CN1371885A - Preparation of aluminium nitride transparent ceramics by discharge plasma sintering method - Google Patents
Preparation of aluminium nitride transparent ceramics by discharge plasma sintering method Download PDFInfo
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- CN1371885A CN1371885A CN 02115663 CN02115663A CN1371885A CN 1371885 A CN1371885 A CN 1371885A CN 02115663 CN02115663 CN 02115663 CN 02115663 A CN02115663 A CN 02115663A CN 1371885 A CN1371885 A CN 1371885A
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Abstract
The preparation method of transparent aluminium nitride ceramics includes the following steps: placing high-purity AlN powder into graphite mould, placing the mould into discharge plasma sintering furnace, applying axial pressure with 20-30 MPa and adopting vacuum condition whose degree of vacuum is superior to 6 Pa or N2 atmosphere, sintering at 1700-2000 deg.c, heating n temp.-rising rate is 100-800 deg.c/min, heat-insulating for 4-20 min., cooling to room temp. with furnace so as to obtain the invented product.
Description
Technical field
The present invention relates to a kind of preparation method of aluminium nitride transparent ceramics.
Background technology
Aluminium nitride transparent ceramics has not only been inherited the advantage (high heat conductance, low-k, high-insulativity etc.) of aluminium nitride ceramics self, but also has the transparency, and it is had a wide range of applications in fields such as irdome and window material.Yet aluminium nitride is the strong covalent bond compound, and sintering activity is low, and aluminium nitride is easy to hydrolysis introducing oxygen impurities.Therefore, pure aluminium nitride has limited its practical application because of its very difficult sintering reaches complete densification.And the sintering of transparent aluminium nitride ceramic is just difficult more.The report of successful foreign sintered aluminum nitride crystalline ceramics is few at present, the people such as Nobuyuki Kuramoto of Japan Tokuyama Soda company in 1984 at periodical " Journal of materials science letters " (No.3, pp471-474) delivered the paper of " Transparent AlN ceramics " by name in, 1989 at periodical " Ceramicbulletin " (Vol.68, No.4, pp883-887) delivered the paper of " Development of transparent aluminumnitride " by name in, adopt hot pressing and pressureless sintering in the literary composition, at N
2Under the atmosphere, with CaO, Ca (NO
3)
2, 3CaOAl
2O
3For additive or do not add any additives, sintering 3～10h has prepared transparent aluminium nitride ceramic under 1800～2000 ℃ sintering temperature.Chinese patent CN 1199036A has reported a kind of method for preparing aluminium nitride transparent ceramics, and this method is with CaC
2, CaC
2With the mixture of rare earth oxide be sintering aid, at N
2, N
2+ Ar or N
2+ H
2Under arbitrary mobile atmosphere, the thermal treatment process with after no pressure, hot pressed sintering and the low temperature hot-press sintering makes transparent aluminium nitride ceramic.The sintering time of above several method is all grown (several hours even tens hours), and energy consumption is big, and has adopted sintering aid mostly.
The present invention has overcome the shortcoming of aforesaid method, adopts discharge plasma sintering method (being called for short SPS), prepares the AlN crystalline ceramics in a short period of time.
The discharge plasma sintering method has following characteristics: heat up, cooling rate is fast; Can be at lower sintering temperature; Sintering time is short.Plasma discharging can also heat sample by pulsed current except the characteristics with hot pressed sintering, makes the very fast sintering of sample.It is generally acknowledged that may there be following several densification approach in discharge plasma sintering: (1) intercrystalline discharge generation localized hyperthermia causes evaporation and fusing at grain surface, and forms " neck " at grain contact point, thereby directly promoted the process of densification; (2) under the effect of pulsed current, grain surface activates easily, and various diffusions are all strengthened, thereby has promoted the process of densification.Each uniform particles ground self-heating makes the particle surface activation in the discharge plasma sintering body, thereby has very high thermo-efficiency, can make the sintered compact densification in the quite short time.At present, the mechanism of discharge plasma sintering is still among further studying.
The discharge plasma sintering method has been successfully applied to the preparation of multiple materials such as function-graded material, metal-base composites, fibre reinforced composites, nano material, porous material.At present, Shang Weijian is equipped with the relevant report of crystalline ceramics with the discharge plasma sintering legal system.
Summary of the invention
The objective of the invention is to adopt the discharge plasma sintering method, preparation AlN crystalline ceramics.
The present invention realizes by following manner: high-purity AlN powder is directly inserted in the graphite jig, then mould is put into the discharge plasma sintering stove, apply the axle pressure of 20～30MPa, adopt vacuum tightness to be better than vacuum condition or the N of 6Pa
2Atmosphere is carried out sintering in 1700～2000 ℃, and temperature rise rate is 100～800 ℃/min, insulation 4～20min, sample cools to room temperature with the furnace, with sample corase grind, fine grinding and polishing both surfaces to 0.5mm.
Wherein, the content of oxygen is 1.0～1.1wt% in high-purity aluminium nitride powder, and the content of nitrogen reaches 33～33.5wt%, and other foreign matter content all is lower than 50ppm.
The invention has the advantages that: (1) has reduced sintering time greatly (whole sintering process can be short to has had only several minutes, and adopt traditional hot pressing, pressureless sintering method, need several hours even tens hours), thereby saved the energy greatly, very important meaning has been arranged at save energy, aspect such as enhance productivity; (2) the present invention can adopt N
2Atmosphere also can adopt vacuum sintering, and need not moulding in the preparation process, do not add any sintering aid, has simplified process system.
With the transparent aluminium nitride ceramic that the method for the invention makes, its density can reach 3.25g.cm
-3Pottery with the preparation of means of testing such as X-ray diffraction, electronic probe proof is pure aluminium nitride; Scanning electron microscope shows that the crystal grain growth of sintered compact is fairly perfect, the shape comparison rule, and also size is consistent, arranges closely, and structure is dense on the whole, and it is more even to distribute, and pore is seldom; Sample at the maximum transmission of middle-infrared band (2.5～25 μ m) greater than 70%.Show the discharge plasma sintering method be can be used for preparing the AlN crystalline ceramics a kind of effectively, means efficiently.
Specific embodiments
Example 1: aluminium nitride powder is inserted in the graphite jig, then mould is put into the discharge plasma sintering stove, apply the axle pressure of 25MPa, be better than in vacuum tightness under the vacuum condition of 6Pa, temperature rise rate with 200 ℃/min is warming up to 1800 ℃, insulation 15min, and sample cools to room temperature with the furnace.
From Fig. 1: as can be seen, the aluminium nitride transparent ceramics that makes possesses good light transmittance the transparent aluminium nitride ceramic design sketch.Performance is as follows:
Density (g.cm
-3): 3.25
Crystalline phase (X ray, electron probe microanalysis): AlN
2.5～25 mu m waveband maximum transmissions (%):＞60%
From Fig. 2: transparent aluminium nitride ceramic profile scanning Electronic Speculum figure as can be seen, the crystal grain of sintered compact is grown fairly perfect, the shape comparison rule, and size is consistent, arranges closely, and structure is dense on the whole, it is more even to distribute, pore seldom, wherein major part all is distributed on the crystal boundary, the intracrystalline pore seldom.This structure provides good basis for the light transmission of pottery undoubtedly.
Example 2: aluminium nitride powder is inserted in the graphite jig, then mould is put into the discharge plasma sintering stove, apply the axle pressure of 20MPa, be better than in vacuum tightness under the vacuum condition of 6Pa, temperature rise rate with 600 ℃/min is warming up to 1900 ℃, insulation 20min, and sample cools to room temperature with the furnace.
Density (g.cm
-3): 3.25
Crystalline phase (X ray, electron probe microanalysis): AlN
Fig. 3: the transparent aluminium nitride ceramic transmission plot shows, this material is at 2.5～25 mu m wavebands, the maximum transmission of light (%):＞70%.
Example 3: aluminium nitride powder is inserted in the graphite jig, then mould is put into the discharge plasma sintering stove, apply the axle pressure of 30MPa, under nitrogen atmosphere in 1700 ℃ of sintering, temperature rise rate with 100 ℃/min heats up, insulation 4min, and sample cools to room temperature with the furnace.
Density (g.cm
-3): 3.23
Crystalline phase (X ray, electron probe microanalysis): AlN
2.5～25 mu m wavebands, the maximum transmission of light (%):＞60%
Claims (1)
1, a kind of Preparation of Translucent AlN Ceramics method, it is characterized in that adopting the discharge plasma sintering legal system to be equipped with aluminium nitride ceramics, directly insert high-purity aluminium nitride powder in the graphite jig, mould is put into the discharge plasma sintering stove, apply the axle pressure of 20～30MPa, adopt vacuum tightness to be better than vacuum condition or the N of 6Pa
2Atmosphere, sintering under 1700～2000 ℃ sintering temperature, temperature rise rate with 100～800 ℃/min heats up, after insulation 4～20min, cool to room temperature with the furnace, prepare transparent aluminium nitride ceramics, wherein, the content of oxygen is 1.0～1.1wt% in the aluminium nitride powder, and the content of nitrogen reaches 33～33.5wt%, and other foreign matter content all is lower than 50ppm.
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| CN 02115663 CN1371885A (en) | 2002-04-01 | 2002-04-01 | Preparation of aluminium nitride transparent ceramics by discharge plasma sintering method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304195C (en) * | 2004-12-14 | 2007-03-14 | 清华大学 | Micelle ceramic/metal block composite material and preparation method thereof |
| CN102351515A (en) * | 2011-07-13 | 2012-02-15 | 清华大学 | In-Ga-O base oxide thermoelectric ceramic material and preparation method thereof |
| CN101775578B (en) * | 2009-01-12 | 2012-09-19 | E.I.内穆尔杜邦公司 | ZnAl target preparation method and prepared ZnAl target |
| CN104446498A (en) * | 2014-11-19 | 2015-03-25 | 浙江工业大学 | Manufacturing method of transparent aluminum nitride ceramics |
| CN105837224A (en) * | 2016-05-31 | 2016-08-10 | 武汉理工大学 | Method for preparing aluminum nitride ceramics by aid of ammonium fluoride which is used as additive |
| CN108675795A (en) * | 2018-07-03 | 2018-10-19 | 北京科技大学 | A kind of method that SPS sintering prepares high heat conduction and high intensity aluminium nitride ceramics |
-
2002
- 2002-04-01 CN CN 02115663 patent/CN1371885A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304195C (en) * | 2004-12-14 | 2007-03-14 | 清华大学 | Micelle ceramic/metal block composite material and preparation method thereof |
| CN101775578B (en) * | 2009-01-12 | 2012-09-19 | E.I.内穆尔杜邦公司 | ZnAl target preparation method and prepared ZnAl target |
| CN102351515A (en) * | 2011-07-13 | 2012-02-15 | 清华大学 | In-Ga-O base oxide thermoelectric ceramic material and preparation method thereof |
| CN104446498A (en) * | 2014-11-19 | 2015-03-25 | 浙江工业大学 | Manufacturing method of transparent aluminum nitride ceramics |
| CN105837224A (en) * | 2016-05-31 | 2016-08-10 | 武汉理工大学 | Method for preparing aluminum nitride ceramics by aid of ammonium fluoride which is used as additive |
| CN105837224B (en) * | 2016-05-31 | 2019-01-01 | 武汉理工大学 | It is a kind of using ammonium fluoride as the preparation method of the aluminium nitride ceramics of additive |
| CN108675795A (en) * | 2018-07-03 | 2018-10-19 | 北京科技大学 | A kind of method that SPS sintering prepares high heat conduction and high intensity aluminium nitride ceramics |
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