CN101050115A - Ceramics of containing powder body of cubic silicon nitride, and preparation method - Google Patents
Ceramics of containing powder body of cubic silicon nitride, and preparation method Download PDFInfo
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- CN101050115A CN101050115A CN 200710048600 CN200710048600A CN101050115A CN 101050115 A CN101050115 A CN 101050115A CN 200710048600 CN200710048600 CN 200710048600 CN 200710048600 A CN200710048600 A CN 200710048600A CN 101050115 A CN101050115 A CN 101050115A
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Abstract
This invention discloses a ceramic containing cubic nitride powder. The ceramic is composed of: gamma-Si3N4 5-100 wt.%, at least one of Al2O3, ZrO2, alpha- or beta-Si3N4, SiC, BN and AlN 0-95 wt.%, and at least one of Y2O3, Al2O3 and La2O (sintering aid) 0-10 wt.%. The ceramic is prepared by: preparing the raw materials, dry-cooling, grinding by isostatic cool pressing, dry-pressing, assembling the sintering chamber, and sintering under an ultrahigh pressure. The method has such advantages as simple process, easy operation, low sintering temperature, and short sintering time. The ceramic has such advantages as high compactness, uniform microstructure, and good mechanical properties, and can be used in the fields of mechanics, chemical engineering, aviation and photoelectronics.
Description
Technical field
The present invention relates to a kind of pottery and preparation method thereof, particularly a kind of pottery that contains powder body of cubic silicon nitride and preparation method thereof.This pottery is applicable to technical fields such as machinery, chemical industry, aerospace, photoelectron.
Background technology
(Silicon Nitride, chemical formula are Si to silicon nitride
3N
4) pottery is the excellent high structural ceramics that grows up the fifties, it is one of combination property best material in the advanced ceramics.Excellent properties such as it has hot strength and hardness height, creep is little, anti-oxidant, corrosion-resistant, proportion is little, thermal expansivity is low, thermal-shock resistance is good, fracture toughness property height and be widely used in high performance structure ceramic material and the high speed cutting instrument made.The third phase-cubic silicon nitride of silicon nitride (or claims c-Si
3N
4Or γ-Si
3N
4, hereinafter to be referred as γ-Si
3N
4) have spinel structure, successfully synthesized by high-temperature and high-pressure technique in 1999.People are by theoretical prediction with to the research of synthetic powder characteristic, think γ-Si
3N
4Be the third superhard material after diamond and cubic boron nitride, its bulk modulus is 290 (5) GPa, and Vickers hardness is 30～43GPa, and the room temperature average hardness is 35.31GPa, can match in excellence or beauty with stipoverite (stishovite).γ-Si
3N
4Being a kind of wide energy carrying semiconductor material (bandwidth is 3.45eV), also is the high optical material of a kind of refractive index (static permittivity 4.70), can be used as semiconductor, purple or Ultra-Violet Laser and light LED material etc.
But silicon nitride is high covalent linkage compound, atomic diffusivity is low, volume diffusion that densification is required and crystal boundary velocity of diffusion, sintering motivating force are very little, have only when sintering temperature during near silicon nitride dispersion temperature (greater than 1850 ℃), and atomic migration just has enough speed.This has determined pure silicon nitride can not lean on conventional solid state sintering to reach densification, so except that reaction sintering, other method all need adopt sintering aid, utilizes the liquid phase sintering principle to carry out densification sintering.At present, the sintering of silicon nitride ceramics is mainly with α-Si
3N
4Or β-Si
3N
4Powder is raw material, under the condition of adding sintering aid, adopt the sintering methods such as hot pressed sintering, pressureless sintering, HIP sintering, gas pressure sintering to carry out, but sintering temperature height, and the sintering aid that adds easily forms grain boundary glassy phase, glassy phase easily forms molten mass under hot conditions, affect the applied at elevated temperature performance of silicon nitride ceramic material.
Recently, the people such as Muscovite Yunoshov and the present application people Tang Jing friend research group by the detonation driven device can the synthetic capacity of single γ-Si
3N
4Powder, and find with α-Si
3N
4Or β-Si
3N
4Make raw material and under the surge of 50GPa, be converted into γ-Si
3N
4Ratio up to 85%, this makes and makes in batches γ-Si more than the conversion ratio height that is used for the graphite synthesizing nano diamond with similar techniques
3N
4The technology of powder becomes and may and come true very soon.
Yet, Si
3N
4With SiC, BN, AlN, B
4The non-oxidized substances such as C are the same, and sintering is very difficult under normal pressure.At present, silicon nitride ceramics is at N
2Sintering temperature in the atmosphere, more than 1700 ℃, soaking time is long, sintering period is long, production cost is higher, but its microstructure undesirable (crystal grain is big, pore is big, void content is higher, crystal boundary is obvious etc.), especially surface working poor performance (being difficult to obtain the surface of high planeness), ambient temperature mechanical properties is not high, high-temperature behavior since crystal boundary glassy phase softening and significantly descending remain further to be improved.
γ-Si
3N
4Constant-pressure and high-temperature phase equilibrium temperature be 1670K, and the sintering temperature of general sintering process is up to (except reaction-sintered) more than the 2000K.Therefore, the traditional ceramics sintering technology is not suitable for γ-Si
3N
4Sintering, exploitation contains γ-Si
3N
4The new sintering technology of powdered ceramics is to development and utilization γ-Si
3N
4The performance of pottery is all significant.
Summary of the invention
Purpose of the present invention is intended to overcome above-mentioned deficiency of the prior art, by adopting ultra-high pressure sintering mode etc., provide a kind of uniform microstructure, good mechanical performance, production cost low contain pottery of powder body of cubic silicon nitride and preparation method thereof.
Content of the present invention is: a kind of pottery that contains powder body of cubic silicon nitride, its feature part are that this ceramic weight percent consists of: γ-Si
3N
45%～100%, Al
2O
3, Zr0
2, α or β phase Si
3N
4, at least a 0～95% among SiC, BN, the AlN, and sintering aid Y
2O
3, Al
2O
3, La
2Among the O at least a 0～10%.
Another content of the present invention is: a kind of preparation method who contains the pottery of powder body of cubic silicon nitride, its feature part is to comprise the following steps:
A. batching is ground: press γ-Si
3N
45%～100%, Al
2O
3, ZrO
2, α or β phase Si
3N
4, at least a 0～95% among SiC, BN, the AlN, sintering aid Y
2O
3, Al
2O
3, La
2After the amount of the getting batching, mixed grinding 4～8 hours obtains finely dispersed composite granule at least a 0～10% weight percent respectively among the O;
B. dry: that composite granule is done dry the processing through infrared ray, vacuum or a conventional oven;
Drying temperature be controlled at 120 ℃ with interior, be preferably 60 ℃～120 ℃, be 10 minutes～1 hour time of drying;
C. isostatic cool pressing granulation: dried composite granule is suppressed through isostatic cool pressing under the pressure of 200～250MPa, taken out the back fragmentation,, obtain single-size after 1～3mm square hole sieve;
D. dry-pressing formed: is the mold (8) of right cylinder, square, rectangular parallelepiped or similar shape by punching block, under the pressure of 5～40MPa through press compression moulding with the particle after the granulation;
Being preferably putting into steel die after the uniformed powder weighing is mold (8) with the compression moulding of 300 tons of press cover half, makes releasing agent with whiteruss, ejects with die block;
E. the assembling of sintering cavity: is white clouds madreporic canal (2) profile of packing into cubes, the middle part is in the hole of agalmatolite body (1) of circular hole, graphite heating pipe (3) is packed in the white clouds madreporic canal (2), cubic boron nitride heat-transfer pipe (4) is packed in the graphite heating pipe (3), with mold (8) the molybdenum cup (5) (or other high temperature material) of packing into, again the molybdenum cup (5) that mold (8) is housed is put into cubic boron nitride heat-transfer pipe (4), load rhombspar plug (9) respectively at molybdenum cup (5) two ends, load onto graphite sheet (10) (concordant) in each rhombspar plug (9) outside with two of carbon tube, 2 copper current-conducting pieces (6) are placed the two ends of graphite heating pipe (3) respectively, 2 Conducting steel bowls (7) are contained in the outside of each copper current-conducting piece (6) respectively, promptly constitute a sintering cavity.
F. ultra-high pressure sintering: the sintering cavity that assembles is put into cubic hinge press, begin heating after being pressurized to 1～7GPa, be warmed up to 800～1500 ℃, heat-insulation pressure keeping 15min, then release, cooling, taking-up mold (8) namely make and contain γ-Si
3N
4The ceramic product of powder.
In another content of the present invention: the grinding described in the step (a) is preferably wet grinding in solvent dehydrated alcohol, aqueous ethanol, acetone, water, removes by filter solvent then.
In another content of the present invention: it is diameter 8～40mm, height cylindric of 5～20mm that the compression moulding described in the step (d) is preferably compression moulding.
In another content of the present invention: γ-Si described in the step (a)
3N
4Granularity be that sub-micron is to nanometer preferably; Described Al
2O
3, ZrO
2, α or β phase Si
3N
4, SiC, BN or AlN granularity be that tens of microns are to sub-micron preferably; Described sintering aid Y
2O
3, Al
2O
3, La
2The granularity of O is that tens of microns are to sub-micron preferably.
Compared with prior art, the present invention has following characteristics and beneficial effect:
(1) adopts the γ-Si that contains that the present invention makes
3N
4The silicon nitride ceramic material of powder, density height, uniform microstructure, mechanical property excellence; This new ceramics is a kind of ultra hard ceramic, because its high rigidity (hardness only is lower than diamond and cubic boron nitride) and chemical inertness (under normal temperature and the not too high temperature not with all acid-base reaction), its sintered body can be made various machining tools, bad working environments (strong acid and strong base, high temperature, rub by force sassafras) time instrument and meter, bearing supporting member; Also be wide energy carrying semiconductor material and the high optical material of refractive index, can be used as the high performance device in the optoelectronic areas; This pottery can be widely used in machinery,, the technical field such as chemical industry, Aero-Space, photoelectron;
(2) the present invention adopt super-pressure (1～7GPa), low temperature, fast, the sintering technology controlled of no atmosphere, can burn to realize the multi-disc dress by the appropriate design sintering cavity, the acquisition silicon nitride (or other) ceramic uniform microstructure, mechanical property excellence, cost is lower;
(3) technology of the present invention is simple, easy handling, and sintering temperature is low, and sintering time and with short production cycle is practical.
Description of drawings
Fig. 1 is the assembling vertical profile TV structure synoptic diagram of sintering cavity in the embodiment of the invention;
Fig. 2 is the sintered compact photo of the undressed processing that makes of the embodiment of the invention 1;
Fig. 3 is sintered compact (middle body) photo of the face that makes of the embodiment of the invention 1 after through polishing;
Fig. 4 is the sintered compact fracture sem photograph that the embodiment of the invention 1 makes;
Fig. 5 is the sintered compact photo of the undressed processing that makes of the embodiment of the invention 2;
Fig. 6 is sintered compact (middle body) photo of the face that makes of the embodiment of the invention 2 after through polishing;
Fig. 7 is the sintered compact fracture sem photograph that the embodiment of the invention 2 makes.
Among the figure: 1-agalmatolite body, 2-white clouds madreporic canal, 3-graphite heating pipe, 4-cubic boron nitride heat-transfer pipe, 5-molybdenum cup, 6-copper current-conducting piece, 7-Conducting steel bowl, 8-mold, 9-rhombspar plug, 10-graphite sheet.
Embodiment
Embodiment 1: referring to accompanying drawing 1-4.
A kind of preparation method who contains the pottery of powder body of cubic silicon nitride comprises the following steps:
A, batching are ground: press γ-Si
3N
425% (particle mean size 30nm), α-Si
3N
470% (200 order), sintering aid (being 200 orders) Y
2O
31%, Al
2O
32%, La
2The weight percent of O 2% after the amount of the getting batching, carried out mixed grinding 4 hours take absolute ethyl alcohol as abrasive media respectively, obtained finely dispersed composite granule;
B, drying: the composite granule after will grinding in infrared drying oven (power 500W) dry 10 minutes;
C, isostatic cool pressing granulation: dried composite granule is suppressed through isostatic cool pressing under the pressure of 250MPa, taken out the back fragmentation,, obtain single-size after 1～3mm square hole sieve;
D, dry-pressing formed: is the cylindric mold 8 of 8 * 7.5mm by punching block, under the pressure of 25MPa through 300 tons of press compression mouldings with the particle after the granulation;
E, the assembling of sintering cavity: is white clouds madreporic canal 2 profile of packing into cubes, the middle part is in the hole of agalmatolite body 1 of circular hole, graphite heating pipe 3 is packed in the white clouds madreporic canal 2, cubic boron nitride heat-transfer pipe 4 is packed in the graphite heating pipe 3, with the mold 8 molybdenum cup 5 of packing into, again the molybdenum cup 5 that mold 8 is housed is put into cubic boron nitride heat-transfer pipe 4, load rhombspar plug 9 respectively at molybdenum cup 5 two ends, load onto graphite sheet 10 in each rhombspar plug 9 outside, 2 copper current-conducting pieces 6 are placed the two ends of graphite heating pipe 3 respectively, 2 Conducting steel bowls 7 are contained in the outside of each copper current-conducting piece 6 respectively, promptly constitute a sintering cavity;
The physical dimension of agalmatolite body 1 (mould) is 32.5 * 32.5 * 32.5cm
3, there is the circular hole of a 18mm centre, counts from a side, and hole depth 25.5mm, opposite side are the circular hole of 14 * 7mm;
The design of sintering mold and material:
The main body mould: the 1 usefulness pyrophyllite powder briquetting compression moulding of agalmatolite body, agalmatolite is placed on the outside of sintering cavity, plays pressure transmission, insulation and adiabatic effect;
Heating material: realize heating by electrical heating, formed by Conducting steel bowl, heating graphite pipe, graphite and copper current-conducting piece;
Internal layer pressure transmission heat-transfer medium: be lathed pipe with natural rhombspar, make the internal layer pressure tube; Make heat-transfer pipe with the cold-rolled sintered method of hexagonal boron nitride;
Sample protection spare: the molybdenum cup that two internal-and external diameters making with metal molybdenum material match oppositely fastens sample;
F, ultra-high pressure sintering: the sintering cavity that assembles is put into cubic hinge press, be pressurized to and begin heating behind the 5.7GPa, be warmed up to 1300 ℃, heat-insulation pressure keeping 15min, then release, cooling, taking-up mold 8 are namely finished and are contained γ-Si
3N
4The silicon nitride ceramics sintering of powder, make and contain γ-Si
3N
4The ceramic product of powder (sintered body in the accompanying drawing).
This preparation method can also comprise polishing, cleaning step, uses diamond abrasive that is:, contains γ-Si to making
3N
4The ceramic product of powder---fine grinding, polishing are carried out in the silicon nitride ceramics surface; Soak the silicon nitride ceramics that has polished with watery hydrochloric acid again, running water cleans.
The salient features of the silicon nitride ceramics knot body that this embodiment makes sees the following form.
| Performance indications | Test data |
| Relative density/% | 98.7 |
| Rockwell hardness H RA | 100 |
| Vickers hardness H V/ GPa (indentation load 1kgf) | 21.2 |
Find out that from performance test data the relative density of pottery reaches 98.7%, than traditional technology of preparing height (relative density such as the silicon nitride ceramics of atmosphere sintering is below 95%); Its Vickers hardness reaches 21.2GPa, than not adding γ-Si
3N
4α-Si
3N
4The Vickers hardness height (usually less than 20GPa) of pottery.
Embodiment 2: referring to accompanying drawing 1,5～7.
A kind of preparation method who contains the pottery of powder body of cubic silicon nitride comprises the following steps:
A, batching are ground: press γ-Si
3N
495% (particle mean size 30nm), sintering aid (being 200 orders) Y
2O
31%, Al
2O
32%, La
2The weight percent of O 2% after the amount of the getting batching, carried out mixed grinding 4 hours take absolute ethyl alcohol as abrasive media respectively, obtained finely dispersed composite granule;
B, drying: the composite granule after will grinding in infrared drying oven (power 500W) dry 10 minutes; Temperature is controlled in 120 ℃;
C, isostatic cool pressing granulation: dried composite granule is suppressed through isostatic cool pressing under the pressure of 250MPa, taken out the back fragmentation,, obtain single-size after 1～3mm square hole sieve;
D, dry-pressing formed: is the cylindric mold 8 of 8 * 7.5mm by punching block, under the pressure of 25MPa through press compression moulding with the particle after the granulation;
E, the assembling of sintering cavity: is white clouds madreporic canal 2 profile of packing into cubes, the middle part is in the hole of agalmatolite body 1 of circular hole, graphite heating pipe 3 is packed in the white clouds madreporic canal 2, cubic boron nitride heat-transfer pipe 4 is packed in the graphite heating pipe 3, with the mold 8 molybdenum cup 5 of packing into, again the molybdenum cup 5 that mold 8 is housed is put into cubic boron nitride heat-transfer pipe 4, load rhombspar plug 9 respectively at molybdenum cup 5 two ends, load onto graphite sheet 10 in each rhombspar plug 9 outside, 2 copper current-conducting pieces 6 are placed the two ends of graphite heating pipe 3 respectively, 2 Conducting steel bowls 7 are contained in the outside of each copper current-conducting piece 6 respectively, promptly constitute a sintering cavity;
F, ultra-high pressure sintering: the sintering cavity that assembles is put into cubic hinge press, and (agglomerating plant realizes containing γ-Si
3N
4Powder silicon nitride ceramics low temperature, fast, the sintering controlled of no atmosphere; Cavity temperature is demarcated with the pressure variation by the phase transformation of bismuth, thallium, barium with double platinum rhodium thermocouple measurement, pressure) in, begin heating after being pressurized to 5.7GPa, be warmed up to 1500 ℃, heat-insulation pressure keeping 25min, then release, cooling, taking-up mold 8 are namely finished and are contained γ-Si
3N
4The silicon nitride ceramics sintering of powder, make and contain γ-Si
3N
4The ceramic product of powder (sintered body in the accompanying drawing).
This preparation method can also comprise polishing, cleaning step, uses diamond abrasive that is:, contains γ-Si to making
3N
4The ceramic product of powder---fine grinding, polishing are carried out in the silicon nitride ceramics surface; Soak the silicon nitride ceramics that has polished with watery hydrochloric acid again, running water cleans.
The salient features of the silicon nitride ceramics knot body that this embodiment makes sees the following form.
| Performance indications | Test data |
| Relative density/% | 96.8 |
| Rockwell hardness H RA | 120 |
| Vickers hardness H V/ GPa (indentation load 1kgf) | 25.2 |
From performance test data, find out γ-Si
3N
4The relative density of pottery is 96.8%, and its Vickers hardness reaches 25.2GPa, has higher Vickers hardness.
Embodiment 3-9:
A kind of pottery that contains powder body of cubic silicon nitride, this ceramic weight percent composition sees the following form respectively:
γ-Si described in the table
3N
4Granularity be that sub-micron is to nanometer; Described Al
2O
3, ZrO
2, α or β phase Si
3N
4, SiC, BN or AlN granularity be that tens of microns are to sub-micron; Described sintering aid Y
2O
3, Al
2O
3, La
2The granularity of O is that tens of microns are to sub-micron.
Each embodiment contains the preparation method of pottery of powder body of cubic silicon nitride with embodiment 1 or 2 or identical with the process step described in the content of the present invention and condition, parameter, slightly in the table.
The invention is not restricted to above-described embodiment, content of the present invention is described all can implement and have described good result.
Claims (5)
1. a pottery that contains cubic silicon nitride is characterized in that this ceramic weight percent consists of: γ-Si
3N
45%～100%, Al
2O
3, ZrO
2, α or β phase Si
3N
4, at least a 0～95% among SiC, BN, the AlN, and sintering aid Y
2O
3, Al
2O
3, La
2Among the O at least a 0～10%.
2. a preparation method who contains the pottery of powder body of cubic silicon nitride is characterized in that comprising the following steps:
A. batching is ground: press γ-Si
3N
45%～100%, Al
2O
3, ZrO
2, α or β phase Si
3N
4, at least a 0～95% among SiC, BN, the AlN, sintering aid Y
2O
3, Al
2O
3, La
2After the amount of the getting batching, mixed grinding 4～8 hours obtains finely dispersed composite granule at least a 0～10% weight percent respectively among the O;
B. dry: that composite granule is done dry the processing through infrared ray, vacuum or a conventional oven;
C. isostatic cool pressing granulation: dried composite granule is suppressed through isostatic cool pressing under the pressure of 200～250MPa, taken out the back fragmentation,, obtain single-size after 1～3mm square hole sieve;
D. dry-pressing formed: is the mold (8) of right cylinder, square, rectangular parallelepiped or similar shape by punching block, under the pressure of 5～40MPa through press compression moulding with the particle after the granulation;
E. the assembling of sintering cavity: is white clouds madreporic canal (2) profile of packing into cubes, the middle part is in the hole of agalmatolite body (1) of circular hole, graphite heating pipe (3) is packed in the white clouds madreporic canal (2), cubic boron nitride heat-transfer pipe (4) is packed in the graphite heating pipe (3), with mold (8) the molybdenum cup (5) of packing into, again the molybdenum cup (5) that mold (8) is housed is put into cubic boron nitride heat-transfer pipe (4), load rhombspar plug (9) respectively at molybdenum cup (5) two ends, load onto graphite sheet (10) in each rhombspar plug (9) outside, 2 copper current-conducting pieces (6) are placed the two ends of graphite heating pipe (3) respectively, 2 Conducting steel bowls (7) are contained in the outside of each copper current-conducting piece (6) respectively, promptly constitute a sintering cavity;
F. ultra-high pressure sintering: the sintering cavity that assembles is put into cubic hinge press, begin heating after being pressurized to 1～7GPa, be warmed up to 800～1500 ℃, heat-insulation pressure keeping 15～80min, then release, cooling, taking-up mold (8) namely make and contain γ-Si
3N
4The ceramic product of powder.
3. by the described preparation method who contains the pottery of powder body of cubic silicon nitride of claim 2, it is characterized in that: the grinding described in the step (a) is wet grinding in solvent dehydrated alcohol, aqueous ethanol, acetone, water, removes by filter solvent then.
4. by the described preparation method who contains the pottery of powder body of cubic silicon nitride of claim 2, it is characterized in that: the compression moulding described in the step (d) is that compression moulding is diameter 8～40mm, height 5～20mm cylindric.
5. by the described preparation method who contains the pottery of powder body of cubic silicon nitride of claim 2, it is characterized in that: γ-Si described in the step (a)
3N
4Granularity be that sub-micron is to nanometer; Described Al
2O
3, ZrO
2, α or β phase Si
3N
4, SiC, BN, AlN granularity be that tens of microns are to sub-micron; Described sintering aid Y
2O
3, Al
2O
3, La
2The granularity of O is that tens of microns are to sub-micron.
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