CN101913879B - 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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- CN101913879B CN101913879B CN 201010271873 CN201010271873A CN101913879B CN 101913879 B CN101913879 B CN 101913879B CN 201010271873 CN201010271873 CN 201010271873 CN 201010271873 A CN201010271873 A CN 201010271873A CN 101913879 B CN101913879 B CN 101913879B
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 3
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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 heating device and preparation method thereof, belong to field of inorganic nonmetallic material.
Background technology
On market, the heater block of the instantaneously heated type heater of each brand generally is made of metal or the coated ceramic coating 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 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 the problems such as wayward temperature.This well heater and water are non-contacting, so heating efficiency is low, are subject to the influence of hydraulic pressure water temperature in use.In addition, commonplace heater structure is to do with copper material the structure that the heating element outsourcing forms the combined type heating element after nichrome wire outsourcing insulating material at present, because residual large quantity of air makes the high temperature resistance silk extremely short because of oxidation life.
And ceramic heating element because of heat transfer efficiency is high can rapid heating, be difficult for being corroded, the advantage such as 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 temperature controlled, 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 patent, this heating element is that resistance wire and silicon nitride composite material are sintered into one, although because isolated air source is improved its life-span greatly, but this structure still can't be broken away from air residual in sintered compact to the threat of 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, although after adding the nano-grade silicon nitride powder, its surface can be 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, low, the ceramic heating element that product is stable of a kind of cost of development and Design 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 heating device 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 comprised 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, and the lighter in weight of preparing, hardness and intensity are high, corrosion resistance and good, and the silicon nitride material thermal conductivity is high, and 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 larger 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, in described silicon nitride powder, α phase silicon nitride content is more than 96%.
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 like this nano-scale particle in 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 comprises the following steps:
1). take 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 grinding stirring 8～40 hours;
2) slip that ball milling is good is crossed 30 mesh sieves, then insert baking oven, 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, namely get the heating unit that this silicon nitride material of silicon nitride material is made, described heating unit is made of wire, the heating element that is connected with wire 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 larger than the powder particle size of raw material, has mobility preferably.
Further, the grinding medium in 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 after obtaining powder, is packed in the spherical rubber mould powder in the granulation of pressure 80MPa isostatic cool pressing into, obtains the powder that median size is 80～120 μ m after drying.
Adopt the beneficial effect of above-mentioned further scheme to be, after granulation, median size increases, and improves the mobility 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 heating device, 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 silicon nitride material described above.
The beneficial effect of silicon nitride heating device 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, and toughness and intensity are high, and 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 temperature of silicon nitride ceramics, and thermal conductivity is high, and thermal expansivity and silicon nitride ceramics differ and be not very large, 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, epoxy resin, alcohol and cellulose thickener.
Adopt the beneficial effect of above-mentioned further scheme to be, conducting medium and epoxy resin, 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 larger, 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 large just abundant sintering of conducting medium wolfram varbide or molybdenum silicide content in ceramic heater make the insufficient strength of resistance heating element, and skewness size partly is large, thereby is caused 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 Au Ag Pt Pd, 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 heating device comprises the following steps:
A. silicon nitride material is put into prefabricated mould, resistance heater is inserted by prefabricated shape and position, in the compression moulding of pressure 60～200MPa isostatic cool pressing, obtain green compact;
B. the green compact that obtain are processed into prefabricated shape through lathe or grinding machine, put into stove and carry out gas pressure sintering, namely get product.
The preparation method's of silicon nitride heating device 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 on matrix by prefabricated shape cloth for conducting electricity slurries, and lamination oxide compound on 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, the lamination oxide compound carry out sintering can promote metallic particles and matrix integrated.
Further, in 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 more excellent.
further, in described step B, the detailed process of sintering is: temperature was risen to 1000～1100 ℃ within 2 hours, 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 temperature-rise period, constant temperature pressurize 0.5～1 hour, then temperature is risen to 1500～1640 ℃ and continue simultaneously to be pressurized to 2～3MPa, heat-insulation pressure keeping 1 hour, continue to be warmed up to 1750 ℃, heat-insulation pressure keeping 1 hour, be warming up to again 1800～1850 ℃, pressure reaches 5～6MPa, be incubated 2 hours, then stop heating, unload be pressed in 8 hours after temperature be down 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 the situation that guarantee that 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 in described step B is nitrogen or argon gas.
Further, the atmosphere in 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 silicon nitride material of the present invention schema;
Fig. 2 is the preparation method's of silicon nitride heating device of the present invention schema.
Embodiment
Below in conjunction with accompanying drawing, principle of the present invention and feature are described, example only is used for explaining the present invention, is not be used to limiting scope of the present invention.
Fig. 1 is the preparation method's of 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 comprises the following steps:
1) take 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 tank, add abrasive and grinding medium, ball grinding stirring 8～40 hours;
2) slip that ball milling is good 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 silicon nitride heating device of the present invention schema, and as shown in Figure 2, the preparation method of silicon nitride heating device of the present invention comprises the following steps:
A. silicon nitride material is put into prefabricated mould, resistance heater is inserted by prefabricated shape and position, through dry-pressing and isostatic cool pressing compression moulding, obtain green compact;
B. the green compact that obtain are processed into desired shape through lathe or grinding machine, put into the furnace atmosphere pressure sintering, namely get goods.
it is the silicon nitride powder (wherein α phase silicon nitride content surpasses 96%) of 0.6 μ m with the 92.5g median size, 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 after the grinding medium silicon nitride ball milling 10 hours, put into again 80 ℃ of oven for drying 6 hours, afterwards with powder in the granulation of 100MPa isostatic cool pressing, the silicon nitride base-material diameter of particle that obtains is 150 microns left and right, put into afterwards prefabricated mould, simultaneously tungsten filament is imbedded in the silicon nitride base-material as requested as resistance heater, at the 150MPa cold isostatic compaction, blank after moulding is put into sintering oven, the nitrogen atmosphere protection, in following heating process sintering: temperature was risen to 1100 ℃ within 2 hours, begin pressurization, continue to be warming up to 1200 ℃, be pressurized to simultaneously 0.3MPa, 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 again 1750 ℃, kept 1 hour, continue to be warming up to 1800 ℃, this moment, pressure reached 5.6 MPa, be incubated 2 hours, then stopped heating heats up, unload be pressed in 8 hours after temperature be down 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: in 5% sulphuric acid soln, boiling is 6 hours, and corrosion rate is less than 9g/m
2H; The alkali resistant corrosive power: in 30% sodium hydroxide solution, boiling is 6 hours, 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 is the silicon nitride powder of 6 microns with the 89g median size, the 4g median size is the aluminium sesquioxide of 5 microns, the 4g median size is that yttrium oxide and the 3g wolfram varbide of 7 microns put into the container of ball mill special use, the ethylene glycol that adds equivalent weight, put into after the grinding medium silicon nitride ball milling 40 hours, put into again 120 ℃ of oven for drying 20 hours, with powder in the granulation of 60MPa isostatic cool pressing, put into afterwards prefabricated mould, the metal tungsten wire that designs is inserted according to both allocations, at the 160MPa cold isostatic compaction, insert in accurate argon gas atmosphere sintering oven, pass into the argon gas atmosphere protection, in following heating process sintering, temperature was risen to 1000 ℃ within 2 hours, 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 again 1750 ℃, kept 1 hour, continue to heat up and be pressurized to 1850 ℃, pressure reaches 6MPa, be incubated 2 hours, then stop heating, unload be pressed in 8 hours after temperature be down 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 860MPa; Rockwell hardness is 91; The fracture toughness property scope is 7.9MPam
1/2Thermal expansivity is 3.5 * 10
-6/ ℃ antiacid corrosive power: in 5% sulphuric acid soln, boiling is 6 hours, and corrosion rate is less than 9g/m
2H; The alkali resistant corrosive power: in 30% sodium hydroxide solution, boiling is 6 hours, 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
be the aluminium sesquioxide that the silicon nitride powder of 3 microns and 9g median size are 2 microns with the 78g median size, the 9g median size is the yttrium oxide of 4 microns, the 4g wolfram varbide is put into the container of ball mill special use, the deionized water that adds equivalent weight, put into after the grinding medium alumina ceramic grinding ball ball milling 24 hours, put into again 60 ℃ of oven for drying 10 hours, with powder in the granulation of 70MPa isostatic cool pressing, put into afterwards prefabricated mould at the 200MPa cold isostatic compaction, with the conduction slurries according to set graphic printing on the ceramic blank plate after the moulding, put into accurate nitrogen atmosphere sintering oven, in following heating process sintering, temperature was risen to 1100 ℃ within 2 hours, be before this vacuum sintering, 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 again 1750 ℃, kept 1 hour, continue to heat up and be pressurized to 1850 ℃, pressure reaches 5MPa, be incubated 2 hours, then stop heating, unload be pressed in 8 hours after temperature be down to 140 ℃, naturally cool to room temperature, obtain hot-plate, then carry out the heating and calcining desolventizing, and make the metallic particles sintering, the slurries heating element that contains like this electrical conductor just is baked 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 the described heating unit of embodiment 6, 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 the described heating unit of embodiment 7, 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 above-described embodiment 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: in 5% sulphuric acid soln, boiling is 6 hours, and corrosion rate is less than 9g/m
2H; The alkali resistant corrosive power: in 30% sodium hydroxide solution, boiling is 6 hours, 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 is only 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., within all should being included in protection scope of the present invention.
Claims (9)
1. a silicon nitride material, is characterized in that, described silicon nitride material is comprised 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, comprises the following steps:
1). take 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 container, add abrasive and grinding medium, put into the ball mill ball grinding stirring 8～40 hours;
2) slip that ball milling is good is crossed 30 mesh sieves, then inserts baking oven, 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, namely get silicon nitride material.
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 drying.
5. silicon nitride heating device, 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 the described silicon nitride material of 2 any one.
6. silicon nitride heating device according to claim 5, is characterized in that, the slurries heating element of described electrical conductor comprises: conducting medium, epoxy resin, alcohol and cellulose thickener, described conducting medium are metallic particles, wolfram varbide or molybdenum silicide.
7. silicon nitride heating device according to claim 6, is characterized in that, described metallic particles is the particle of Au Ag Pt Pd, 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 heating device as described in claim 5 to 6 any one,
It is characterized in that, comprise the following steps:
A. silicon nitride material is put into prefabricated mould as matrix, then resistance heater is inserted by prefabricated shape and position, under pressure 60～200MPa, dry-pressing or isostatic cool pressing compression moulding obtain green compact;
B. the green compact that obtain are processed into prefabricated shape through lathe or grinding machine, put into stove and carry out gas pressure sintering, namely get heater members, wherein, described sintering process is: temperature was risen to 1000～1100 ℃ within 2 hours, 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 temperature-rise period, constant temperature pressurize 0.5～1 hour, then temperature is risen to 1500～1640 ℃ and continue simultaneously to be pressurized to 2～3MPa, heat-insulation pressure keeping 1 hour, continue to be warmed up to 1750 ℃, heat-insulation pressure keeping 1 hour, be warming up to again 1800～1850 ℃, pressure reaches 5～6MPa, be incubated 2 hours, then stop heating, release, temperature is down to 140 ℃ after 8 hours, naturally cool to room temperature.
9. the preparation method of silicon nitride heating device according to claim 8, it is characterized in that described steps A) expect on matrix lamination oxide compound on described matrix by prefabricated shape cloth for conducting electricity slurries, calcine, obtain the green compact that the metallic particles sintering forms in the above.
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| CN102584187B (en) * | 2012-01-16 | 2013-10-16 | 芜湖市天地电子科技有限公司 | High-boron tube and preparation method thereof |
| CN103922750B (en) * | 2014-04-18 | 2015-07-08 | 淄博大方新材料科技有限公司 | Wear-resistant silicon nitride ceramic material and preparation method thereof |
| CN105884563A (en) * | 2014-09-20 | 2016-08-24 | 盖德新材料科技南通有限公司 | Preparation method of special ceramic ignition device |
| CN104446507A (en) * | 2014-11-19 | 2015-03-25 | 东莞市国研电热材料有限公司 | Manufacturing method of ceramic heating element and ceramic heating element |
| CN105924179A (en) * | 2016-04-14 | 2016-09-07 | 北京中材人工晶体研究院有限公司 | Silicon nitride ceramic heater protection tube, preparation method and applications thereof |
| CN106083066A (en) * | 2016-06-12 | 2016-11-09 | 辽宁伊菲科技股份有限公司 | Silicon nitride adds the manufacture method of heat pipe |
| CN106255237A (en) * | 2016-08-25 | 2016-12-21 | 广东聚荣塑胶制品有限公司 | Electric heating water bag heater material prescription |
| CN109413783B (en) * | 2018-11-23 | 2021-07-30 | 福建闽航电子有限公司 | Manufacturing method of ceramic heating device for intelligent closestool |
| CN109620442A (en) * | 2018-12-20 | 2019-04-16 | 四川华柚医疗器械有限公司 | A kind of novel artificial tooth and preparation method thereof |
| CN110400928A (en) * | 2019-08-13 | 2019-11-01 | 上海电气集团股份有限公司 | A kind of preparation method of silicon based composite material |
| CN112385901A (en) * | 2019-10-23 | 2021-02-23 | 湖北中烟工业有限责任公司 | Heating element and preparation method and application thereof |
| CN116606146A (en) * | 2023-05-25 | 2023-08-18 | 宁波银瓷新材料有限公司 | High-yield silicon nitride substrate and preparation method thereof |
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