighing alpha-Al according to the proportion in the molecular formula2O3160.331g of powder and 19.689g of MgO powder are added into 720g of alumina balls and 500ml of absolute ethyl alcohol for ball milling for 24 hours to obtain slurry; taking out the slurry, drying the slurry at 70 ℃ under a vacuum condition, and then sieving the dried slurry with a 100-mesh sieve to obtain mixed powder;
2) loading the mixed powder obtained in the step 1) into a graphite mold, placing the graphite mold in a high-current reaction synthesis device, filling high-purity nitrogen gas of 0.05MPa into the high-current reaction synthesis device as protective gas, directly applying high current of 14kA to the graphite mold, keeping the synthesis temperature at 1900 ℃, the heating rate at 300 ℃/min, keeping the temperature for 10min, and cooling at 40 ℃/min to obtain a blocky crude product;
3) crushing the massive crude product obtained in the step 2) by using agate, and then sieving the crushed massive crude product with a 50-mesh sieve; adding 960g of alumina balls into the sieved powder, carrying out dry grinding for 48h, and then adding 300ml of absolute ethyl alcohol, carrying out wet grinding for 72h, thus obtaining slurry; taking out the slurry, drying at 70 deg.C under vacuum condition, sieving with 200 mesh sieve to obtain MgO.3.22 Al2O3The magnesia-alumina spinel transparent ceramic powder with high aluminum content.
It is apparent that the above embodiments are only examples for clearly illustrating and do not limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are therefore intended to be included within the scope of the invention as claimed.
Claims (10)
1. The transparent ceramic powder of the magnesia-alumina spinel with high aluminum content is characterized in that the molecular formula of the transparent ceramic powder is MgO. nAl2O3Wherein n is more than or equal to 2.33 and less than or equal to 3.22, and n is Al2O3Molar ratio to MgO.
2. The high aluminum content magnesia alumina spinel transparent ceramic powder of claim 1, wherein the transparent ceramic powder has an average particle size of 200nm to 1 μm.
3. A method for preparing the magnesia alumina spinel transparent ceramic powder with high aluminum content according to claim 1 or 2, which is characterized by comprising the following steps:
1) with MgO powder and alpha-Al2O3The powder is taken as a raw material, and is ball-milled, dried and sieved after being mixed in proportion to obtain mixed powder;
2) placing the mixed powder obtained in the step 1) in a graphite mold, and then placing the graphite mold in a high-current reaction synthesis device, wherein inert gas with the gas pressure not more than 0.05MPa is filled in the high-current reaction synthesis device; directly applying a large current of 12-15 kA to a graphite mold, heating to 1700-1900 ℃ at a heating rate of 100-500 ℃/min, preserving heat for 5-30 min, and cooling at a rate of 30-40 ℃/min to obtain a block crude product;
3) crushing and screening the massive crude product obtained in the step 2), then performing ball milling twice, performing dry milling and wet milling, and drying and screening after the wet milling is finished to obtain the magnesia-alumina spinel transparent ceramic powder with high aluminum content.
4. The method according to claim 3, wherein in the step 1), α -Al2O3The average particle size of the powder is below 200 nm; the average particle diameter of the MgO powder is 300nm or less.
5. The method according to claim 3, wherein in the step 1), MgO powder and α -Al are mixed2O3Adding the powder into absolute ethyl alcohol and alumina balls, then carrying out ball milling for not less than 24 hours to obtain slurry, drying for 10-15 hours at 50-70 ℃, and then sieving with a 100-mesh sieve to obtain mixed powder.
6. The preparation method according to claim 5, wherein the volume-to-volume mass ratio of the absolute ethanol to the raw material is 400-500 ml:180g, and the mass ratio of the alumina balls to the raw material is 4-5: 1.
7. The method according to claim 3, wherein in the step 2), the inert gas is nitrogen or argon.
8. The preparation method according to claim 3, wherein in the step 3), the massive crude product obtained in the step 2) is crushed and then is sieved by a 50-mesh sieve; adding alumina balls for dry milling for not less than 24h, and adding absolute ethyl alcohol for wet milling for not less than 48 h; drying after ball milling, and then sieving with a 200-mesh sieve to obtain the magnesia-alumina spinel transparent ceramic powder with high aluminum content.
9. The preparation method of claim 8, wherein the mass ratio of the alumina balls to the massive crude product is 5-6: 1; the volume-mass ratio of the absolute ethyl alcohol to the massive crude product is 300-500 ml:180 g.
10. The method of claim 8, wherein the drying conditions are: drying for 10-15 h at 50-70 ℃.
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