CN103011830A - Ultrahigh-pressure low-temperature sintering preparation method of transparent aluminium nitride ceramic - Google Patents
Ultrahigh-pressure low-temperature sintering preparation method of transparent aluminium nitride ceramic Download PDFInfo
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- CN103011830A CN103011830A CN2012105839593A CN201210583959A CN103011830A CN 103011830 A CN103011830 A CN 103011830A CN 2012105839593 A CN2012105839593 A CN 2012105839593A CN 201210583959 A CN201210583959 A CN 201210583959A CN 103011830 A CN103011830 A CN 103011830A
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Abstract
The invention relates to an ultrahigh-pressure low-temperature sintering preparation method of transparent aluminium nitride ceramic. The preparation method comprises the following steps of: (1) selecting materials by selecting AlN (aluminium nitride) micron powder with an average grain diameter of 40 mu m as a raw material; (2) pre-processing the AlN powder; (3) adding a sintering accessory ingredient which is selected from calcium carbide and/or rare earth oxide in an addition amount of 2.0-5.0wt%; (4) high-pressure forming with a forming pressure of 1Gpa; and (5) high-pressure low-temperature sintering with a high-pressure temperature of 1500-1700 DGE C, a pressure of 4.0-5.5Gpa; and insulating for 20-60 minutes, naturally cooling samples to obtain the transparent aluminium nitride ceramic. The transparent aluminium nitride ceramic prepared by the invention has the advantages of small grains, regular shape, even and compact structure, pore-free property, high density and small grains. The preparation method has no need of the atmosphere control and also has the advantages of simple process flow, convenience in operation and short production period.
Description
Technical field
The invention belongs to the Non-oxide Transparent Ceramics field, specifically relate to a kind of ultra-high voltage low-temperature melt producing method of transparent aluminium nitride ceramic.
Background technology
Aluminium nitride (AlN) pottery because of have good heat conductivity (the thermal conductivity theoretical value is 320 W/ (mK)), reliable electrical insulating property (volume specific resistance is greater than 1012 Ω m), low specific inductivity (being about 8 under the 1MHz) and dielectric loss, linear expansivity nontoxic and that be complementary with silicon (Si) and gallium arsenide (GaAs) (during 293～773K, 4.8 * 10
-6K
-1) etc. a series of good characteristics, be considered to heat sink material and the packaged material of desirable large-scale integrated circuit, semiconductor module circuit and the high power device of a new generation.Aluminium nitride transparent ceramics not only has the above-mentioned advantage of aluminium nitride ceramics material, but also has the transparency, therefore has a wide range of applications in fields such as irdome and window material.But because the AlN compound is the strong covalent bond compound, sintering activity is extremely low, is not difficult to sintering so add the pure AlN of sintering aid.The sintering of transparent aluminium nitride ceramic is just more difficult, and except a top reason, the easy and airborne water vapour of aluminium nitride reacts, thereby introduces oxygen impurities, also is a major reason.
In recent years, aluminium nitride ceramics is received vast material scholar and engineering technical personnel's concern, particularly transparent aluminium nitride ceramic because of its excellent over-all properties also becomes the focus of people's research.From domestic and foreign literature, the report of successful sintered aluminum nitride crystalline ceramics is few, successfully prepares the earliest aluminium nitride ceramics and be the people such as Noboyuki Kuramoto of Japanese Tokuyama Soda company.1984; the people such as Noboyuki Kuramoto have delivered relevant paper at periodicals such as " Jounal of materials science letters "; the preparation method who adopts in the literary composition is hot pressing and pressureless sintering; under the flowing nitrogen protection; take CaO etc. as sintering aid; sintering condition is: temperature 1800-2000 ℃, and sintering time 3-10h.They observe in test (the N0 with Ca
3)
2Be the sintering process of the transparent aluminium nitride of sintering adjuvant, finding has three obvious processes: at first be 1300-1600 ℃ of AlN particle re-arrangement under the liquid phase effect; Separating out of the dissolving of the 2nd, 1600-1800 ℃ of aluminum nitride particle and crystal grain; The 3rd, 1800-2000 ℃ of holding stage aluminum nitride grain growth.By research, they think that the sintering of this system is more typical liquid phase sintering.
Chinese patent CN 1199036A has reported a kind of method for preparing aluminium nitride transparent ceramics, the preparation method that the method adopts is the thermal treatment process after pressureless sintering, hot pressed sintering and the low temperature hot-press sintering, made transparent aluminium nitride ceramic, the method is with the mixture (Y of technical grade carbide of calcium or technical grade carbide of calcium and rare earth oxide
2O
3, Sm
2O
3Deng) be sintering aid, at N
2Lower Deng flowing gas protection, obtained transmittance greater than 62% transparent AlN ceramics through the sintering of several hours even tens hours or thermal treatment, the shortcoming of the method is that sintering temperature is high, sintering time is long, energy consumption is large.
Chinese patent CN 1371885 has reported discharge plasma sintering method (SPS) preparation aluminium nitride ceramics, the preparation method that the method adopts is the discharge plasma sintering method, the equipment that adopts is the discharge plasma sintering stove, sintering temperature is 1700 ℃-2000 ℃, soaking time is 4-20min, and the transmittance of the transparent aluminium nitride ceramics that it is prepared is greater than 70%.The shortcoming of the method is that plasma sintering equipment is expensive, and temperature distribution is extremely inhomogeneous during the SPS sintering, and especially large-sized product has reduced the quality of product.In addition, its mould uses repetition rate low, has increased the cost of product.
Summary of the invention
The present invention has overcome the shortcoming of above several sintering methods, and has developed a kind of ultra-high voltage low-temperature melt producing method of transparent aluminium nitride ceramic, and the method is to adopt ultra-high pressure sintering method (being called for short HPS), prepares in a short period of time the AlN crystalline ceramics.High-pressure sinter (general claim that the sintering method that carries out under greater than 1GPa pressure is high-pressure sinter) is having certain superiority aspect the sintering of material, not only can make material reach rapidly high-compactness, has small grains, and crystalline structure even atom, electronic state are changed, high pressure conditions is kept (intercepting and capturing) to atmospheric pressure state, thereby give material in lower inaccessible performance of the techniques such as ordinary sinter or hot pressed sintering.
The object of the invention is to adopt the ultra-high pressure sintering method, prepare high performance AlN crystalline ceramics.
The present invention utilizes domestic six-plane piercer to be agglomerating plant, improve at aspects such as the design of the improvement of sintering aid selection, the pre-treatment of AlN powder, forming method, the synthetic piece assembling of ultra-high voltage, ultra-high voltage hot-pressing sintering techniques, the content of microstructure, oxygen level and other impurity of control AlN pottery, the transparent aluminium nitride ceramic of excellent.
Technical scheme of the present invention is achieved in the following ways in sum:
A kind of ultra-high voltage low-temperature melt producing method of transparent aluminium nitride ceramic, it may further comprise the steps:
(1) select materials: selecting median size is raw material at the AlN micro-powder of 40 μ m;
(2) the AlN powder carries out pre-treatment;
(3) add sintering aid: the sintering aid of selecting is carbide of calcium and/or rare earth oxide, and add-on is: 2.0%-5.0wt%;
(4) high-pressure molding: forming pressure is at 1Gpa;
(5) high pressure low temperature sintering: the high pressure temperature is 1500-1700 ℃, and pressure is 4.0-5.5GPa, insulation 20-60min, and the sample naturally cooling had both got transparent aluminium nitride ceramic.
Further, to carry out pre-treatment be to utilize vacuum oven that powder is processed to the AlN powder in described (2) step, and condition is: 720 ℃ of temperature, time: 50min.
Further, to carry out pre-treatment be to adopt the flowing nitrogen protection to the AlN powder in described (2) step, carries out the pre-treatment of powder under the normal pressure, and condition is: 720 ℃ of temperature, time: 50min.
Further, adding sintering aid in described (3) step is CaC
2, addition is 2.0-4.0%.
Further, adding sintering aid in described (3) step is carbide of calcium and rare earth oxide mixture, and the carbide of calcium addition is 2.0-3.0%, and the rare earth oxide addition is 1.0-2.0%.
Further, described rare earth oxide is at least a Y
2O
3, Sm
2O
3Or La
2O
3
Further, add the mixture of the Samarium trioxide of yttrium oxide that sintering aid is 2% carbide of calcium and 1% and 1% in described (3) step.
Further, the AlN powder in described (4) step carries out high-pressure molding, and the powder with mixing coats with graphite paper, and the agalmatolite of packing into synthesizes piece, utilizes dry pressure formedly, and forming pressure is at 1GPa.
Beneficial effect of the present invention:
The present invention compares with the method that with no pressure and hot pressed sintering prepare the transparent aluminium nitride ceramic material, have the following advantages: (1) the present invention adopts the ultra-high pressure sintering technology, be characterized in that ultra-high voltage (4.0-5.5GPa), sintering temperature are low, do not need atmosphere control, sintering is quick, the transparent aluminium nitride ceramic excellent property of preparation, cost is lower; (2) transparent AlN ceramics that makes of ultra-high pressure sintering method of the present invention, its relative density only 100%, density reachable 3.26g/cm
3, greater than 60%, it is tiny to have crystal grain at the maximum transmission of middle-infrared band (2.5-25 μ m), regular shape, and even structure is fine and close, and pore-free has high-compactness, and crystal grain is tiny; (3) this preparation method need not atmosphere control; (4) this preparation technology's flow process is simple, easy to operate, with short production cycle, at save energy, the aspect such as enhance productivity very important meaning is arranged.
Description of drawings:
Fig. 1 is the transparent aluminium nitride fracture SEM figure of the embodiment of the invention one;
Fig. 2 is the transparent aluminium nitride transmittance curve of the embodiment of the invention two.
Embodiment:
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
Embodiment one:
Selecting the particle diameter of Japanese Cao Da company preparation is 40 μ m AlN powders, under vacuum condition, and 720 ℃ of thermal treatment 50 minutes, adding 3.5% carbide of calcium is sintering aid, mixes; Powder with mixing coats with graphite paper, and the agalmatolite of packing into synthesizes piece, and it is dry pressure formed to utilize six-plane piercer to carry out, and forming pressure is at 1Gpa; The sample of forming is coated with molybdenum foil, put into the insulation tube that zirconium white and magnesium oxide are made with coating good sample, insulation tube is put into carbon tube, the pyrophyllite composite block of again carbon tube being packed into, transmission medium take agalmatolite as ultra-high pressure sintering, after assembling, at the enterprising horizontal high voltage sintering of six-plane piercer, the high-pressure sinter temperature is 1600 ℃, pressure is 4.0 GPa, be incubated 30 min, sample had both got transparent aluminium nitride ceramic with the six-plane piercer naturally cooling.
Performance with the prepared transparent aluminium nitride ceramic of method of the present invention is as follows:
Density (g/cm
3): 3.25;
Principal crystalline phase (X ray);
AlN intensity (MPa): 520;
Specific inductivity (1MHz, 25 ℃): 8.0;
Thermal conductivity (Wm
-1K
-1): 180;
2.5-25 the maximum transmission (%) of μ m infrared band:＞60.
Shown in Fig. 1, from the analysis of SEM fracture apperance as seen, transparent AlN crystal grain is full, regular shape, and it is complete to grow, and all with crystal face two dimension close contact, therefore pore-free causes material transparent to crystal grain.
Embodiment two:
Select the particle diameter 40 μ m AlN powders of Japanese Cao Da company preparation, take the yttrium oxide mixture of 3.0% carbide of calcium and 1.0% as sintering aid, the high pressure temperature is 1600 ℃, pressure is 5.0 GPa, be incubated 40 min, sample is with the six-plane piercer naturally cooling, and other operation is identical with embodiment one.The performance of prepared transparent aluminium nitride ceramic is as follows:
Density (g/cm
3): 3.26;
Principal crystalline phase (X ray): AlN;
Intensity (MPa): 500;
Specific inductivity (1MHz, 25 ℃): 8.0;
Thermal conductivity (Wm
-1K
-1): 190;
As shown in Figure 2, the maximum transmission (%) of 2.5-25 μ m infrared band:＞63, SEM fracture apperance is analyzed identical with embodiment one.
Embodiment three:
Select domestic particle diameter 40 μ m AlN powders from spreading the method preparation, take the Samarium trioxide mixture of 2% carbide of calcium and 2% as sintering aid, the compression moulding of high-pressure molding method, after synthetic piece assembles, carry out ultra-high pressure sintering at six-plane piercer, the high pressure temperature is 1650 ℃, pressure is 5.2 GPa, be incubated 35 min, sample namely gets transparent aluminium nitride ceramic with the six-plane piercer naturally cooling.Other operation is identical with embodiment one.The performance of prepared transparent aluminium nitride ceramic is as follows:
Density (g/cm
3): 3.24;
Principal crystalline phase (X ray): AlN;
Intensity (MPa): 490;
Specific inductivity (1MHz, 25 ℃): 8.0;
Thermal conductivity (Wm
-1K
-1): 170;
2.5-25 the maximum transmission (%) of μ m infrared band:＞60.
The SEM fracture apperance is analyzed identical with embodiment one.
Embodiment four
Select domestic median size 40 μ m AlN powders from spreading the method preparation, take the Samarium trioxide mixture of the yttrium oxide of 2% carbide of calcium and 1% and 1% as sintering aid, adopt the high-pressure molding method, carry out ultra-high pressure sintering at six-plane piercer, the high pressure temperature is 1600 ℃, and pressure is 5.0 GPa, is incubated 30 min, sample namely gets transparent aluminium nitride ceramic with the six-plane piercer naturally cooling.Other operation is identical with embodiment one.The performance of prepared transparent aluminium nitride ceramic is as follows:
Density (g/cm
3): 3.24;
Principal crystalline phase (X ray): AlN;
Intensity (MPa): 500;
Specific inductivity (1MHz, 25 ℃): 8.0;
Thermal conductivity (Wm
-1K
-1): 170;
2.5-25 the maximum transmission (%) of μ m infrared band:＞60.
The SEM fracture apperance is analyzed identical with embodiment one.
Embodiment five
Select the median size 40 μ m AlN powders of Japanese Cao Da company preparation, take the mixture of the lanthanum trioxide of 3.0% carbide of calcium and 1.5% as sintering aid, adopt high pressure (1GPa) forming method, carry out ultra-high pressure sintering at domestic six-plane piercer, main technologic parameters: the high pressure temperature is 1700 ℃, and pressure is 5.5 GPa, is incubated 40 min, sample namely gets transparent aluminium nitride ceramic with the six-plane piercer naturally cooling.Other operation is identical with embodiment one.The performance of prepared transparent aluminium nitride ceramic is as follows:
Density (g/cm
3): 3.25;
Principal crystalline phase (X ray): AlN;
Intensity (MPa): 540;
Specific inductivity (1MHz, 25 ℃): 8.0;
Thermal conductivity (Wm
-1K
-1): 175;
2.5-25 the maximum transmission (%) of μ m infrared band:＞61.
The SEM fracture apperance is analyzed identical with embodiment one.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. the ultra-high voltage low-temperature melt producing method of a transparent aluminium nitride ceramic, it is characterized in that: it may further comprise the steps:
(1) select materials: selecting median size is raw material at the AlN micro-powder of 40 μ m;
(2) the AlN powder carries out pre-treatment;
(3) add sintering aid: the sintering aid of selecting is carbide of calcium and/or rare earth oxide, and add-on is: 2.0%-5.0wt%;
(4) high-pressure molding: forming pressure is at 1Gpa;
(5) high pressure low temperature sintering: the high pressure temperature is 1500-1700 ℃, and pressure is 4.0-5.5GPa, insulation 20-60min, and the sample naturally cooling had both got transparent aluminium nitride ceramic.
2. the ultra-high voltage low-temperature melt producing method of a kind of transparent aluminium nitride ceramic according to claim 1 is characterized in that: adding sintering aid in described (3) step is CaC
2, addition is 2.0-4.0%.
3. the ultra-high voltage low-temperature melt producing method of a kind of transparent aluminium nitride ceramic according to claim 1, it is characterized in that: adding sintering aid in described (3) step is carbide of calcium and rare earth oxide mixture, the carbide of calcium addition is 2.0-3.0%, and the rare earth oxide addition is 1.0-2.0%.
4. the ultra-high voltage low-temperature melt producing method of a kind of transparent aluminium nitride ceramic according to claim 3, it is characterized in that: described rare earth oxide is at least a Y
2O
3, Sm
2O
3Or La
2O
3
5. the ultra-high voltage low-temperature melt producing method of a kind of transparent aluminium nitride ceramic according to claim 4 is characterized in that: the mixture that adds sintering aid in described (3) step and be the Samarium trioxide of 2% carbide of calcium, 1% yttrium oxide and 1%.
6. the ultra-high voltage low-temperature melt producing method of each described a kind of transparent aluminium nitride ceramic according to claim 1 ~ 5, it is characterized in that: to carry out pre-treatment be to utilize vacuum oven that powder is processed to the AlN powder in described (2) step, condition is: 720 ℃ of temperature, time: 50min.
7. the ultra-high voltage low-temperature melt producing method of each described a kind of transparent aluminium nitride ceramic according to claim 1 ~ 5; it is characterized in that: to carry out pre-treatment be to adopt the flowing nitrogen protection to the AlN powder in described (2) step; carry out the pre-treatment of powder under the normal pressure; condition is: 720 ℃ of temperature, time: 50min.
8. the ultra-high voltage low-temperature melt producing method of each described a kind of transparent aluminium nitride ceramic according to claim 1 ~ 5, it is characterized in that: the AlN powder in described (4) step carries out high-pressure molding, with the powder that mixes, coat with graphite paper, the agalmatolite of packing into synthesizes piece, utilize dry pressure formedly, forming pressure is at 1GPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387393A (en) * | 2013-07-25 | 2013-11-13 | 中国计量学院 | Aluminum nitride (AlN) ceramics and preparation method thereof |
| CN110072826A (en) * | 2016-12-21 | 2019-07-30 | 日本碍子株式会社 | Transparent AlN sintered body and its preparation method |
| CN110282983A (en) * | 2019-07-05 | 2019-09-27 | 河南理工大学 | A kind of high rigidity TiB of no interphase2-B4C ceramic composite preparation method and applications |
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| CN1749213A (en) * | 2005-07-29 | 2006-03-22 | 四川艺精长运超硬材料有限公司 | Process for preparing AIN ceramic material |
| CN101050115A (en) * | 2007-03-09 | 2007-10-10 | 西南科技大学 | Ceramics of containing powder body of cubic silicon nitride, and preparation method |
| US20080111085A1 (en) * | 2001-10-31 | 2008-05-15 | Yasushi Kawashima | Method and device for generating ultra-high pressure |
-
2012
- 2012-12-31 CN CN2012105839593A patent/CN103011830A/en active Pending
Patent Citations (4)
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| CN1199036A (en) * | 1998-04-24 | 1998-11-18 | 中国科学院上海硅酸盐研究所 | Process for preparation of transparent aluminium nitride ceramic |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387393A (en) * | 2013-07-25 | 2013-11-13 | 中国计量学院 | Aluminum nitride (AlN) ceramics and preparation method thereof |
| CN103387393B (en) * | 2013-07-25 | 2014-11-05 | 中国计量学院 | Aluminum nitride (AlN) ceramics and preparation method thereof |
| CN110072826A (en) * | 2016-12-21 | 2019-07-30 | 日本碍子株式会社 | Transparent AlN sintered body and its preparation method |
| CN110072826B (en) * | 2016-12-21 | 2022-03-01 | 日本碍子株式会社 | Transparent AlN sintered body and process for producing the same |
| CN110282983A (en) * | 2019-07-05 | 2019-09-27 | 河南理工大学 | A kind of high rigidity TiB of no interphase2-B4C ceramic composite preparation method and applications |
| CN110282983B (en) * | 2019-07-05 | 2022-07-29 | 河南理工大学 | High-hardness TiB without intermediate phase 2 -B 4 Preparation method and application of C ceramic composite material |
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Application publication date: 20130403 |