CN101913879A - Silicon nitride material and preparation method thereof, as well as silicon nitride heating device and production method thereof - Google Patents
Silicon nitride material and preparation method thereof, as well as silicon nitride heating device and production method thereof Download PDFInfo
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- CN101913879A CN101913879A CN 201010271873 CN201010271873A CN101913879A CN 101913879 A CN101913879 A CN 101913879A CN 201010271873 CN201010271873 CN 201010271873 CN 201010271873 A CN201010271873 A CN 201010271873A CN 101913879 A CN101913879 A CN 101913879A
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Abstract
The invention relates to a silicon nitride material and a preparation method thereof, as well as a silicon nitride heating device and production method thereof. The silicon nitride material comprises the following components in percentage by weight: 78%-98% of silicon nitride power, 0.2%-9% of aluminum oxide, 0.2%-9% of yttrium oxide and 0.05%-5% of tungsten carbide, and the silicon nitride material is prepared by the following steps of: weighing all the raw materials. putting in a container, ball-milling and stirring; putting material slurry obtained after ball milling in an oven for drying to obtain material powder; and finally pelleting by cold isostatic pressing. The silicon nitride heating device comprises resistor heating units and a substrate; the resistor heating units are arranged on the surface of the substrate or in the substrate; and the substrate is made of the silicon nitride material. The production method of the heating device comprises the steps of: imbedding the silicon nitride material and the resistor heating units according to prefabricated shape and position and pressing into green ware, and then putting the green ware in a furnace atmosphere to carry out pressure sintering to obtain the finished heating device.
Description
Technical field
The present invention relates to silicon nitride material and preparation method thereof and silicon nitride heater members and preparation method thereof, belong to field of inorganic nonmetallic material.
Background technology
The heater block of the instantaneously heated type heater of each brand generally is made of metal or the coated ceramic coating on the market now, metal well heater has generally been arranged resistance wire heating element at the back side of aluminium sheet, its existing problem is that the thickness of metal its hot-plate of well heater need reach 15 centimetres, because thin metal sheet can produce crooked and strain etc. in heat-processed, if the hot-plate thickening is become the heaviness except meeting makes well heater, the temperature of hot-plate can not become with voltage or strength of current immediately yet, has so just caused problems such as wayward temperature.This well heater and water are noncontacts, so heating efficiency is low, are subject to the influence of hydraulic pressure water temperature in the use.In addition, commonplace heater structure is to do the structure that the heating element outsourcing forms the combined type heating element with copper material behind the nichrome wire outsourcing insulating material at present, because residual a large amount of air make the high temperature resistance silk extremely short because of the oxidation life-span.
Advantages such as and ceramic heating element can rapid heating because of the heat transfer efficiency height, is difficult for being corroded, and dirt can not given birth in the surface, and the life-span is long, thereby the development and Design ceramic heater becomes a kind of trend.
The flat 9-306642 of Japan's public publication, the flat 4-324276 of Japanese public publication etc. have proposed ceramic heater, wherein adopt aluminium nitride as base material (because aluminium nitride thermal conductivity up to 180W/m.K), and on the surface of this aluminium nitride base material or the inner resistance heating element that forms of base material.Because the aluminium nitride base material has high thermal conductivity, so the temperature of hot-plate can change rapidly with the temperature of resistance heating element, make its Controllable Temperature, but aluminium nitride is expensive as base material.
Publication number is to have announced a kind of silicon nitride heat generating body and preparation method thereof in 99113534.2 the patent, this heating element is that resistance wire and silicon nitride composite material are sintered into one, though because the secluding air source is improved its life-span greatly, but this structure still can't be broken away from the threat of air residual in the sintered compact to resistance wire, 01136305.3 having announced, number patent utilize the nano-grade silicon nitride powder to insert the ceramic heater that common silicon nitride powder carries out modification, though after adding the nano-grade silicon nitride powder its surface energy is increased, the intergranular contact area strengthens, temperature and pressure when having reduced sintering, realized the moulding of normal temperature sintered silicon nitride, but α-phase nano-grade silicon nitride micro mist add-on too conference causes the bad grasp of shrinkage, quantity acts on not too obvious very little, and its sintering temperature is up to 2100 ℃; And current, German BACH.RC and company of Kyocera occupy monopoly position in the international market.
Therefore, a kind of cost of development and Design ceramic heating element low, that product is stable becomes a kind of necessity.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of silicon nitride material and preparation method thereof and silicon nitride heater members and preparation method thereof are provided, to obtain a kind of ceramic heating element, be 30 times of metal heater life-span the work-ing life of the ceramic heating element that this material and preparation method make, adopt the gas pressure sintering can mass production, reduced the well heater cost, product be stable, long service life is used general.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of silicon nitride material, described silicon nitride material is made up of each raw material of following weight proportion: silicon nitride powder 78%～98%, aluminium sesquioxide 0.2%～9%, yttrium oxide 0.2%～9% and wolfram varbide 0.05%～5%.
The beneficial effect of silicon nitride material of the present invention is: silicon nitride material density is low, the lighter in weight of preparing, hardness and intensity height, and corrosion resistance and good, and silicon nitride material thermal conductivity height, insulation can not cause safety problem.The powder cost is low, does not need to add nano level powder or other the thermal expansivity metal-salt bigger than body material improves, and can obviously improve sintering effect, improves toughness or intensity.
On the basis of technique scheme, the present invention can also do following improvement.
Further, α phase silicon nitride content is more than 96% in the described silicon nitride powder.
Further, the median size of described silicon nitride powder is 0.1～6 μ m, and the median size of described aluminium sesquioxide is＜6 μ m, and the median size of described yttrium oxide is＜8 μ m.
Adopt the beneficial effect of above-mentioned further scheme to be, adopt the silicon nitride powder size range wider, contain nano-scale particle like this in the silicon nitride powder and more help sintering, aluminum oxide and yttrium oxide mix as sintering aid.
Another technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of silicon nitride material may further comprise the steps:
1). take by weighing each raw material by following weight proportion: silicon nitride powder 78%～98%, aluminium sesquioxide 0.2%～9%, yttrium oxide 0.2%～9% and wolfram varbide 0.05%～5%, insert in the alumina-ceramic can container, add abrasive and grinding medium, put into the ball mill ball milling and stirred 8～40 hours;
2) ball milling is good slip is crossed 30 mesh sieves, insert baking oven then, in 50～120 ℃ of temperature, dry 4～20 hours, after obtaining powder, with the powder isostatic cool pressing granulation under pressure 30MPa～120MPa in the spherical rubber mould of packing into, pulverize, after sieve, promptly get the heating unit that this silicon nitride material of silicon nitride material is made, described heating unit is made of lead, the heating element that links to each other with lead and matrix, it is characterized in that, described resistance heater is arranged in matrix inside, and described matrix is the silicon nitride material matrix.
The preparation method's of silicon nitride material of the present invention beneficial effect is: make silicon nitride powder mix, drying-granulating sieves and obtains the powder bigger than the powder particle size of raw material, has good mobility.
Further, the grinding medium in the described step 1) is ethanol, ethylene glycol or deionized water, and described grinding medium is silicon nitride or aluminum oxide.
Adopt the beneficial effect of above-mentioned further scheme to be, utilize grinding medium and mill ball that raw material is mixed.
Further, described step 2) in, slip drying 8～12 hours, obtain powder after, powder is packed in the spherical rubber mould in the granulation of pressure 80MPa isostatic cool pressing, obtain the powder that median size is 80～120 μ m after the drying.
Adopt the beneficial effect of above-mentioned further scheme to be, median size increases after the granulation, improves the flowability of powder, prepares the silicon nitride product of excellent performance.
The another technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of silicon nitride heater members, described heater members comprises resistance heater and matrix, described resistance heater is arranged in matrix surface or inside, described matrix is the silicon nitride material matrix, described resistance heater is the slurries heating element of tungsten filament, molybdenum filament or electrical conductor, and described silicon nitride material matrix is made by above-mentioned described silicon nitride material.
The beneficial effect of silicon nitride heater members of the present invention is: this heater members good insulating, and thermal conductivity is better, and is corrosion-resistant, and the life-span is long, toughness and intensity height, cost is low.
Further, described heating element is the slurries heating element of tungsten filament, molybdenum filament or electrical conductor.
Adopt the beneficial effect of above-mentioned further scheme to be, its fusing point of the electrical conductor that tungsten filament, molybdenum filament and slurries contain is far above the SINTERING FOR SILICON NITRIDE CERAM temperature, the thermal conductivity height, and thermal expansivity and silicon nitride ceramics differ and are not very big, can not cause the damage of ceramic body, be a kind of good heating element.
Further, the slurries of described electrical conductor comprise conducting medium, Resins, epoxy, alcohol and cellulose thickener.
Adopt the beneficial effect of above-mentioned further scheme to be, conducting medium and Resins, epoxy, alcohol and Mierocrystalline cellulose are mixed into the conduction slurries can be prepared into various required shapes and be printed on the stupalith matrix.
Further, described conducting medium is metallic particles, wolfram varbide or molybdenum silicide.
Adopt the beneficial effect of above-mentioned further scheme to be, metallic particles and wolfram varbide, molybdenum silicide thermal conductivity are bigger, can fully heat; Thermal expansivity and ceramic body are more or less the same, and are difficult for causing the ceramic body cracking; The too big just abundant sintering of conducting medium wolfram varbide or molybdenum silicide content in the ceramic heater makes the insufficient strength of resistance heating element, and skewness size partly is big, thereby causes the damage of resistance heating element; If wolfram varbide content just can not fully be heated very little.
Further, described metallic particles is the particle of gold and silver, platinum, palladium, lead, tungsten, molybdenum or nickel, and the median size of described metallic particles is 0.1～100 μ m.
Adopt the beneficial effect of above-mentioned further scheme to be, these metals are not easy oxidized, and have the ohmic value that is enough to produce heat.
Further, described metallic particles is tungsten or molybdenum.
Adopt the beneficial effect of above-mentioned further scheme to be, tungsten and molybdenum are the metals that fusing point is higher and thermal conductivity is best, and tungsten filament often is used to make the filament heating element.
The technical scheme again that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of silicon nitride heater members may further comprise the steps:
A. silicon nitride material is put into prefabricated mould, resistance heater is inserted by ready-formed shape and position,, obtain green compact in the compression moulding of pressure 60～200MPa isostatic cool pressing;
B. the green compact that obtain are processed into the ready-formed shape through lathe or grinding machine, put into stove and carry out gas pressure sintering, promptly get product.
The preparation method's of silicon nitride heater members of the present invention beneficial effect is: gas pressure sintering makes the resistance heating element heating element and the silicon nitride matrix material that occur in the integral production sintering process differ the rhegma phenomenon that causes greatly because of thermal expansivity, be fit to mass production, and making sintering process thermal expansivity because of body material and exothermic material can not occur differs and stress concentration occurs greatly and make product impaired, operating procedure is oversimplified, save raw material, greatly reduced production cost.
Further, described steps A expects matrix on by ready-formed shape cloth that for conducting electricity slurries lamination oxide compound on the described matrix is calcined, and obtains the green compact that the metallic particles sintering forms.
Adopt the beneficial effect of above-mentioned further scheme to be, coming the purpose of cloth according to shape is according to the power setting resistance sizes, and the lamination oxide compound carries out sintering and can promote metallic particles and matrix integrated.
Further, in the described steps A under pressure 150MPa～180MPa, isostatic cool pressing compression moulding.
Adopt the beneficial effect of above-mentioned further scheme to be, eliminate product defects, make sintering after product performance excellent more.
Further, the agglomerating detailed process is among the described step B: within 2 hours temperature is risen to 1000～1100 ℃, again pressure is added to 0.1～0.3MPa, continue to be warmed up to 1300 ℃, continue to be pressurized to 0.7～1MPa in the temperature-rise period, constant temperature pressurize 0.5～1 hour rises to temperature 1500～1640 ℃ then and continues to be pressurized to 2～3MPa simultaneously, heat-insulation pressure keeping 1 hour, continue to be warmed up to 1750 ℃, heat-insulation pressure keeping 1 hour is warming up to 1800～1850 ℃ again, pressure reaches 5～6MPa, be incubated 2 hours, stop then heating, unload and be pressed in after 8 hours temperature and reduce to 140 ℃, naturally cool to room temperature, obtain finished product.
Adopt the beneficial effect of above-mentioned further scheme to be, gas pressure sintering is lower than hot pressing sintering temperature, in that guarantee under the situation of excellent product performance can mass production, this has just shortened the technological process of production greatly, technological operation is oversimplified, save raw material, thereby greatly reduced production cost.
Further, the atmosphere among the described step B is nitrogen or argon gas.
Further, the atmosphere among the described step B is preferably nitrogen.
Adopt the beneficial effect of above-mentioned further scheme to be, the anti-oxidation of sintering under inert atmosphere.
Description of drawings
Fig. 1 is the preparation method's of a silicon nitride material of the present invention schema;
Fig. 2 is the preparation method's of a silicon nitride heater members of the present invention schema.
Embodiment
Below in conjunction with accompanying drawing principle of the present invention and feature are described, institute gives an actual example and only is used to explain the present invention, is not to be used to limit scope of the present invention.
Fig. 1 is the preparation method's of a silicon nitride material of the present invention schema, and as shown in Figure 1, the preparation method of silicon nitride material of the present invention may further comprise the steps:
1) takes by weighing each raw material by following weight percent: silicon nitride powder 78%～98%, aluminium sesquioxide 0.2%～9%, yttrium oxide 0.2%～9% and wolfram varbide 0.05%～5%, insert in the alumina-ceramic jar, add abrasive and grinding medium, ball milling stirred 8～40 hours;
2) ball milling is good slip sieves, and puts into baking oven, and in 50～120 ℃ of temperature, dry 4～20 hours, isostatic cool pressing granulation or spray drying granulation obtained silicon nitride powder under pressure 30MPa～120MPa.
Fig. 2 is the preparation method's of a silicon nitride heater members of the present invention schema, and as shown in Figure 2, the preparation method of silicon nitride heater members of the present invention may further comprise the steps:
A. silicon nitride material is put into prefabricated mould, resistance heater is inserted by ready-formed shape and position,, obtain green compact through dry-pressing and isostatic cool pressing compression moulding;
B. the green compact that obtain are processed into desired shape through lathe or grinding machine, put into the furnace atmosphere pressure sintering, promptly get goods.
With the 92.5g median size is the silicon nitride powder (wherein α phase silicon nitride content surpasses 96%) of 0.6 μ m; the 3g median size is the aluminium sesquioxide of 0.4 μ m; the 4g median size is that yttrium oxide and the 2g wolfram varbide of 0.5 μ m put into the ball milling special container; the ethanol that adds equivalent weight; put into behind the grinding medium silicon nitride ball milling 10 hours; put into 80 ℃ of oven for drying again 6 hours; afterwards with powder in the granulation of 100MPa isostatic cool pressing; the silicon nitride base-material diameter of particle that obtains is about 150 microns; put into prefabricated mould afterwards; simultaneously tungsten filament is imbedded in the silicon nitride base-material as requested as resistance heater; at the 150MPa cold isostatic compaction; blank after the moulding is put into sintering oven; the nitrogen atmosphere protection; in following heating process sintering: within 2 hours, temperature is risen to 1100 ℃; begin pressurization; continue to be warming up to 1200 ℃; be pressurized to 0.3MPa simultaneously; pressure reaches 1 MPa when being warming up to 1300 ℃; constant temperature pressurize 1 hour; when rising to 1640 ℃, temperature continues to be pressurized to 3MPa; heat-insulation pressure keeping 1 hour; be warming up to 1750 ℃ again; kept 1 hour; continue to be warming up to 1800 ℃; this moment, pressure reached 5.6 MPa; be incubated 2 hours, stop heat temperature raising then, unload and be pressed in after 8 hours temperature and reduce to 140 ℃; naturally cool to room temperature; obtain heater members, again with heater members and external wire bonds, process cutting and grinding machine are processed into the heating unit of desired size.
Through check, the technical indicator of the heating unit that makes is: the bending strength scope is 900MPa; Rockwell hardness is 92; The fracture toughness property scope is 9MPam
1/2Thermal expansivity is 3.6 * 10
-6/ ℃; Antiacid corrosive power: boiling is 6 hours in 5% sulphuric acid soln, and corrosion rate is less than 9g/m
2H; The alkali resistant corrosive power: boiling is 6 hours in 30% sodium hydroxide solution, and corrosion rate is less than 0.5g/m
2H, its power-adjustable are that the suitable medium of 1kw can be water or other liquid etc.
It with the 89g median size 6 microns silicon nitride powder; the 4g median size is 5 microns a aluminium sesquioxide; the 4g median size is that 7 microns yttrium oxide and 3g wolfram varbide put into the container of ball mill special use; the ethylene glycol that adds equivalent weight; put into behind the grinding medium silicon nitride ball milling 40 hours; put into 120 ℃ of oven for drying again 20 hours; with powder in the granulation of 60MPa isostatic cool pressing; put into prefabricated mould afterwards; the metal tungsten wire that designs is inserted according to both allocations; at the 160MPa cold isostatic compaction; insert in the accurate argon gas atmosphere sintering oven; the protection of feeding argon gas atmosphere; in following heating process sintering; within 2 hours, temperature is risen to 1000 ℃; begin to be forced into 0.1MPa when after this heating up; continue to be warming up to 1300 ℃; pressure reaches 0.8MPa; constant temperature pressurize 0.5 hour; when rising to 1500 ℃, temperature continues to be pressurized to 2MPa; heat-insulation pressure keeping 1 hour; be warming up to 1750 ℃ again; kept 1 hour; continuing to heat up is pressurized to 1850 ℃, and pressure reaches 6MPa, is incubated 2 hours; stop then heating; unload and be pressed in after 8 hours temperature and reduce to 140 ℃, naturally cool to room temperature, obtain heater members; with heater members and external wire bonds, process cutting and grinding machine are processed into the heating unit of desired size again.
Through check, the technical indicator of the heating unit that makes is: the bending strength scope is 860MPa; Rockwell hardness is 91; The fracture toughness property scope is 7.9MPam
1/2Thermal expansivity is 3.5 * 10
-6/ ℃ antiacid corrosive power: boiling is 6 hours in 5% sulphuric acid soln, and corrosion rate is less than 9g/m
2H; The alkali resistant corrosive power: boiling is 6 hours in 30% sodium hydroxide solution, and corrosion rate is less than 0.5g/m
2H, its power-adjustable are that the suitable medium of 0.85kw can be water or other liquid etc.
Embodiment 3
With the 78g median size is the aluminium sesquioxide that 3 microns silicon nitride powder and 9g median size are 2 microns, the 9g median size is 4 microns a yttrium oxide, the 4g wolfram varbide is put into the container of ball mill special use, the deionized water that adds equivalent weight, put into behind the grinding medium alumina lap ball ball milling 24 hours, put into 60 ℃ of oven for drying again 10 hours, with powder in the granulation of 70MPa isostatic cool pressing, put into prefabricated mould afterwards at the 200MPa cold isostatic compaction, with the conduction slurries according on the ceramic blank plate of set graphic printing after the moulding, put into accurate nitrogen atmosphere sintering oven, in following heating process sintering, within 2 hours, temperature is risen to 1100 ℃, be vacuum sintering before this, pressure is-0.1MPa, after this begin pressurization, pressure reaches 0.7MPa when being warming up to 1300 ℃, constant temperature pressurize 0.8 hour, when rising to 1600 ℃, temperature continues to be pressurized to 2.5MPa, heat-insulation pressure keeping 1 hour, be warming up to 1750 ℃ again, kept 1 hour, continue to heat up and be pressurized to 1850 ℃, pressure reaches 5MPa, be incubated 2 hours, stop then heating, unload and be pressed in after 8 hours temperature and reduce to 140 ℃, naturally cool to room temperature, obtain hot-plate, carry out heating and calcining then and remove and to desolvate, and make the metallic particles sintering, the slurries heating element that contains electrical conductor is so just cured on hot-plate, form heater members, again with heater members and external wire bonds, process cutting and grinding machine are processed into the heating unit of desired size.
Method according to embodiment 3 prepares heating unit, and the embodiment of the kind of described resistance heater is as shown in table 1 below.
Table 1 embodiment 4-6
According to embodiment 6 described heating units, the embodiment of the concrete kind of the slurries heating element of wherein said electrical conductor is as shown in table 2 below.
Table 2 embodiment 7-9
According to embodiment 7 described heating units, wherein said metallic particles concrete kind and the size embodiment as shown in table 3 below.
Table 3 embodiment 10-17
Through check, the technical indicator of the heating unit that the foregoing description makes is: the bending strength scope is 700～900MPa; Rockwell hardness is 91～92; The fracture toughness property scope is 7～9MPam
1/2Thermal expansivity is 3.3～3.6 * 10
-6/ ℃ antiacid corrosive power: boiling is 6 hours in 5% sulphuric acid soln, and corrosion rate is less than 9g/m
2H; The alkali resistant corrosive power: boiling is 6 hours in 30% sodium hydroxide solution, and corrosion rate is less than 0.5g/m
2H, its power-adjustable are that the suitable medium of 0.5～2kw can be water or other liquid etc.
The above only is preferred embodiment of the present invention, and is in order to restriction the present invention, within the spirit and principles in the present invention not all, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a silicon nitride material is characterized in that, described silicon nitride material is made up of each raw material of following weight percent: silicon nitride powder 78%～98%, aluminium sesquioxide 0.2%～9%, yttrium oxide 0.2%～9% and wolfram varbide 0.05%～5%.
2. silicon nitride material according to claim 1 is characterized in that, the median size of described silicon nitride powder is 0.1～6 μ m, and the median size of described aluminium sesquioxide is＜6 μ m, and the median size of described yttrium oxide is＜8 μ m.
3. the preparation method of silicon nitride material according to claim 1 is characterized in that, may further comprise the steps:
1). take by weighing each raw material by following weight percent: silicon nitride powder 78%～98%, aluminium sesquioxide 0.2%～9%, yttrium oxide 0.2%～9% and wolfram varbide 0.05%～5%, insert in the container, add abrasive and grinding medium, put into the ball mill ball milling and stirred 8～40 hours;
2) ball milling is good slip is crossed 30 mesh sieves, inserts baking oven then, in 50～120 ℃ of temperature, dry 4～20 hours, obtain powder after, with the powder isostatic cool pressing granulation under pressure 30MPa～120MPa in the spherical rubber mould of packing into, pulverize,, promptly get silicon nitride material after sieve.
4. the preparation method of silicon nitride material according to claim 3, it is characterized in that, described step 2) in, slip drying 8～12 hours, after obtaining powder, powder is packed in the spherical rubber mould in the granulation of pressure 80MPa isostatic cool pressing, obtain the powder that median size is 80～120 μ m after the drying.
5. silicon nitride heater members, described heater members comprises resistance heater and matrix, it is characterized in that, described resistance heater is arranged in matrix surface or inside, described matrix is the silicon nitride material matrix, described resistance heater is the slurries heating element of tungsten filament, molybdenum filament or electrical conductor, and described silicon nitride material matrix is made by claim 1 or 2 each described silicon nitride materials.
6. silicon nitride heater members according to claim 5 is characterized in that, the slurries heating element of described electrical conductor comprises: conducting medium, Resins, epoxy, alcohol and cellulose thickener, described conducting medium are metallic particles, wolfram varbide or molybdenum silicide.
7. silicon nitride heater members according to claim 6 is characterized in that, described metallic particles is the particle of gold and silver, platinum, palladium, lead, tungsten, molybdenum or nickel, and the median size of described metallic particles is 0.1～100 μ m.
8. the preparation method of a silicon nitride heater members is characterized in that, may further comprise the steps:
A. silicon nitride material is put into prefabricated mould as matrix, resistance heater is inserted by ready-formed shape and position again, under pressure 60～200MPa, dry-pressing or isostatic cool pressing compression moulding obtain green compact;
B. the green compact that obtain are processed into the ready-formed shape through lathe or grinding machine, put into stove and carry out gas pressure sintering, promptly get heater members.
9. the preparation method of silicon nitride heater members according to claim 8, it is characterized in that described step 1) is expected on the matrix lamination oxide compound on the described matrix for conducting electricity slurries by ready-formed shape cloth, calcine, obtain the green compact that the metallic particles sintering forms in the above.
10. the preparation method of silicon nitride heater members according to claim 8, it is characterized in that, described step 2) the agglomerating detailed process is in: within 2 hours temperature is risen to 1000～1100 ℃, again pressure is added to 0.1～0.3MPa, continue to be warmed up to 1300 ℃, continue to be pressurized to 0.7～1MPa in the temperature-rise period, constant temperature pressurize 0.5～1 hour, temperature is risen to 1500～1640 ℃ then and continue to be pressurized to 2～3MPa simultaneously, heat-insulation pressure keeping 1 hour continues to be warmed up to 1750 ℃, heat-insulation pressure keeping 1 hour, be warming up to 1800～1850 ℃ again, pressure reaches 5～6MPa, is incubated 2 hours, stop then heating, unload and be pressed in after 8 hours temperature and reduce to 140 ℃, naturally cool to room temperature, obtain finished product.
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