CN102595665A - Silicon nitride heating sheet and manufacturing method thereof - Google Patents
Silicon nitride heating sheet and manufacturing method thereof Download PDFInfo
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- CN102595665A CN102595665A CN2012100471693A CN201210047169A CN102595665A CN 102595665 A CN102595665 A CN 102595665A CN 2012100471693 A CN2012100471693 A CN 2012100471693A CN 201210047169 A CN201210047169 A CN 201210047169A CN 102595665 A CN102595665 A CN 102595665A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 47
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000010438 heat treatment Methods 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 123
- 239000011651 chromium Substances 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 28
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 16
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 15
- 238000003466 welding Methods 0.000 claims abstract description 15
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 29
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 21
- 238000005516 engineering process Methods 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 20
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 14
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- 239000011733 molybdenum Substances 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 239000011265 semifinished product Substances 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 230000009514 concussion Effects 0.000 claims description 3
- 238000007731 hot pressing Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 abstract description 3
- 238000010304 firing Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract 2
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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Abstract
The invention relates to a heating sheet, in particular to a silicon nitride heating sheet and a manufacturing method thereof. The silicon nitride heating sheet comprises a body and a heating body positioned in the body, wherein the body is formed by firing silicon nitride powder, and the silicon nitride heating sheet is characterized in that the heating body comprises a heating area and a non-heating area which is positioned at the tail end of the heating body and used for welding a leading wire, and the heating area is formed by mixing and firing titanium carbide (TiC) powder, tantalous carbide (TaC) powder, aluminum oxide (Al2O3) powder, zirconium oxide (ZrO2) powder, yttrium oxide (Y2O3) powder, tungsten carbide (WC) powder, nickel (Ni) powder, chromium (Cr) powder and silicon nitride (Si3N4) powder. Compared with the prior art, because the heating body in the heating sheet body of the heating sheet disclosed by the invention is formed by sintering conductive ceramic powder, the stability of a product can be effectively improved, the shortcomings that the heating body in the prior art is easy to fracture, poor in integrity when sintered with the body, low in finished product rate of a product, instable in using performances and the like can be overcome, and the heating sheet has the significant advantages of stable performances, high production efficiency, high power and the like.
Description
Technical field
The present invention relates to a kind of heating plate, specifically a kind of silicon nitride heating plate and manufacturing approach thereof.
Background technology
As everyone knows, silicon nitride ceramic material has good thermal stability, can on very little area, produce powerful heating element, and the silicon nitride heating plate is that a kind of application prospect is extensive, the product of good energy-conserving effect.The tungsten filament that the general employing of silicon nitride heating plate at present will be used to generate heat directly adds in the beta-silicon nitride powder, forms through firing then.Because tungsten filament and beta-silicon nitride powder have tangible interface, be difficult to behind the sintering become one, tungsten filament is prone to short splitting in the production process of product, or resistance value changes in sintering process, causes properties of product unstable, and rate of finished products is lower.In order to address the above problem, CN102300347A proposes a kind of silicon nitride composite exothermic body and preparation method thereof, and its pyrotoxin is processed by multiple metal-powder such as copper, tungsten, nickel etc., in the hope of obtaining the integraty behind the sintering.But in fact; Because its pyrotoxin that adopts is still metallics; Still there is the interface in made heater and the silicon nitride of metal-powder behind the sintering, and product still exists defectives such as finished product rate variance, power are low, unstable properties, the pyrotoxin that adopts metal material to make in addition; Heating effect is undesirable, can not satisfy the demand of high-power heating plate.
Summary of the invention
The present invention is directed to the shortcoming and defect that exists in the prior art, propose a kind of add thermally-stabilised, the life-span long, not fragile and be specially adapted to silicon nitride heating plate and the manufacturing approach thereof that high-power heating plate is made.
The present invention can reach through following measure:
A kind of silicon nitride heating plate comprises body and is positioned at intrinsic calandria that body is fired by silicon nitride powder and formed; It is characterized in that calandria is made up of the not hot zone that is used for welding lead terminal with being positioned at calandria, hot zone; The hot zone is by titanium carbide TiC powder, ramet TaC powder, aluminium oxide Al
2O
3Powder, zirconia ZrO
2Powder, yittrium oxide Y
2O
3Powder, tungsten carbide wc powder, nickel powder, chromium Cr powder, silicon nitride Si
3N
4The powder mixed sintering forms.
The ratio of each component is of the hot zone of calandria described in the present invention: titanium carbide TiC powder 10%, ramet TaC powder 10%, aluminium oxide Al
2O
3Powder 5%, zirconia ZrO
2Powder 5%, yittrium oxide Y
2O
3Powder 5%, tungsten carbide wc powder 5%, nickel powder 5%, chromium Cr powder 3%, silicon nitride Si
3N
4Powder 42%.
The not hot zone of calandria described in the present invention is low and can effectively improve material that product fires integraty for example nickel powder, titanium carbide TiC powder, chromium Cr powder, molybdenum Mo powder and silicon nitride Si by resistivity
3N
4The powder mixed sintering forms.
Each set of dispense of the not hot zone of calandria described in the present invention is than being nickel powder 20%, titanium carbide TiC powder 10%, chromium Cr powder 20%, molybdenum Mo powder 20% and silicon nitride Si
3N
4Powder 30%.
A kind of manufacturing approach of the heating plate of silicon nitride as stated; Its steps in sequence is flouring technology, blank-making technology, sintering process, technique for grinding, welding procedure and finished product detection; It is characterized in that said blank-making technology comprises the steps: calculating body length, calandria powder thickness, and after making corresponding mould, process earlier in the calandria hot zone and the powder base of hot zone not respectively; Wherein tonnage is 2MPa, produces upper and lower two Si then
3N
4Powder base, tonnage are 10 MPa, at last above-mentioned three kinds of powder base covers are pressed into the blank piece, and pressure is 100 MPa in the casing pressure process, obtain blank.
Flouring technology is meant the raw material of taking by proportioning after ball mill, the levigate mixing of sand mill among the present invention, at argon Ar protection drying tower drying-granulating.
Sintering process is meant that the blank that blank-making technology is obtained places hot pressing concussion sintering furnace among the present invention, and making blank is 5Hz, amplitude 200Kg-500Kg, total pressure 300Kg/cm at 1850 ℃, frequency of oscillation
2Condition under, sintering makes semi-finished product.
Technique for grinding described in the present invention is meant the semi-finished product polishing processing that makes in the sintering process, obtains surface smoothness and reach 0.8 heating plate.
Welding procedure described in the present invention is meant after the lead end of heating plate after the polishing is with CVD technology sputtered with Ti ion; Use CVD technology sputter Ni ion on the Ti sheath again; Then to the lead end electroplated Ni layer; The Ni layer thickness is 0.2 μ m, at last in hydrogen furnace to the lead end welding lead, obtain finished product.
After detecting, can use again through the finished product that sintering process obtains among the present invention.
The present invention compared with prior art; Through using the conductivity ceramics powder sintering to make the intrinsic heater of heating plate; Can effectively improve the stability of product; Overcome the heater easy fracture that exists in the prior art, poor with the sintering integrated property of body, shortcomings such as the finished product rate is low, serviceability instability have stable performance, the high significant advantage of production efficiency.
Description of drawings:
Accompanying drawing 1 is a structural representation of the present invention.
Reference numeral: body 1, hot zone 2, hot zone 3 not.
Embodiment:
Below in conjunction with accompanying drawing the present invention is further described:
The present invention proposes a kind of silicon nitride heating plate; Shown in accompanying drawing, comprise body 1 and the calandria that is positioned at body 1, body 1 is fired by silicon nitride powder and is formed; It is characterized in that calandria is made up of the not hot zone 3 that is used for welding lead terminal with being positioned at calandria, hot zone 2; Hot zone 2 is by titanium carbide TiC powder, ramet TaC powder, aluminium oxide Al
2O
3Powder, zirconia ZrO
2Powder, yittrium oxide Y
2O
3Powder, tungsten carbide wc powder, nickel powder, chromium Cr powder, silicon nitride Si
3N
4The powder mixed sintering forms, the ratio of each component is of the hot zone 2 of calandria described in the present invention: titanium carbide TiC powder 10%, ramet TaC powder 10%, aluminium oxide Al
2O
3Powder 5%, zirconia ZrO
2Powder 5%, yittrium oxide Y
2O
3Powder 5%, tungsten carbide wc powder 5%, nickel powder 5%, chromium Cr powder 3%, silicon nitride Si
3N
4Powder 42%, the not hot zone 3 of calandria described in the present invention are low and can effectively improve material that product fires integraty for example nickel powder, titanium carbide TiC powder, chromium Cr powder, molybdenum Mo powder and silicon nitride Si by resistivity
3N
4The powder mixed sintering forms, and each set of dispense of the not hot zone 3 of calandria described in the present invention is than being nickel powder 20%, titanium carbide TiC powder 10%, chromium Cr powder 20%, molybdenum Mo powder 20% and silicon nitride Si
3N
4Powder 30%.
A kind of manufacturing approach of the heating plate of silicon nitride as stated, its steps in sequence are flouring technology, blank-making technology, sintering process, technique for grinding, welding procedure and finished product detection,
Wherein flouring technology comprises:
(1) manufacturing of silicon nitride powder, silicon nitride powder are granulated at Ar argon shield drying tower inner drying through ball mill mixing, after sand mill is levigate, D50 ≈ 0.3-0.5 μ,
(2) being made as by proportioning of hot zone 2 powders taken each component powder in the calandria, is specially: titanium carbide TiC powder 10%, ramet TaC powder 10%, aluminium oxide Al
2O
3Powder 5%, zirconia ZrO
2Powder 5%, yittrium oxide Y
2O
3Powder 5%, tungsten carbide wc powder 5%, nickel powder 5%, chromium Cr powder 3%, silicon nitride Si
3N
4Powder 42%, behind the mixed powder of getting powder ball milling, granulation in argon gas (Ar) protection drying tower, D50 ≈ 0.7-1 μ,
(3) in the calandria not being made as of hot zone 3 powders by proportioning take nickel powder 20%, titanium carbide TiC powder 10%, chromium Cr powder 20%, molybdenum Mo powder 20% and silicon nitride Si
3N
4Powder 30%, granulation is subsequent use after ball milling mixes powder;
Said blank-making technology comprises the steps: calculating body 1 length, calandria powder thickness; And after making corresponding mould; Process earlier in the calandria hot zone 2 and the powder base of hot zone 3 not respectively, wherein tonnage is 2MPa, produces upper and lower two Si then
3N
4Powder base, tonnage are 10 MPa, at last above-mentioned three kinds of powder base covers are pressed into the blank piece, and pressure is 100 MPa in the casing pressure process, obtain blank, and the blank piece that is obtained can not have damaged, crackle;
Said sintering process is meant that the blank that blank-making technology is obtained places hot pressing concussion sintering furnace, and blank is 5Hz, amplitude 200Kg-500Kg, total pressure 300Kg/cm at 1850 ℃, frequency of oscillation
2Condition under; Sintering makes semi-finished product, makes this half-finished technical parameter reach following standard: bending strength 7800MPa, compression strength 4000MPa; Fracture toughness 8-9MPa; In the heatproof impact test, after 2 seconds, be raised to 1300 ℃ (surface temperatures) by room temperature and do not ftracture hardness HRA91-93 200 times;
Said technique for grinding is meant the semi-finished product polishing processing that makes in the sintering process, obtains surface smoothness and reaches 0.8 heating plate,
Said welding procedure is meant after the lead end of heating plate after the polishing is with CVD technology sputtered with Ti ion; Use CVD technology sputter Ni ion on the Ti sheath again; To the lead end electroplated Ni layer, the Ni layer thickness is 0.2 μ m then, at last in hydrogen furnace to the lead end welding lead; Obtain finished product, the lead-in wire that welds through welding procedure among the present invention can bear the pulling force of 20Kg; Shake through the number of times test of switching on, gross power, leakage current, heat again through the finished product that welding procedure obtains and to use after the detection such as test.
The present invention compared with prior art; Through using the conductivity ceramics powder sintering to make the intrinsic heater of heating plate; Can effectively improve the stability of product; Overcome the heater easy fracture that exists in the prior art, poor with the sintering integrated property of body, shortcomings such as the finished product rate is low, serviceability instability have stable performance, high, the high significant advantage of power of production efficiency.
Claims (7)
1. silicon nitride heating plate; Comprise body and be positioned at intrinsic calandria; Body is fired by silicon nitride powder and is formed, and it is characterized in that calandria is made up of the not hot zone that is used for welding lead terminal with being positioned at calandria, hot zone, and the hot zone is by titanium carbide TiC powder; Ramet TaC powder, aluminium oxide Al
2O
3Powder, zirconia ZrO
2Powder, yittrium oxide Y
2O
3Powder, tungsten carbide wc powder, nickel powder, chromium Cr powder, silicon nitride Si
3N
4The powder mixed sintering forms.
2. a kind of silicon nitride heating plate according to claim 1 is characterized in that the ratio of each component is of hot zone of said calandria: titanium carbide TiC powder 10%, ramet TaC powder 10%, aluminium oxide Al
2O
3Powder 5%, zirconia ZrO
2Powder 5%, yittrium oxide Y
2O
3Powder 5%, tungsten carbide wc powder 5%, nickel powder 5%, chromium Cr powder 3%, silicon nitride Si
3N
4Powder 42%.
3. a kind of silicon nitride heating plate according to claim 1, the not hot zone that it is characterized in that said calandria is by nickel powder, titanium carbide TiC powder, chromium Cr powder, molybdenum Mo powder and silicon nitride Si
3N
4The powder mixed sintering forms.
4. a kind of silicon nitride heating plate according to claim 3 is characterized in that each set of dispense ratio of the not hot zone of said calandria is nickel powder 20%, titanium carbide TiC powder 10%, chromium Cr powder 20%, molybdenum Mo powder 20% and silicon nitride Si
3N
4Powder 30%.
5. manufacturing approach of silicon nitride heating plate according to claim 1; Its steps in sequence is flouring technology, blank-making technology, sintering process, technique for grinding, welding procedure and finished product detection; It is characterized in that said blank-making technology comprises the steps: calculating body length, calandria powder thickness, and after making corresponding mould, process earlier in the calandria hot zone and the powder base of hot zone not respectively; Wherein tonnage is 2MPa, produces upper and lower two Si then
3N
4Powder base, tonnage are 10 MPa, at last above-mentioned three kinds of powder base covers are pressed into the blank piece, and pressure is 100 MPa in the casing pressure process, obtain blank.
6. the manufacturing approach of silicon nitride heating plate according to claim 5; It is characterized in that said sintering process is meant that the blank that blank-making technology is obtained places hot pressing concussion sintering furnace, making blank is 5Hz, amplitude 200Kg-500Kg, total pressure 300Kg/cm at 1850 ℃, frequency of oscillation
2Condition under, sintering makes semi-finished product.
7. the manufacturing approach of silicon nitride heating plate according to claim 5; It is characterized in that said welding procedure is meant after the lead end of heating plate after the polishing is with CVD technology sputtered with Ti ion; Use CVD technology sputter Ni ion on the Ti sheath again, then to the lead end electroplated Ni layer, the Ni layer thickness is 0.2 μ m; At last in hydrogen furnace to the lead end welding lead, obtain finished product.
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|---|---|---|---|
| CN201210047169.3A CN102595665B (en) | 2012-02-28 | 2012-02-28 | Silicon nitride heating sheet and manufacturing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210047169.3A CN102595665B (en) | 2012-02-28 | 2012-02-28 | Silicon nitride heating sheet and manufacturing method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN102595665A true CN102595665A (en) | 2012-07-18 |
| CN102595665B CN102595665B (en) | 2014-07-09 |
Family
ID=46483731
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|---|---|---|---|
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Cited By (8)
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| CN104030691A (en) * | 2013-09-09 | 2014-09-10 | 昆山申嘉特种陶瓷有限公司 | Method for preparing air pressure sintering structural member ceramic by taking silicon nitride as raw material |
| CN104860681A (en) * | 2014-02-26 | 2015-08-26 | 东莞市国研电热材料有限公司 | Cofired ceramic heating member and preparation technology thereof |
| CN104860683A (en) * | 2014-02-26 | 2015-08-26 | 东莞市国研电热材料有限公司 | All-in-one ceramic heating member and preparation technology thereof |
| CN104897460A (en) * | 2015-05-19 | 2015-09-09 | 吉林大学 | A test-piece clamp for multi-load coupling loading and a multi-physics field coupling loading method thereof |
| CN106376107A (en) * | 2016-11-24 | 2017-02-01 | 常德科锐新材料科技有限公司 | Large-power silicon nitride ceramic heating plate and inner-soft outer-hard manufacturing method thereof |
| CN107046739A (en) * | 2016-11-24 | 2017-08-15 | 常德科锐新材料科技有限公司 | High-power silicon nitride ceramics heating plate and its interior hard outer soft preparation method |
| CN109951903A (en) * | 2019-03-26 | 2019-06-28 | 深圳市聚威新材科技有限公司 | A kind of nano microcrystalline lattice mutually separate thermo electric material and preparation method thereof |
| WO2021018263A1 (en) * | 2019-07-31 | 2021-02-04 | 湖北中烟工业有限责任公司 | Multi-subgroup element-based ceramic heating body and preparation method and application thereof |
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| CN107046739A (en) * | 2016-11-24 | 2017-08-15 | 常德科锐新材料科技有限公司 | High-power silicon nitride ceramics heating plate and its interior hard outer soft preparation method |
| CN107046739B (en) * | 2016-11-24 | 2019-10-29 | 常德科锐新材料科技有限公司 | High-power silicon nitride ceramics heating sheet and its interior hard outer soft production method |
| CN106376107B (en) * | 2016-11-24 | 2020-03-20 | 常德科锐新材料科技有限公司 | High-power silicon nitride ceramic heating plate and manufacturing method of high-power silicon nitride ceramic heating plate with soft inside and hard outside |
| CN109951903A (en) * | 2019-03-26 | 2019-06-28 | 深圳市聚威新材科技有限公司 | A kind of nano microcrystalline lattice mutually separate thermo electric material and preparation method thereof |
| CN109951903B (en) * | 2019-03-26 | 2021-06-04 | 深圳市聚威新材科技有限公司 | Nano microcrystalline lattice phase separation electrothermal material and preparation method thereof |
| WO2021018263A1 (en) * | 2019-07-31 | 2021-02-04 | 湖北中烟工业有限责任公司 | Multi-subgroup element-based ceramic heating body and preparation method and application thereof |
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