CN100381398C - Preparation method of AlN Si3N4-SiC ceramic material - Google Patents
Preparation method of AlN Si3N4-SiC ceramic material Download PDFInfo
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- CN100381398C CN100381398C CNB2005100412619A CN200510041261A CN100381398C CN 100381398 C CN100381398 C CN 100381398C CN B2005100412619 A CNB2005100412619 A CN B2005100412619A CN 200510041261 A CN200510041261 A CN 200510041261A CN 100381398 C CN100381398 C CN 100381398C
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910010293 ceramic material Inorganic materials 0.000 title abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011230 binding agent Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000011812 mixed powder Substances 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000009413 insulation Methods 0.000 claims description 29
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000012423 maintenance Methods 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000011863 silicon-based powder Substances 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000009702 powder compression Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 235000015895 biscuits Nutrition 0.000 abstract 3
- 238000000227 grinding Methods 0.000 abstract 2
- 239000008187 granular material Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 22
- 238000005516 engineering process Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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Abstract
The present invention discloses a preparation method of AlN-Si3N4-SiC ceramic material. Said method includes the following steps: mixing Al powder, S; powder and SiC granules according to the mass ratio of 1-5:1-7:3-7 to prepare raw material; adding anhydrous ethanol into above-mentioned raw material, ball-grinding to obtain a powder material, standing still in air and making solid-liquid separation, drying at 60-80deg.C; grinding dried powder material, adding binding agent, stirring and granulating; press-forming the granulated mixed powder material; drying press-formed biscuit at 100-120deg.C; prenitriding dried biscuit, making the prenitrided biscuit undergo the processes of nitridation reaction and sintering treatment so as to obtain the AlN-Si3N4-SiC ceramic material.
Description
One, technical field
The present invention relates to a kind of technology of preparing of diphase ceramic material, particularly a kind of AlN-Si
3N
4The preparation method of-SiC stupalith.
Two, background technology
Si
3N
4With SiC all is to use stupalith very widely at present.Si
3N
4Based composites is a kind of as high-temperature structural ceramics, have high temperature resistantly, corrosion-resistant, wear-resistant, anti-wash away, a series of excellent properties such as anti-oxidant behavior, can bear the harsh Working environment that metallic substance and organic polymer material are difficult to bear.But, Si
3N
4Stupalith is the compound based on covalent linkage, even it is at high temperature, the spread coefficient of atom is still very low, therefore, and simple Si
3N
4Stupalith is difficult to be prepared into fine and close high-strength material, must improve its tissue and performance by means of additive.And SiC is ceramic owing to have high sintering temperature, and sintering condition is also relatively harsher, and therefore also needing to add certain sintering aid reduces its sintering temperature, improves its sintering character.At present, Si
3N
4Be widely used in high-temperature material and superhard Materials with High Strength in conjunction with the SiC stupalith, still, in this material, Si
3N
4Exist tangible interfacial configuration between matrix and the SiC particle, the combination at this interface has limited Si
3N
4In conjunction with the further raising of SiC material property, also limited the add-on of SiC, with Si
3N
4Body material is compared, and the reinforced effects of this material is very limited.
Three, summary of the invention
The object of the present invention is to provide a kind of technology simple, AlN-Si with low cost and well behaved
3N
4The preparation method of-SiC stupalith.
The technical scheme that realizes the object of the invention is: a kind of AlN-Si
3N
4The preparation method of-SiC stupalith may further comprise the steps:
1.1 is 1～5: 1～7 with Al powder, Si powder and SiC particle by mass ratio: 3～7 preparation raw material;
1.2 the raw material for preparing is added dehydrated alcohol, ball milling in ball grinder;
1.3 leaving standstill, the powder that ball milling is good after solid-liquid separation, puts into the loft drier drying in air, dry under 60～80 ℃ of temperature;
1.4 dried powder is ground refinement;
1.5 in the powder that ground, add binding agent, carry out granulation by stirring then;
1.6 mixed powder compression moulding through granulation;
1.7 the material base after the compression moulding is carried out drying once more under 100～120 ℃ of temperature;
1.8 the material base that drying is crossed carries out pre-nitrogenize, the ceramic body after the pre-nitrogenize carries out the nitrogenizing reaction sintering and obtains AlN-Si
3N
4-SiC stupalith.
AlN-Si of the present invention
3N
4The preparation method's of-SiC stupalith pre-nitrogenize may further comprise the steps:
2.1 the material base shove charge that drying is crossed, and in stove, leave standstill to guarantee that whole base substrate has the uniform temperature field;
2.2 be warmed up to 400 ℃ with 10～40 ℃/hour heat-up rates, feed minor N
2, and vacuumize, make to keep-0.06 in the stove～-little negative pressure of 0.001MPa;
2.3 after vacuumizing end, with N
2: H
2=80～95: 20～5 volume ratio fed gas, keeps the pressure-fired of 0.001～0.040MPa in the stove, with 20～60 ℃/hour heat-up rates to 500 ℃ insulation 5～10 hours;
2.4 continue to be warmed up to 600 ℃～1000 ℃, be incubated outage after 20～60 hours, close air valve, rely on water-cooled cooling.
AlN-Si of the present invention
3N
4The preparation method's of-SiC stupalith nitrogenizing reaction sintering may further comprise the steps:
3.1 with the ceramic body shove charge after the pre-nitrogenize;
3.2 be warmed up to 400 ℃ with 10～40 ℃/hour heat-up rates, feed minor N
2, and vacuumize, make to keep-0.06 in the stove～-little negative pressure of 0.001MPa;
3.3 after vacuumizing end, with N
2: H
2=80～95: 20～5 volume ratio feeds gas, keeps the pressure-fired of 0.001～0.040MPa in the stove, with 20～60 ℃/hour heat-up rates to 500 ℃;
3.4 in 10～30 hours, furnace temperature is risen to 1000 ℃;
3.5 press N
2: H
2=75～80: 25～20 volume ratio feeds gas, when the stove internal gas pressure begins to descend, is incubated the state that returns to pressure-fired up to the stove internal gas pressure, heats up again;
3.6 temperature continues to be elevated to 1140 ℃, furnace pressure descends, this temperature maintenance 12 hours, and 1200 ℃ of insulations 9 hours, 1240 ℃ of insulations 8 hours, 1280 ℃ of insulations 7 hours, 1300 ℃ of insulations 5 hours;
3.7 temperature is elevated to 1360～1420 ℃, furnace pressure just often begins outage, but can not turn off intake valve, air outlet valve to prevent material base oxidation after the nitrogenize;
3.8 when temperature in the stove is dropped to 800 ℃, turn off intake valve and air outlet valve, rely on the recirculated water cooling.
AlN-Si of the present invention
3N
4The preparation method of-SiC stupalith can carry out pre-nitrogenize and nitrogenizing reaction sintering in the lump, may further comprise the steps:
4.1 the material base shove charge that drying is crossed, and in stove, leave standstill to guarantee that whole base substrate has the uniform temperature field;
4.2 be warmed up to 400 ℃ with 10～40 ℃/hour heat-up rates, feed minor N
2, and vacuumize, make to keep-0.06 in the stove～-little negative pressure of 0.001MPa;
4.3 after vacuumizing end, with N
2: H
2=80～95: 20～5 volume ratio fed gas, keeps the pressure-fired of 0.001～0.040MPa in the stove, with 20～60 ℃/hour heat-up rates to 500 ℃ insulation 5～10 hours;
4.4 continue to be warmed up to 600 ℃～1000 ℃, be incubated and do not cut off the power supply after 20～60 hours, press N
2: H
2=75～80: 25～20 volume ratio feeds gas, when the stove internal gas pressure begins to descend, is incubated the state that returns to pressure-fired up to the stove internal gas pressure, heats up again;
4.5 temperature continues to be elevated to 1140 ℃, furnace pressure descends, this temperature maintenance 12 hours, and 1200 ℃ of insulations 9 hours, 1240 ℃ of insulations 8 hours, 1280 ℃ of insulations 7 hours, 1300 ℃ of insulations 5 hours;
4.6 temperature is elevated to 1360～1420 ℃, furnace pressure just often begins outage, but can not turn off intake valve, air outlet valve to prevent material base oxidation after the nitrogenize;
4.7 when temperature in the stove is dropped to 800 ℃, turn off intake valve and air outlet valve, rely on the recirculated water cooling.
The present invention compared with prior art, its remarkable advantage is: (1) utilizes the AlN-Si of Si powder, Al powder and the preparation of particulate state SiC direct reaction sintering
3N
4-SiC stupalith has not only been simplified the preparation technology of material, and has reduced the preparation cost of material; (2) AlN-Si
3N
4-SiC stupalith and Si
3N
4-SiC stupalith is compared its mechanical property and is had increased significantly, and comprehensive use properties is better; (3) compare AlN-Si with the AlN-SiC stupalith
3N
4-SiC stupalith has significantly reduced sintering temperature, has changed the comparatively harsh present situation of sintering condition, has improved sintering character; (4) at Si
3N
4After adding Al in the SiC material, can utilize Al in the process of reaction sintering, to improve Si with the character of SiC formation sosoloid
3N
4Interfacial configuration between matrix and the SiC particle makes script be tending towards disappearing in the interface clearly, thereby has greatly eliminated boundary defect to effect of material performance.
Four, description of drawings
Fig. 1 is AlN-Si of the present invention
3N
4The preparation method's of-SiC stupalith schema.
Fig. 2 is AlN-Si of the present invention
3N
4The heating process curve of the pre-nitrogenize of preparation method of-SiC stupalith.
Fig. 3 is AlN-Si of the present invention
3N
4Preparation method's nitrogenizing reaction agglomerating heating process curve of-SiC stupalith.
Fig. 4 is AlN-Si of the present invention
3N
4Pre-nitrogenize of the preparation method of-SiC stupalith and the disposable heating process curve of nitrogenizing reaction sintering.
Five, embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
In conjunction with Fig. 1, AlN-Si of the present invention
3N
4The preparation method of-SiC stupalith may further comprise the steps:
1.1 is 2: 7: 3 preparation raw material with Al powder, Si powder and SiC particle by mass ratio.
1.2 the raw material for preparing is added dehydrated alcohol, ball milling in ball grinder, dehydrated alcohol did not have powder, treat that gas drains back sealing ball grinder, promptly adopt the mode that adds the dehydrated alcohol ball milling to carry out the refinement and the mixing of powder, material ball ratio is 1: 3, and the ball milling time is 2 hours.
Put into the loft drier drying 1.3 the powder that ball milling is good leaves standstill for some time in air after solid-liquid separation, drying temperature is 80 ℃, is no more than 80 ℃.
1.4 dried powder is ground refinement.
1.5 add the binding agent polyvinyl alcohol in the powder that ground, the concentration of polyvinyl alcohol is 6%, add-on is 10%, carries out granulation by stirring then, and the granulation particle diameter is about 0.5mm.
1.6 the mixed powder through granulation carries out dry-pressing formed under the pressure of 25MPa～250MPa.
1.7 the material base after dry-pressing formed is carried out drying once more, so that get rid of too much moisture in the green compact, under 40～60 ℃ temperature, be dried to water balance earlier when dry, reheat to 120 ℃ is incubated 24 hours.
1.8 the material base that drying is crossed carries out pre-nitrogenize, the ceramic body after the pre-nitrogenize carries out the nitrogenizing reaction sintering and obtains AlN-Si
3N
4-SiC stupalith.
In conjunction with Fig. 2, pre-nitrogenize wherein may further comprise the steps:
The first step, the material base shove charge that drying is crossed, and leaving standstill in stove about 10 hours makes blank adapt to temperature in the stove, to guarantee whole base substrate the uniform temperature field is arranged, and prevents in the temperature-rise period because the cracking of the blank that thermal stresses occurs;
Second step was warmed up to 400 ℃ with 20 ℃/hour heat-up rates, fed minor N
2, and vacuumize, to take out altogether 1.5 hours, per half hour, take out once, makes the little negative pressure of maintenance-0.01MPa in the stove;
The 3rd the step, vacuumize end after, with N
2: H
2=80～95: 20～5, as N
2: H
2=95: 5 volume ratio feeds gas, keeps 0.01 pressure-fired in the stove, goes out in the gas cylinder bubbling phenomenon and keeps constantly and be as the criterion, and too not fierce use nitrogen with 30 ℃/hour heat-up rates to 500 ℃, is incubated 5 hours;
In the 4th step, the volume ratio and the flow of gas remain unchanged, and continue to be warmed up to 1000 ℃, are incubated outage after 20 hours, close air valve, rely on water-cooled cooling.
In conjunction with Fig. 3, nitrogenizing reaction sintering wherein may further comprise the steps:
The first step with the ceramic body shove charge after the pre-nitrogenize, left standstill about 10 hours, made blank adapt to the interior temperature of stove;
Second step was warmed up to 400 ℃ with 20 ℃/hour heat-up rates, fed minor N
2, and vacuumize, to take out altogether 1.5 hours, per half hour, take out once, little negative pressure of maintenance-0.01MPa in the stove, this stage is not incubated;
The 3rd the step, vacuumize end after, the beginning with N
2: H
2=80～95: 20～5, as N
2: H
2=95: 5 ratio feeds gas, keeps the pressure-fired of 0.01MPa in the stove, keeps constantly and is as the criterion to go out in the gas cylinder bubbling phenomenon, does not use nitrogen too intensely, keeps 20 ℃/hour temperature rise rate to 500 ℃;
The 4th step, press in air flow, ratio of gas mixture and the stove to remain unchanged, with 20 hours furnace temperature is risen to 1000 ℃;
The 5th step changed ventilation volume than forming, and suitable increasing feeds the flow of gas, presses N
2: H
2=75～80: 25～20, as N
2: H
2=75: 25 volume ratio feeds gas, when the temperature of reaction furnace pressure begins to descend, because it is different that furnace pressure begins the temperature value that descends at every turn, begin to be incubated the state that returns to pressure-fired up to the stove internal gas pressure from that time that begins to descend, about 1070 ℃ of the temperature that begins to descend as furnace pressure, holding time is 24 hours, heats up again;
In the 6th step, temperature continues to be elevated to 1140 ℃, and furnace pressure descends, this temperature maintenance 12 hours, and 1200 ℃ of insulations 9 hours, 1240 ℃ of insulations 8 hours, 1280 ℃ of insulations 7 hours, 1300 ℃ of insulations 5 hours;
In the 7th step, temperature is elevated to 1360～1420 ℃, and furnace pressure just often begins outage, but can not turn off intake valve, air outlet valve to prevent material base oxidation after the nitrogenize;
The 8th step, when temperature in the stove is dropped to 800 ℃, turn off intake valve and air outlet valve, rely on the recirculated water cooling.
In conjunction with Fig. 4, in addition, AlN-Si of the present invention
3N
4Among the preparation method of-SiC stupalith, if ceramic material base need not machining after pre-nitrogenize, then pre-nitrogenize and nitrogenizing reaction sintering twice technology can be carried out in the lump, may further comprise the steps:
The first step, the material base shove charge that drying is crossed, and in stove, leave standstill to guarantee that whole base substrate has the uniform temperature field;
Second step was warmed up to 400 ℃ with 20 ℃/hour heat-up rates, fed minor N
2, and vacuumize, make the little negative pressure of maintenance-0.01MPa in the stove;
The 3rd the step, vacuumize end after, with N
2: H
2=80～95: 20～5, as N
2: H
2=95: 5 volume ratio fed gas, keeps the pressure-fired of 0.01MPa in the stove, with 30 ℃/hour heat-up rates to 500 ℃ insulation 5 hours;
The 4th step, continue to be warmed up to 1000 ℃, be incubated and do not cut off the power supply after 50 hours, press N
2: H
2=75～80: 25～20, as N
2: H
2=75: 25 volume ratio feeds gas, when the temperature of reaction furnace pressure begins to descend, because it is different that furnace pressure begins the temperature value that descends at every turn, begin to be incubated the state that returns to pressure-fired up to the stove internal gas pressure from that time that begins to descend, about 1070 ℃ of the temperature that begins to descend as furnace pressure, holding time is 24 hours, heats up again;
In the 5th step, temperature continues to be elevated to 1140 ℃, and furnace pressure descends, this temperature maintenance 12 hours, and 1200 ℃ of insulations 9 hours, 1240 ℃ of insulations 8 hours, 1280 ℃ of insulations 7 hours, 1300 ℃ of insulations 5 hours;
In the 6th step, temperature is elevated to 1420 ℃, and furnace pressure just often begins outage, but can not turn off intake valve, air outlet valve to prevent material base oxidation after the nitrogenize;
The 7th step, when temperature in the stove is dropped to 800 ℃, turn off intake valve and air outlet valve, rely on the recirculated water cooling.
Claims (4)
1. AlN-Si
3N
4The preparation method of-SiC stupalith is characterized in that may further comprise the steps:
1.1 is 1～5: 1～7 with Al powder, Si powder and SiC particle by mass ratio: 3～7 preparation raw material;
1.2 the raw material for preparing is added dehydrated alcohol, ball milling in ball grinder;
1.3 leaving standstill, the powder that ball milling is good after solid-liquid separation, puts into the loft drier drying in air, dry under 60～80 ℃ of temperature;
1.4 dried powder is ground refinement;
1.5 in the powder that ground, add binding agent, carry out granulation by stirring then;
1.6 mixed powder compression moulding through granulation;
1.7 the material base after the compression moulding is carried out drying once more under 100～120 ℃ of temperature;
1.8 the material base that drying is crossed carries out pre-nitrogenize, the ceramic body after the pre-nitrogenize carries out the nitrogenizing reaction sintering and obtains AlN-Si
3N
4-SiC stupalith.
2. AlN-Si according to claim 1
3N
4The preparation method of-SiC stupalith is characterized in that pre-nitrogenize may further comprise the steps:
2.1 the material base shove charge that drying is crossed, and in stove, leave standstill to guarantee that whole base substrate has the uniform temperature field;
2.2 be warmed up to 400 ℃ with 10～40 ℃/hour heat-up rates, feed minor N
2, and vacuumize, make to keep-0.06 in the stove～-little negative pressure of 0.001MPa;
2.3 after vacuumizing end, with N
2: H
2=80～95: 20～5 volume ratio fed gas, keeps the pressure-fired of 0.001～0.040MPa in the stove, with 20～60 ℃/hour heat-up rates to 500 ℃ insulation 5～10 hours;
2.4 continue to be warmed up to 600 ℃～1000 ℃, be incubated outage after 20～60 hours, close air valve, rely on water-cooled cooling.
3. AlN-Si according to claim 1
3N
4The preparation method of-SiC stupalith is characterized in that the nitrogenizing reaction sintering may further comprise the steps:
3.1 with the ceramic body shove charge after the pre-nitrogenize;
3.2 be warmed up to 400 ℃ with 10～40 ℃/hour heat-up rates, feed minor N
2, and vacuumize, make to keep-0.06 in the stove～-little negative pressure of 0.001MPa;
3.3 after vacuumizing end, with N
2: H
2=80～95: 20～5 volume ratio feeds gas, keeps the pressure-fired of 0.001～0.040MPa in the stove, with 20～60 ℃/hour heat-up rates to 500 ℃;
3.4 in 10～30 hours, furnace temperature is risen to 1000 ℃;
3.5 press N
2: H
2=75～80: 25～20 volume ratio feeds gas, when the stove internal gas pressure begins to descend, is incubated the state that returns to pressure-fired up to the stove internal gas pressure, heats up again;
3.6 temperature continues to be elevated to 1140 ℃, furnace pressure descends, this temperature maintenance 12 hours, and 1200 ℃ of insulations 9 hours, 1240 ℃ of insulations 8 hours, 1280 ℃ of insulations 7 hours, 1300 ℃ of insulations 5 hours;
3.7 temperature is elevated to 1360～1420 ℃, furnace pressure just often begins outage, but can not turn off intake valve, air outlet valve to prevent material base oxidation after the nitrogenize;
3.8 when temperature in the stove is dropped to 800 ℃, turn off intake valve and air outlet valve, rely on the recirculated water cooling.
4. AlN-Si according to claim 1
3N
4The preparation method of-SiC stupalith is characterized in that pre-nitrogenize and nitrogenizing reaction sintering are carried out in the lump, may further comprise the steps:
4.1 the material base shove charge that drying is crossed, and in stove, leave standstill to guarantee that whole base substrate has the uniform temperature field;
4.2 be warmed up to 400 ℃ with 10～40 ℃/hour heat-up rates, feed minor N
2, and vacuumize, make to keep-0.06 in the stove～-little negative pressure of 0.001MPa;
4.3 after vacuumizing end, with N
2: H
2=80～95: 20～5 volume ratio fed gas, keeps the pressure-fired of 0.001～0.040MPa in the stove, with 20～60 ℃/hour heat-up rates to 500 ℃ insulation 5～10 hours;
4.4 continue to be warmed up to 600 ℃～1000 ℃, be incubated and do not cut off the power supply after 20～60 hours, press N
2: H
2=75～80: 25～20 volume ratio feeds gas, when the stove internal gas pressure begins to descend, is incubated the state that returns to pressure-fired up to the stove internal gas pressure, heats up again;
4.5 temperature continues to be elevated to 1140 ℃, furnace pressure descends, this temperature maintenance 12 hours, and 1200 ℃ of insulations 9 hours, 1240 ℃ of insulations 8 hours, 1280 ℃ of insulations 7 hours, 1300 ℃ of insulations 5 hours;
4.6 temperature is elevated to 1360～1420 ℃, furnace pressure just often begins outage, but can not turn off intake valve, air outlet valve to prevent material base oxidation after the nitrogenize;
4.7 when temperature in the stove is dropped to 800 ℃, turn off intake valve and air outlet valve, rely on the recirculated water cooling.
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|---|---|---|---|
| CNB2005100412619A CN100381398C (en) | 2005-07-29 | 2005-07-29 | Preparation method of AlN Si3N4-SiC ceramic material |
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|---|---|---|---|
| CNB2005100412619A CN100381398C (en) | 2005-07-29 | 2005-07-29 | Preparation method of AlN Si3N4-SiC ceramic material |
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| CN107963891A (en) * | 2016-10-20 | 2018-04-27 | 南京理工大学 | A kind of single-phase silicon nitride ceramic material and its microwave sintering preparation process |
| CN113686161A (en) * | 2021-08-27 | 2021-11-23 | 江苏双发机械有限公司 | Method for sintering and curing inner barrel hanging piece of castable preheater and inner barrel hanging piece |
| CN114149269B (en) * | 2021-12-02 | 2022-11-04 | 北京科技大学 | AlN-SiC solid solution combined SiC composite refractory material for side wall of aluminum electrolytic cell and preparation method thereof |
| CN115772039A (en) * | 2022-12-14 | 2023-03-10 | 衡阳凯新特种材料科技有限公司 | Preparation method of silicon nitride heating body with heating film |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061961A (en) * | 1990-11-26 | 1992-06-17 | E.R.斯奎布父子公司 | 1,2-indane and quinoline |
| CN1063859A (en) * | 1991-02-08 | 1992-08-26 | 中国科学院上海硅酸盐研究所 | The preparation of silicon-carbide-silicon nitride complex phase gradient material |
| CN1026482C (en) * | 1991-02-04 | 1994-11-09 | 冶金工业部钢铁研究总院 | Making method of crystal whisker excess weld metal silicon nitride compound material |
| CN1045282C (en) * | 1993-09-03 | 1999-09-29 | 中国科学院上海硅酸盐研究所 | High-compact low-porosity silicon nitride-silicon carbide-oxide system as refractory material |
-
2005
- 2005-07-29 CN CNB2005100412619A patent/CN100381398C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061961A (en) * | 1990-11-26 | 1992-06-17 | E.R.斯奎布父子公司 | 1,2-indane and quinoline |
| CN1026482C (en) * | 1991-02-04 | 1994-11-09 | 冶金工业部钢铁研究总院 | Making method of crystal whisker excess weld metal silicon nitride compound material |
| CN1063859A (en) * | 1991-02-08 | 1992-08-26 | 中国科学院上海硅酸盐研究所 | The preparation of silicon-carbide-silicon nitride complex phase gradient material |
| CN1045282C (en) * | 1993-09-03 | 1999-09-29 | 中国科学院上海硅酸盐研究所 | High-compact low-porosity silicon nitride-silicon carbide-oxide system as refractory material |
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