CN101209925A - Modified method for aluminum oxide/titanium oxide diphase fine ceramic material - Google Patents
Modified method for aluminum oxide/titanium oxide diphase fine ceramic material Download PDFInfo
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- CN101209925A CN101209925A CNA2007101448941A CN200710144894A CN101209925A CN 101209925 A CN101209925 A CN 101209925A CN A2007101448941 A CNA2007101448941 A CN A2007101448941A CN 200710144894 A CN200710144894 A CN 200710144894A CN 101209925 A CN101209925 A CN 101209925A
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Abstract
The invention relates to a modification method of Al2O3/ TiO2 complex phase fine ceramic material, which relates to ceramic material modification method field; the invention solves the problem of low bending strength, low fracture toughness and low rigidity of Al2O3/ TiO2 complex phase ceramics. The steps of the method are that: fine Al2O3/TiO2 powder, a modifier, adhesive polyvinyl alcohol are blended into uniform slurry in a ball mill by using deionized water as a medium, spray dried and re-granulated, and then the obtained powder is heat treated; the heat treated powder is pre-pressurized and molded; the obtained blank are cool isostatic pressed and molded and sintered. The invention realizes the low temperature rapid sintering of ceramics during the preparation process of fine ceramic material, apparently reduces the production cost, and enhances the bending strength, fracture thoughness and rigidness of manufactured products. The invention is simple and easy for operation and suitable for industrialization.
Description
Technical field
The present invention relates to a kind of method of modifying of stupalith.
Background technology
Stupalith has a wide range of applications in a lot of fields.But its most fatal weakness is high fragility and low reliability, thereby has limited its application in a lot of occasions.How to improve this weakness of stupalith, be the problem that the stupalith investigator is concerned about always.Along with science and technology development, the particularly development of the energy, space technology, also more and more higher to the performance requriements of stupalith.Will significantly reduce the energy consumption in the high-performance ceramic preparation process, obviously reduce its production cost, promote the industrialization of ceramic product, the low temperature Fast Sintering that realizes pottery is crucial.For the structural ceramics powder, general hope is thin more good more, helps high temperature sintering, can reduce firing temperature.But not so, especially for dry pressing, the false granularity of powder is thin more when being shaped, and flowability is bad on the contrary, can not be full of mould, easily produces the cavity, causes the green compact density not high.
At fine alumina (Al
2O
3) a certain amount of titanium oxide (TiO of middle adding
2), they are prepared into fine alumina/titanium oxide (Al of different proportionings
2O
3/ TiO
2) composite oxide power, this class powdered preparation is become block Al
2O
3/ TiO
2Diphase ceramic material, this composite diphase material are expected in the high-abrasive material field, biomaterial (the femoral head position material in the total hip replacement) field obtains to use.Yet performances such as its intensity, toughness are but not high, limited its application.And then the material supply section scholar expects nanotechnology is incorporated into this field, with the fine alumina of nanoscale and titanium dioxide powder again granulation become fine alumina/titanium oxide (Al of nanostructure
2O
3/ TiO
2) composite oxide power and be used to prepare fine structure Al
2O
3/ TiO
2Complex phase ceramic.Studies show that the meticulous Al of this kind
2O
3/ TiO
2The Al of complex phase ceramic and traditional micron order crystal particle scale
2O
3/ TiO
2Complex phase ceramic is compared, and its intensity, toughness and wear resistance all improve, but the meticulous Al of this kind
2O
3-TiO
2The complex phase ceramic mechanical property is low still not ideal enough.
Summary of the invention
The objective of the invention is in order to solve existing Al
2O
3/ TiO
2The problem that the flexural strength of complex phase ceramic, fracture toughness property and hardness performance are low provides a kind of method of modifying of aluminum oxide titanium white multiple phase fine ceramics material.The present invention has realized the low temperature Fast Sintering of pottery in the fine ceramics material preparation process, has obviously reduced production cost, and the performance of flexural strength, fracture toughness property and the hardness of the product of being produced is obviously improved.
The method of modifying of aluminum oxide titanium white multiple phase fine ceramics material of the present invention is as follows: one, mixed powder with 1 weight part, 0.3 the deionized water of～0.5 weight part, 0.009 the abrading-ball of～0.014 parts by weight of adhesive polyvinyl alcohol and 2～4 weight parts is put into ball mill, rotating speed with 1000～1300rpm mixes 3～5h, described mixed powder is by weight by 5～9.9 parts nano aluminium oxide, 0.1 the properties-correcting agent of～5 parts nano-titanium oxide and 0.5～2.5 part is formed, described properties-correcting agent is made up of 0.25～2.25 part nano-cerium oxide and 0.25～2.25 part zirconium white by weight; Two, carry out spraying drying granulation again with mixing back gained slurry in the step 1, obtain the powder that particle diameter is 20～80 μ m, inlet temperature is 220～250 ℃ during spray-drier work, and temperature out is 100～130 ℃, and the nozzle rotating speed is 35000～37000r/min; Three, will be again the powder of the granulation fine alumina crucible of packing into, crucible is put into high temperature box type resistance furnace heat-treat, treating processes is as follows: temperature rise rate is 9～11 ℃/min in the heat treatment process, is warming up to 580～620 ℃ earlier, insulation 50～70min; Heating up reaches 1150～1250 ℃ again, and insulation 50～70min cools to room temperature then with the furnace; Four, powder after the thermal treatment is put into mould, under 80～100MPa pressure, carry out pre-molding, pressurize 2～4min; Five, the blocks behind the pre-molding is put into rubber mold, eliminating gas also encapsulates, and puts into cold isostatic press again, at the 260MPa forming under the pressure, and pressurize 2～4min; Six, gained blank after the isostatic cool pressing is put into resistance furnace, carry out pressureless sintering under 1000～1500 ℃ temperature, sintering time is 50～150min, and temperature rise rate is 5～10 ℃/min, cools to room temperature then with the furnace.
The present invention adopts spray granulation can prepare quality homogeneous, the good ball-type powder of repeatability, shortens the preparation process of powder, also helps automatization, serialization production, is the effective ways of mass preparation advanced ceramics dry mash.Use the meticulous Al that the inventive method is produced
2O
3/ TiO
2/ CeO
2/ ZrO
2Complex phase ceramic and Al
2O
3/ TiO
2Complex phase ceramic is compared the density maximum can improve 12.5%, and flexural strength is Al
2O
3/ TiO
21.3～4.4 times of complex phase ceramic, fracture toughness property is Al
2O
3/ TiO
21.7～2 times of complex phase ceramic, Vickers' hardness is Al
2O
3/ TiO
21.6～3.3 times of complex phase ceramic.
Description of drawings
Fig. 1 is Al under the different sintering temperatures
2O
3/ TiO
2And Al
2O
3/ TiO
2/ CeO
2/ ZrO
2The density design sketch of pottery, Fig. 2 is the flexural strength comparison diagram of the following two kinds of ceramic bodies of different sintering temperatures, and Fig. 3 is the fracture toughness property comparison diagram of the following two kinds of ceramic bodies of different sintering temperatures, and Fig. 4 is the Vickers' hardness comparison diagram of the following two kinds of ceramic bodies of different sintering temperatures.Among Fig. 1-4-■-expression Al
2O
3/ TiO
2Pottery ,-●-expression Al
2O
3/ TiO
2/ CeO
2/ ZrO
2Pottery.
Embodiment
Embodiment one: the method for modifying of aluminum oxide titanium white multiple phase fine ceramics material is as follows in the present embodiment: one, mixed powder with 1 weight part, 0.3 the deionized water of～0.5 weight part, 0.009 the abrading-ball of～0.014 parts by weight of adhesive polyvinyl alcohol and 2～4 weight parts is put into ball mill, rotating speed with 1000～1300rpm mixes 3～5h, described mixed powder is by weight by 5～9.9 parts nano aluminium oxide, 0.1 the properties-correcting agent of～5 parts nano-titanium oxide and 0.5～2.5 part is formed, described properties-correcting agent is made up of 0.25～2.25 part nano-cerium oxide and 0.25～2.25 part zirconium white by weight; Two, carry out spraying drying granulation again with mixing back gained slurry in the step 1, obtain the powder that particle diameter is 20～80 μ m, inlet temperature is 220～250 ℃ during spray-drier work, and temperature out is 100～130 ℃, and the nozzle rotating speed is 35000 ~ 37000r/min; Three, will be again the powder of the granulation fine alumina crucible of packing into, crucible is put into high temperature box type resistance furnace heat-treat, treating processes is as follows: temperature rise rate is 9～11 ℃/min in the heat treatment process, is warming up to 580～620 ℃ earlier, insulation 50～70min; Heating up reaches 1150～1250 ℃ again, and insulation 50～70min cools to room temperature then with the furnace; Four, powder after the thermal treatment is put into mould, under 80～100MPa pressure, carry out pre-molding, pressurize 2～4min; Five, the blocks behind the pre-molding is put into rubber mold, eliminating gas also encapsulates, and puts into cold isostatic press again, at the 260MPa forming under the pressure, and pressurize 2～4min; Six, gained blank after the isostatic cool pressing is put into resistance furnace, carry out pressureless sintering under 1000～1500 ℃ temperature, sintering time is 50～150min, and temperature rise rate is 5～10 ℃/min, cools to room temperature then with the furnace.
In the present embodiment in step 1 used ball mill be AX5 type agitating ball mill; Used spray-drier is a LPG type Highspeedcentrifugingandsprayingdrier in step 2; High temperature box type resistance furnace is the SX-8-16 high temperature box type resistance furnace in step 3; Be to carry out pre-molding in step 4 with YBO4-5 type hand press; Cold isostatic press in step 5 is a LDJ200/1000-300 type cold isostatic press; Used resistance furnace is the SX-8-16 high temperature box type resistance furnace in step 6.
Embodiment two: what present embodiment and embodiment one were different is to be made up of 5.1～8.5 parts nano aluminium oxide, 0.2～1.6 part nano-titanium oxide and 0.6～1.6 part properties-correcting agent by weight at the mixed powder described in the step 1, and other step is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is to be made up of 8.6～9.8 parts nano aluminium oxide, 1.7～4.9 parts nano-titanium oxide and 1.7～2.4 parts properties-correcting agent by weight at the mixed powder described in the step 1, and other step is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is to be made up of 8.7 parts nano aluminium oxide, 1.3 parts nano-titanium oxide and 1.5 parts properties-correcting agent by weight at the mixed powder described in the step 1, and other step is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is to be made up of 9.7 parts nano aluminium oxide, 0.3 part nano-titanium oxide and 1.5 parts properties-correcting agent by weight at the mixed powder described in the step 1, and other step is identical with embodiment one.
Embodiment six: what present embodiment and embodiment one were different is to be made up of 8 parts nano aluminium oxide, 2 parts nano-titanium oxide and 1.5 parts properties-correcting agent by weight at the mixed powder described in the step 1, and other step is identical with embodiment one.
Embodiment seven: what present embodiment and embodiment one were different is to be made up of 6 parts nano aluminium oxide, 4 parts nano-titanium oxide and 1.5 parts properties-correcting agent by weight at the mixed powder described in the step 1, and other step is identical with embodiment one.
Embodiment eight: what present embodiment and embodiment one were different is to be made up of 0.26～0.75 part nano-cerium oxide and 0.26～0.75 part zirconium white by weight at the properties-correcting agent described in the step 1, and other step is identical with embodiment one.
Embodiment nine: what present embodiment and embodiment one were different is to be made up of 0.76～2.24 part nano-cerium oxide and 0.76～2.24 part zirconium white by weight at the properties-correcting agent described in the step 1, and other step is identical with embodiment one.
Embodiment ten: what present embodiment and embodiment one were different is to be made up of 0.8 part nano-cerium oxide and 0.7 part zirconium white by weight at the properties-correcting agent described in the step 1, and other step is identical with embodiment one.
Embodiment 11: present embodiment and embodiment one are different is in step 1 the abrading-ball of deionized water, 0.01 parts by weight of adhesive polyvinyl alcohol and 3 weight parts of the mixed powder of 1 weight part, 0.5 weight part to be put in the ball mill, with the rotating speed mixing 4h of 1200rpm.
Embodiment 12: what present embodiment and embodiment one were different is that inlet temperature is 220～240 ℃ when spray-drier described in the step 2 is worked, temperature out is 100～115 ℃, nozzle rotating speed 35000 ~ 36000r/min, other step is identical with embodiment one.
Embodiment 13: what present embodiment and embodiment one were different is that inlet temperature is 240～250 ℃ when spray-drier described in the step 2 is worked, temperature out is 115～130 ℃, nozzle rotating speed 36000 ~ 37000r/min, other step is identical with embodiment one.
Embodiment 14: what present embodiment and embodiment one were different is that inlet temperature is 230 ℃ when the spray-drier described in the step 2 is worked, temperature out is 110 ℃, nozzle rotating speed 36000r/min, other step is identical with embodiment one.
Embodiment 15: present embodiment and embodiment one are different be in step 3 in the heat treatment process temperature rise rate be 10 ℃/min, be warming up to 600 ℃ earlier, insulation 60min; Reach 1200 ℃ in intensification, insulation 60min cools to room temperature then with the furnace, and other step is identical with embodiment one.
Embodiment 16: what present embodiment and embodiment one were different is in step 4 powder after the thermal treatment to be put into mould, carries out pre-molding under 75MPa pressure, pressurize 3min, and other step is identical with embodiment one.
Embodiment 17: what present embodiment and embodiment one were different is in step 5 the blocks behind the pre-molding to be put into rubber mold, eliminating gas also encapsulates, put into cold isostatic press again, at the 260MPa forming under the pressure, pressurize 3min, other step is identical with embodiment one.
Embodiment 18: what present embodiment and embodiment one were different is in step 6 gained blank after the isostatic cool pressing to be put into resistance furnace, under 1100～1200 ℃ temperature, carry out pressureless sintering, sintering time is 51～75min, temperature rise rate is 6～8 ℃/min, cool to room temperature then with the furnace, other step is identical with embodiment one.
Embodiment 19: what present embodiment and embodiment one were different is in step 6 gained blank after the isostatic cool pressing to be put into resistance furnace, under 1210～1490 ℃ temperature, carry out pressureless sintering, sintering time is 76～149min, temperature rise rate is 8.1～9.9 ℃/min, cool to room temperature then with the furnace, other step is identical with embodiment one.
Embodiment 20: what present embodiment and embodiment one were different is in step 6 gained blank after the isostatic cool pressing to be put into resistance furnace, carry out pressureless sintering, under 1250 ℃, 1350 ℃ or 1450 ℃ of three temperature, carry out pressureless sintering, sintering time is 1h, temperature rise rate is 5 ℃/min, cool to room temperature then with the furnace, other step is identical with embodiment one.
Embodiment 21: Al under the different sintering temperatures in the present embodiment
2O
3/ TiO
2And Al
2O
3/ TiO
2/ CeO
2/ ZrO
2The density of pottery is as follows:
Table 1
| Sintering temperature (℃) | Al 2O 3/TiO 2Density (%) | Al 2O 3/TiO 2/CeO 2/ZrO 2Density (%) |
| 1250 | 70.1 | 72.8 |
| 1350 | 80.2 | 92.4 |
| 1450 | 91.5 | 98.3 |
Find out that from Fig. 2 and table 1 along with increasing of sintering temperature, the density of two kinds of stupaliths increases gradually; When each selected temperature is carried out sintering, the density of stupalith that adds properties-correcting agent is all than added-time height not, and the stupalith that adds properties-correcting agent density during than 1450 ℃ of sintering when 1350 ℃ of sintering is also high, and the sintering temperature that can obviously reduce stupalith behind the adding properties-correcting agent is described.
Embodiment 22: the flexural strength of the following two kinds of ceramic bodies of different sintering temperatures is as follows in the present embodiment:
Table 2
| Sintering temperature (℃) | Al 2O 3/TiO 2Flexural strength (MPa) | Al 2O 3/TiO 2/CeO 2/ZrO 2Flexural strength (MPa) |
| 1250 | 69.3±9.9 | 113.4±10.6 |
| 1350 | 139.4±15.1 | 548.5±10.2 |
| 1450 | 342.6±14.4 | 449.8±15.8 |
Find out that from Fig. 3 and table 2 along with increasing of sintering temperature, the flexural strength of two kinds of stupaliths increases; When each temperature was carried out sintering, the flexural strength of stupalith that adds properties-correcting agent was all than added-time height not, and it is the highest to add the flexural strength of stupalith when 1350 ℃ of sintering of properties-correcting agent.
Embodiment 23: the fracture toughness property of the following two kinds of ceramic bodies of different sintering temperatures is as follows in the present embodiment:
Table 3
| Sintering temperature (℃) | Al 2O 3/TiO 2Fracture toughness property (MPam 1/2) | Al 2O 3/TiO 2/CeO 2/ZrO 2Fracture toughness property (MPam 1/2) |
| 1250 | 0.79±0.21 | 1.52±0.25 |
| 1350 | 1.74±0.04 | 3.04±0.06 |
| 1450 | 3.64±0.04 | 4.33±0.08 |
Find out that from Fig. 4 and table 3 along with increasing of sintering temperature, the fracture toughness property of two kinds of stupaliths all increases gradually, reaches maximum value in the time of 1450 ℃ respectively; When each temperature was carried out sintering, the fracture toughness property of stupalith that adds properties-correcting agent was all than added-time height not.
Embodiment 24: the Vickers' hardness of the following two kinds of ceramic bodies of different sintering temperatures is as follows in the present embodiment:
Table 4
| Sintering temperature (℃) | Al 2O 3/TiO 2Flexural strength (GPa) | Al 2O 3/TiO 2/CeO 2/ZrO 2Flexural strength (GPa) |
| 1250 | 0.81±0.15 | 1.05±0.13 |
| 1350 | 2.96±0.22 | 9.73±0.20 |
| 1450 | 7.77±0.30 | 12.09±0.23 |
Find out that from Fig. 5 and table 4 along with increasing of sintering temperature, the Vickers' hardness of two kinds of stupaliths all increases gradually, reaches maximum value in the time of 1450 ℃ respectively; When each temperature was carried out sintering, the Vickers' hardness of stupalith that adds properties-correcting agent was all than added-time height not.
Claims (10)
1. the method for modifying of an aluminum oxide titanium white multiple phase fine ceramics material, the step that it is characterized in that this method is as follows: one, mixed powder with 1 weight part, 0.3 the deionized water of～0.5 weight part, 0.009 the abrading-ball of～0.014 parts by weight of adhesive polyvinyl alcohol and 2～4 weight parts is put into ball mill, rotating speed with 1000～1300rpm mixes 3～5h, described mixed powder is by weight by 5～9.9 parts nano aluminium oxide, 0.1 the properties-correcting agent of～5 parts nano-titanium oxide and 0.5～2.5 part is formed, described properties-correcting agent is made up of 0.25～2.25 part nano-cerium oxide and 0.25～2.25 part zirconium white by weight; Two, carry out spraying drying granulation again with mixing back gained slurry in the step 1, obtain the powder that particle diameter is 20～80 μ m, inlet temperature is 220～250 ℃ during spray-drier work, and temperature out is 100～130 ℃, and the nozzle rotating speed is 35000 ~ 37000r/min; Three, will be again the powder of the granulation fine alumina crucible of packing into, crucible is put into high temperature box type resistance furnace heat-treat, treating processes is as follows: temperature rise rate is 9～11 ℃/min in the heat treatment process, is warming up to 580～620 ℃ earlier, insulation 50～70min; Heating up reaches 1150～1250 ℃ again, and insulation 50～70min cools to room temperature then with the furnace; Four, powder after the thermal treatment is put into mould, under 80～100MPa pressure, carry out pre-molding, pressurize 2～4min; Five, the blocks behind the pre-molding is put into rubber mold, eliminating gas also encapsulates, and puts into cold isostatic press again, at the 260MPa forming under the pressure, and pressurize 2～4min; Six, gained blank after the isostatic cool pressing is put into resistance furnace, carry out pressureless sintering under 1000～1500 ℃ temperature, sintering time is 50～150min, and temperature rise rate is 5～10 ℃/min, cools to room temperature then with the furnace.
2. the method for modifying of aluminum oxide titanium white multiple phase fine ceramics material according to claim 1 is characterized in that the mixed powder described in the step 1 is made up of 5.1～8.5 parts nano aluminium oxide, 0.2～1.6 part nano-titanium oxide and 0.6～1.6 part properties-correcting agent by weight.
3. the method for modifying of aluminum oxide titanium white multiple phase fine ceramics material according to claim 1 is characterized in that the mixed powder described in the step 1 is made up of 8.6～9.8 parts nano aluminium oxide, 1.7～4.9 parts nano-titanium oxide and 1.7～2.4 parts properties-correcting agent by weight.
4. the method for modifying of aluminum oxide titanium white multiple phase fine ceramics material according to claim 1 is characterized in that the mixed powder described in the step 1 is made up of 8.7 parts nano aluminium oxide, 1.3 parts nano-titanium oxide and 1.5 parts properties-correcting agent by weight.
5. the method for modifying of aluminum oxide titanium white multiple phase fine ceramics material according to claim 1, it is characterized in that the mixed powder described in the step 1 is made up of 9.7 parts nano aluminium oxide, 0.3 part nano-titanium oxide and 1.5 parts properties-correcting agent by weight, other step is identical with embodiment one.
6. the method for modifying of aluminum oxide titanium white multiple phase fine ceramics material according to claim 1 is characterized in that the mixed powder described in the step 1 is made up of 8 parts nano aluminium oxide, 2 parts nano-titanium oxide and 1.5 parts properties-correcting agent by weight.
7. the method for modifying of aluminum oxide titanium white multiple phase fine ceramics material according to claim 1, it is characterized in that the mixed powder described in the step 1 is made up of 6 parts nano aluminium oxide, 4 parts nano-titanium oxide and 1.5 parts properties-correcting agent by weight, other step is identical with embodiment one.
8. the method for modifying of aluminum oxide titanium white multiple phase fine ceramics material according to claim 1 is characterized in that described properties-correcting agent is made up of 0.26～0.75 part nano-cerium oxide and 0.26～0.75 part zirconium white by weight.
9. the method for modifying of aluminum oxide titanium white multiple phase fine ceramics material according to claim 1 is characterized in that described properties-correcting agent is made up of 0.76～2.24 part nano-cerium oxide and 0.76～2.24 part zirconium white by weight.
10. the method for modifying of aluminum oxide titanium white multiple phase fine ceramics material according to claim 1 is characterized in that described properties-correcting agent is made up of 0.8 part nano-cerium oxide and 0.7 part zirconium white by weight.
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101898894A (en) * | 2010-04-29 | 2010-12-01 | 中国科学院上海硅酸盐研究所 | Method for preparing beta-Al2O3 precursor powder by spray drying taking water as medium |
| CN101590525B (en) * | 2009-07-02 | 2011-01-26 | 哈尔滨工业大学 | Amorphous-nanocrystalline ceramic composite powder preparation method |
| CN103171024A (en) * | 2011-12-20 | 2013-06-26 | 萍乡市金刚科技有限责任公司 | Wear-resisting aluminum oxide ceramic ball isostatic pressing process and special device |
| CN103386303A (en) * | 2013-07-25 | 2013-11-13 | 中国石油化工股份有限公司 | Hydrogenation catalyst and preparation method thereof |
| CN113292324A (en) * | 2021-06-18 | 2021-08-24 | 中国船舶重工集团公司第七二五研究所 | Preparation method of solid spherical AT13 spray-coated feed without screening |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1978385A (en) * | 2005-12-09 | 2007-06-13 | 中国科学院兰州化学物理研究所 | Nano ceramic water-base gel casting method |
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2007
- 2007-12-21 CN CN2007101448941A patent/CN101209925B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101590525B (en) * | 2009-07-02 | 2011-01-26 | 哈尔滨工业大学 | Amorphous-nanocrystalline ceramic composite powder preparation method |
| CN101898894A (en) * | 2010-04-29 | 2010-12-01 | 中国科学院上海硅酸盐研究所 | Method for preparing beta-Al2O3 precursor powder by spray drying taking water as medium |
| CN101898894B (en) * | 2010-04-29 | 2013-01-16 | 上海电气钠硫储能技术有限公司 | Method for preparing beta-Al2O3 precursor powder by spray drying taking water as medium |
| CN103171024A (en) * | 2011-12-20 | 2013-06-26 | 萍乡市金刚科技有限责任公司 | Wear-resisting aluminum oxide ceramic ball isostatic pressing process and special device |
| CN103171024B (en) * | 2011-12-20 | 2014-12-24 | 萍乡市金刚科技有限责任公司 | Wear-resisting aluminum oxide ceramic ball isostatic pressing process and special device |
| CN103386303A (en) * | 2013-07-25 | 2013-11-13 | 中国石油化工股份有限公司 | Hydrogenation catalyst and preparation method thereof |
| CN103386303B (en) * | 2013-07-25 | 2016-03-02 | 中国石油化工股份有限公司 | A kind of hydrogenation catalyst and preparation method thereof |
| CN113292324A (en) * | 2021-06-18 | 2021-08-24 | 中国船舶重工集团公司第七二五研究所 | Preparation method of solid spherical AT13 spray-coated feed without screening |
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|---|---|
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