CN106342083B - A kind of low temperature is prepared the method for aluminum nitride oxygen transparent ceramic - Google Patents
A kind of low temperature is prepared the method for aluminum nitride oxygen transparent ceramicInfo
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- CN106342083B CN106342083B CN201010049105.8A CN201010049105A CN106342083B CN 106342083 B CN106342083 B CN 106342083B CN 201010049105 A CN201010049105 A CN 201010049105A CN 106342083 B CN106342083 B CN 106342083B
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- aluminum nitride
- transparent ceramic
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- oxygen transparent
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Abstract
The present invention relates to a kind of low temperature and prepare the method for aluminum nitride oxygen transparent ceramic. Step is as follows: (1) is prepared one and contained by Y2O3Or other rare earth oxide and SiO2The aluminium oxynitride powder of the sintering aid of composition; (2) powder obtaining is sieved, compression molding isostatic cool pressing; (3) biscuit of preparation is put into carbon shirt-circuiting furnace and vacuumize after be filled with high pure nitrogen. Furnace temperature is warming up to 1750～1900 DEG C by the speed of 5～25 DEG C/min, and is incubated 4～48 hours. Preparation temperature of the present invention is low, has reduced well the loss of electric power and stove, has correspondingly reduced to a great extent the preparation cost of aluminum nitride oxygen transparent ceramic, prepares aluminum nitride oxygen transparent ceramic transmitance in 45% left and right.
Description
Technical field
The present invention relates to a kind of low temperature and prepare the method for aluminum nitride oxygen transparent ceramic, this crystalline ceramics can be widely used in military and civilianField.
Background technology
(G.YamaguchiH.Yanagida, " Study on the since the people such as Yamaguchi start to report γ-AlON pottery
Reductive Spinel-A New Spinel Formula AlN-Al2O3instead of the Previous one Al3O4”，Bulletin ofThe Chemical Society of Japan, 1959.32 (11) .1264-1265), the performance of people to γ-AlON pottery, preparation and shouldWith having carried out a series of research. This pottery has good optical property, dielectric properties, mechanical performance and chemical property, therebyIt is the first material of high temperature resistant infrared window and dome. Military field can be used as high temperature resistant infrared window and cover, armed helicopter thoroughlyThe windscreen of bright plate armour, supersonic plane, the observation window of tank armor car, commercial field can for the bulletproof window of sedan limousine,High-grade watch dial etc.
At present, report that several different methods prepares aluminum nitride oxygen transparent ceramic, comprised that pressureless sintering method, hot pressed sintering, solid phase are anti-Answer sintering process, hot isostatic pressing method. Although researcher has prepared the transparent pottery of aluminium oxynitride of high permeability by these methodsPorcelain, but its sintering temperature is all more than 1900 DEG C and need for a long time insulation, and this has not only proposed very high wanting to instrument and equipmentAsk, also increased preparation cost simultaneously. As US Patent No. 4,481,300 first adopt carbothermic method to prepare oxynitriding aluminium powderBody, then adds Y2O3And/or La2O3For sintering aid is seen through be incubated 24～48 hours at the temperature higher than 1900 DEG C afterRate is higher than 50% aluminum nitride oxygen transparent ceramic, and what the method adopted is pressureless sintering. Japan Patent 3-126674 is with Y2O3For burningKnot auxiliary agent, first by sample 1850 DEG C of insulations after 5 hours, it is reached after certain density 1900 DEG C of pressures with 200MPaPower carries out having obtained transparent aluminium oxynitride pottery after HIP sintering. And for example US Patent No. 7,163,656B1 with aluminium oxide andAluminium nitride is raw material, adopts the method for hot pressing in 1600 DEG C of temperature that form lower than aluminium oxynitride, make goods densified after again higherTemperature react and generate aluminium oxynitride phase. Although this method can lower sintering time effectively, but exists not simultaneouslyBe applicable to the shortcoming of the goods of preparing complicated shape. Although researcher is down to sintering temperature by the method that adopts microwave sintering1800 DEG C. But the transmitance of the goods of preparing by the method is limited, be difficult to application. In addition, microwave sintering itself also exists notBe applicable to the feature of preparation large scale goods.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing aluminum nitride oxygen transparent ceramic. The method can reduce oxynitriding effectivelyThe temperature of aluminium crystalline ceramics sintering. Thereby both can save the energy, can reduce again the loss to instrument and equipment.
For achieving the above object, technical scheme of the present invention comprises the steps:
(1) sintering aid is mixed with AlON powder, obtain mixed powder;
Described sintering aid is RE2O3And SiO2，RE2O3And ethyl orthosilicate, RE (NO3)3And SiO2，RE(NO3)3With positive siliconOne in acetoacetic ester, wherein RE is Y, La, Eu, Ce, Ho or Dy. Preferably Y2O3And SiO2Or La2O3With
SiO2Mixture.
Described RE2O3，RE(NO3)3，SiO2Or the purity of ethyl orthosilicate is higher than 99.9wt%, preferably higher than 99.99
wt％。
The addition of described sintering aid is with RE2O3And SiO2Count 0.01～1.5wt% of mixed powder.
The preferred addition of described sintering aid is with RE2O3And SiO2Count 0.1～1.0wt% of mixed powder.
RE in described sintering aid2O3Or RE (NO3)3Quality percentage composition with RE2O3Count 10～60wt%.
Described AlON powder is solid reaction process, thermit reduction, the standby powder of carbothermal reduction-nitridation legal system. The purity of powderHigher than 99wt%, preferably higher than 99.9wt%. Solid reaction process comes from but is not limited to X.Wang, W.Li, and
S.Seetharaman，Thermodynamic study and synthesis of gamma-aluminum oxynitride.ScandinavianJournal of Metallurgy, 2002.31 (1) .1-6. Thermit reduction comes from but is not limited to J.C.Zhou, Z.J.Liao, and J.Q.Qi,
W.Pang，Z.M.Cheng，D.X.Wu，and T.C.Lu，Study on synthesis of ALON by the method of reaction-Bonding.Rare Metal Materials and Engineering, 2007.36.72-75. Carbothermic method comes from but is not limited to
L.Y.wei，Preparation of Aluminium Oxynitride by Carbothermal Reduction of Aluminium Oxide in
a Flowing N2Atmosphere.China’Refractories，1996.5(1).24-29。
Described hybrid mode comprises and being dry mixed or wet mixing, described in to be dry mixed incorporation time be 1～12 hour, the wet mixing medium of described wet mixingFor methyl alcohol, absolute ethyl alcohol or propyl alcohol.
After described step (1), preferably mixed powder is calcined 600～800 DEG C of calcining heats, calcination time 1～4 hour.
(2) mixed powder extrusion forming obtains biscuit;
Described pressuring method is dry-pressing isostatic cool pressing, and the pressure of isostatic cool pressing is 150～250MPa.
(3) biscuit sintering, cooling.
Described sintering carries out in blanket of nitrogen, and the pressure of nitrogen is higher than 0.5MPa, preferably 0.1～0.3MPa.
Described sintering condition is for to be warming up to 1750～1900 DEG C with the speed of 5～25 DEG C/min, and is incubated 4～48 hours. Heat upSpeed is 10～20 DEG C/min preferably, and sintering temperature is 1800～1850 DEG C/min preferably, temperature retention time preferably 12～24 hours.
The present invention is by adding by RE2O3And SiO2、RE2O3With ethyl orthosilicate, RE (NO3)3And SiO2Or RE (NO3)3WithThe sintering aid of ethyl orthosilicate composition, forms RSiAlON glassy phase, the fusing point of this phase with aluminium oxynitride at grain boundaries(1700 DEG C) are starkly lower than aluminium oxynitride (2140 DEG C), and therefore sintered body forms high-melting-point and low melting point two-phase. Eutectic when intensificationPoint fusing, forms solid-liquid two-phase, acceleration of sintering.
The invention has the advantages that make sintering temperature from background technology, mention more than 1900 DEG C, be down to 1800 DEG C～1850 DEG C, thus the energy saved, and reduced the loss to instrument and equipment.
Brief description of the drawings
Fig. 1 adopts the aluminum nitride oxygen transparent ceramic that in example 1, technique is prepared.
Fig. 2 adopts the aluminum nitride oxygen transparent ceramic that in example 2, technique is prepared.
Fig. 3 is the straight line transmitance that example 1 and 2 is prepared aluminum nitride oxygen transparent ceramic.
Detailed description of the invention
For a better understanding of the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not onlyOnly be confined to the following examples.
Embodiment 1
Aluminium oxynitride powder that solid reaction process is prepared (particle diameter be about 1～2 μ m) with 0.15% by Y2O3(50%) and
SiO2The sintering aid of composition adopts wet method to mix with planetary ball mill. Rotational speed of ball-mill is 250 revs/min. Ball-milling Time is 3 littleTime. The drying box that the slurry obtaining after ball milling is placed in to 70 DEG C is dried 24 hours. After dry, cross 200 order nylon mesh. By instituteObtain powder pressure dry-pressing with 15MPa on dry press and become piece. Then adopt the pressure of 200MPa to carry out isostatic cool pressing. By gainedBiscuit is placed in crucible, then puts into pyrocarbon pipe furnace, is warming up to 1800 DEG C and be incubated 4 hours with 20 DEG C/min. Will after coolingSample sanding and polishing. After cooling, sample sanding and polishing is obtained to sample (1mm is thick) as shown in Figure 1, its transmitance approaches 25% (Fig. 3
a)。
Embodiment 2
Aluminium oxynitride powder that combination method is prepared (particle diameter be about 1～2 μ m) with 0.15% by Y2O3And SiO (20%)2The sintering aid of composition adopts wet method to mix with planetary ball mill. Rotational speed of ball-mill is 250 revs/min, and Ball-milling Time is 3 hours. WillThe slurry obtaining after ball milling is placed in dry 24 hours of the drying box of 70 DEG C, crosses 200 order nylon mesh after dry. By gained powderPressure dry-pressing with 15MPa on dry press becomes piece. Then adopt the pressure of 200MPa to carry out isostatic cool pressing. Gained biscuit is putIn crucible, then put into pyrocarbon pipe furnace, be warming up to 1850 DEG C and be incubated 6 hours with 20 DEG C/min. After cooling, sample is beatenGrinding and polishing light obtains sample (1mm is thick) as shown in Figure 2, and (Fig. 3 b) in 45% left and right for its transmitance.
Embodiment 3
Aluminium oxynitride powder that combination method is prepared (particle diameter be about 1～2 μ m) with 0.20% by Y2O3And SiO (20%)2The sintering aid of composition adopts wet method to mix with planetary ball mill. Rotational speed of ball-mill is 250 revs/min, and Ball-milling Time is 3 hours. WillThe slurry obtaining after ball milling is placed in dry 24 hours of the drying box of 70 DEG C, crosses 200 order nylon mesh after dry. By gained powderPressure dry-pressing with 15MPa on dry press becomes piece. Then adopt the pressure of 200MPa to carry out isostatic cool pressing. Gained biscuit is putIn crucible, then put into pyrocarbon pipe furnace, be warming up to 1850 DEG C and be incubated 6 hours with 20 DEG C/min. After cooling, obtain sample,Its transmitance is in 40% left and right.
Embodiment 4
Aluminium oxynitride powder that combination method is prepared (particle diameter be about 1～2 μ m) with 0.15% by La2O3And SiO (40%)2The sintering aid of composition adopts wet method to mix with planetary ball mill. Rotational speed of ball-mill is 250 revs/min, and Ball-milling Time is 3 hours. WillThe slurry obtaining after ball milling is placed in dry 24 hours of the drying box of 70 DEG C, crosses 200 order nylon mesh after dry. By gained powderPressure dry-pressing with 15MPa on dry press becomes piece. Then adopt the pressure of 200MPa to carry out isostatic cool pressing. Gained biscuit is putIn crucible, then put into pyrocarbon pipe furnace, be warming up to 1850 DEG C and be incubated 6 hours with 20 DEG C/min. After cooling, obtain sample,Its transmitance is in 40% left and right.
Embodiment 5
Aluminium oxynitride powder that combination method is prepared (particle diameter be about 1～2 μ m) with 0.20% by La2O3And SiO (40%)2The sintering aid of composition adopts wet method to mix with planetary ball mill. Rotational speed of ball-mill is 250 revs/min, and Ball-milling Time is 3 hours. WillThe slurry obtaining after ball milling is placed in dry 24 hours of the drying box of 70 DEG C, crosses 200 order nylon mesh after dry. By gained powderPressure dry-pressing with 15MPa on dry press becomes piece. Then adopt the pressure of 200MPa to carry out isostatic cool pressing. Gained biscuit is putIn crucible, then put into pyrocarbon pipe furnace, be warming up to 1850 DEG C and be incubated 6 hours with 20 DEG C/min. After cooling, obtain sample,Its transmitance is in 39% left and right.
Embodiment 6
Aluminium oxynitride powder that combination method is prepared (particle diameter be about 1～2 μ m) with 0.15% by La2O3And SiO (30%)2The sintering aid of composition adopts wet method to mix with planetary ball mill. Rotational speed of ball-mill is 250 revs/min, and Ball-milling Time is 3 hours. WillThe slurry obtaining after ball milling is placed in dry 24 hours of the drying box of 70 DEG C, crosses 200 order nylon mesh after dry. By gained powderPressure dry-pressing with 15MPa on dry press becomes piece. Then adopt the pressure of 200MPa to carry out isostatic cool pressing. Gained biscuit is putIn crucible, then put into pyrocarbon pipe furnace, be warming up to 1800 DEG C and be incubated 12 hours with 20 DEG C/min. After cooling, obtain sampleProduct, its transmitance is in 42% left and right.
Claims (7)
1. prepare a method for gamma aluminum nitride oxygen transparent ceramic, it is characterized in that it comprises the steps:
(1) sintering aid is mixed with AlON powder, obtain mixed powder, to mixed powder calcining, calcining600～800 DEG C of temperature, calcination time 1～4 hour;
Described sintering aid is RE2O3And SiO2，RE2O3And ethyl orthosilicate, RE (NO3)3And SiO2，
RE(NO3)3With the one in ethyl orthosilicate, the addition of described sintering aid is with RE2O3And SiO2MeterFor 0.01～1.5wt% of mixed powder, wherein RE is Y, La, Eu, Ce, Ho or Dy, described burningRE in knot auxiliary agent2O3Or RE (NO3)3Quality percentage composition with RE2O3Count 10～60wt%;
(2) mixed powder extrusion forming obtains biscuit;
(3) biscuit sintering, cooling, and described sintering carries out in blanket of nitrogen, and the pressure of nitrogen is not higher than 0.5MPa, described sintering condition is the speed with 5～25 DEG C/min, is warming up to 1750～1900 DEG C, and insulation4～48 hours.
2. a kind of method of preparing gamma aluminum nitride oxygen transparent ceramic according to claim 1, is characterized in that:Described sintering aid is Y2O3And SiO2, or La2O3And SiO2Mixture.
3. a kind of method of preparing gamma aluminum nitride oxygen transparent ceramic according to claim 1, is characterized in that:The addition of described sintering aid is with RE2O3And SiO2Count 0.1～1.0wt% of mixed powder.
4. a kind of method of preparing gamma aluminum nitride oxygen transparent ceramic according to claim 1, is characterized in that:Described RE2O3Or RE (NO3)3、SiO2Or the purity of ethyl orthosilicate is higher than 99.9wt%.
5. a kind of method of preparing gamma aluminum nitride oxygen transparent ceramic according to claim 1, is characterized in that:Described AlON powder is solid reaction process, thermit reduction or the standby powder of carbothermal reduction-nitridation legal system,The purity of powder is higher than 99wt%.
6. a kind of method of preparing gamma aluminum nitride oxygen transparent ceramic according to claim 1, is characterized in that:The hybrid mode of described step (1) comprises and being dry mixed or wet mixing, described in to be dry mixed incorporation time be 1～12 hour,The wet mixing medium of described wet mixing is methyl alcohol, absolute ethyl alcohol or propyl alcohol.
7. a kind of method of preparing gamma aluminum nitride oxygen transparent ceramic according to claim 1, is characterized in that:Described pressuring method is dry-pressing isostatic cool pressing, and the pressure of isostatic cool pressing is 150～250MPa.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478108A (en) * | 2015-09-01 | 2017-03-08 | 常熟佳合高级陶瓷材料有限公司 | A kind of method preparing large scale AlON crystalline ceramics |
| CN109354501A (en) * | 2018-11-29 | 2019-02-19 | 湖南工学院 | A kind of preparation method of MgAlON crystalline ceramics |
| CN112225564A (en) * | 2019-07-15 | 2021-01-15 | 中国科学院上海硅酸盐研究所 | Aluminum oxynitride transparent ceramic and preparation method thereof |
| CN116789455A (en) * | 2023-06-14 | 2023-09-22 | 大连海事大学 | Method for preparing AlON transparent ceramic by low-temperature rapid pressureless sintering |
-
2010
- 2010-06-28 CN CN201010049105.8A patent/CN106342083B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478108A (en) * | 2015-09-01 | 2017-03-08 | 常熟佳合高级陶瓷材料有限公司 | A kind of method preparing large scale AlON crystalline ceramics |
| CN109354501A (en) * | 2018-11-29 | 2019-02-19 | 湖南工学院 | A kind of preparation method of MgAlON crystalline ceramics |
| CN109354501B (en) * | 2018-11-29 | 2019-08-23 | 湖南工学院 | A kind of preparation method of MgAlON crystalline ceramics |
| CN112225564A (en) * | 2019-07-15 | 2021-01-15 | 中国科学院上海硅酸盐研究所 | Aluminum oxynitride transparent ceramic and preparation method thereof |
| CN112225564B (en) * | 2019-07-15 | 2022-01-04 | 中国科学院上海硅酸盐研究所 | Aluminum oxynitride transparent ceramic and preparation method thereof |
| CN116789455A (en) * | 2023-06-14 | 2023-09-22 | 大连海事大学 | Method for preparing AlON transparent ceramic by low-temperature rapid pressureless sintering |
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