CN102595665B - Silicon nitride heating sheet and manufacturing method thereof - Google Patents
Silicon nitride heating sheet and manufacturing method thereof Download PDFInfo
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- CN102595665B CN102595665B CN201210047169.3A CN201210047169A CN102595665B CN 102595665 B CN102595665 B CN 102595665B CN 201210047169 A CN201210047169 A CN 201210047169A CN 102595665 B CN102595665 B CN 102595665B
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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 sheet and manufacture method thereof.
Background technology
As everyone knows, silicon nitride ceramic material has good thermal stability, can on very little area, produce powerful heating element, and silicon nitride heating sheet is that a kind of application prospect is extensive, the product of good energy-conserving effect.The general employing of silicon nitride heating sheet directly adds the tungsten filament for generating heat in beta-silicon nitride powder at present, then forms through firing.Because tungsten filament and beta-silicon nitride powder have obvious interface, after sintering, be difficult to become one, easily short splitting of tungsten filament in the production process of product, or in sintering process, resistance value changes, and 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 heat-generation body and preparation method thereof, and its pyrotoxin is made up as copper, tungsten, nickel etc. of various metals powder, to obtaining the integraty after sintering.But in fact, because its pyrotoxin adopting is still metallics, made heater and the still Presence of an interface of silicon nitride of metal-powder after sintering, still there is the defects such as finished product rate variance, power are low, unstable properties in product, the pyrotoxin that adopts in addition metal material to make, heating effect is undesirable, can not meet the demand of high-power heating plate.
Summary of the invention
The present invention is directed to the shortcoming and defect existing in prior art, propose a kind of add thermally-stabilised, the life-span long, not fragile and be specially adapted to silicon nitride heating sheet and the manufacture method thereof that high-power heating plate is made.
The present invention can reach by following measures:
A kind of silicon nitride heating sheet, comprises body and is positioned at intrinsic calandria, body is fired and formed by silicon nitride powder, it is characterized in that calandria is made up of hot zone and the not hot zone for welding lead that is positioned at calandria end, 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
4powder 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 product and fire material for example nickel powder, titanium carbide TiC powder, chromium Cr powder, molybdenum Mo powder and the silicon nitride Si of integraty by resistivity
3n
4powder mixed sintering forms.
Each component proportion of the not hot zone of calandria described in the present invention is 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 manufacture method of silicon nitride heating sheet described above, its step is followed successively by flouring technology, blank-making technology, sintering process, technique for grinding, welding procedure and finished product detection, it is characterized in that described blank-making technology comprises the steps: calculating body length, calandria powder thickness, and make after corresponding mould, first make respectively the powder base of He Bu hot zone in hot zone in calandria, wherein tonnage is 2MPa, then produces upper and lower two Si
3n
4powder base, tonnage is 10 MPa, finally above-mentioned three kinds of powder base covers is pressed into blank piece, in casing pressure process, pressure is 100 MPa, obtains blank.
In the present invention, flouring technology refers to the raw material of taking by proportioning after ball mill, sand mill is levigate mixing, at argon Ar protection drying tower drying-granulating.
In the present invention, sintering process refers to that the blank that blank-making technology is obtained is placed in hot pressing concussion sintering furnace, 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 refers to the semi-finished product polishing processing making in sintering process, obtains surface smoothness and reach 0.8 heating plate.
Welding procedure described in the present invention refers to after the lead end CVD technique sputtered with Ti ion of heating plate after polishing, use again CVD technique sputter Ni ion on Ti sheath, then to lead end electroplated Ni layer, Ni layer thickness is 0.2 μ m, finally in hydrogen furnace to lead end welding lead, obtain finished product.
The finished product obtaining through sintering process in the present invention can use after after testing again.
The present invention compared with prior art, by using 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 prior art, poor with the sintering integrated property of body, the shortcomings such as finished product rate is low, serviceability is unstable, have stable performance, the high significant advantage of production efficiency.
accompanying drawing explanation:
Accompanying drawing 1 is 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 illustrated:
The present invention proposes a kind of silicon nitride heating sheet, as shown in drawings, comprise body 1 and the calandria that is positioned at body 1, body 1 is fired and is formed by silicon nitride powder, it is characterized in that calandria is made up of hot zone 2 and the not hot zone 3 for welding lead that is positioned at calandria end, 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
4powder 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 is low and can effectively improve product and fire material for example nickel powder, titanium carbide TiC powder, chromium Cr powder, molybdenum Mo powder and the silicon nitride Si of integraty by resistivity
3n
4powder mixed sintering forms, and each component proportion of the not hot zone 3 of calandria described in the present invention is nickel powder 20%, titanium carbide TiC powder 10%, chromium Cr powder 20%, molybdenum Mo powder 20% and silicon nitride Si
3n
4powder 30%.
A manufacture method for silicon nitride heating sheet described above, its step is followed successively by flouring technology, blank-making technology, sintering process, technique for grinding, welding procedure and finished product detection,
Wherein flouring technology comprises:
(1) manufacture of silicon nitride powder, silicon nitride powder, through ball mill mixing, after sand mill is levigate, is granulated at Ar argon shield drying tower inner drying, D50 ≈ 0.3-0.5 μ,
(2) in calandria, being made as by proportioning of hot zone 2 powders taken each component powder, 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%, by after mixed got powder ball milling powder, granulation in argon gas (Ar) protection drying tower, D50 ≈ 0.7-1 μ,
(3) in calandria, being made as by proportioning of hot zone 3 powders do not taken nickel powder 20%, titanium carbide TiC powder 10%, chromium Cr powder 20%, molybdenum Mo powder 20% and silicon nitride Si
3n
4powder 30%, after the mixed powder of ball milling, granulation is for subsequent use;
Described blank-making technology comprises the steps: calculating body 1 length, calandria powder thickness, and make after corresponding mould, first make respectively in calandria hot zone 2 and the powder base of hot zone 3 not, wherein tonnage is 2MPa, then produces upper and lower two Si
3n
4powder base, tonnage is 10 MPa, finally above-mentioned three kinds of powder base covers is pressed into blank piece, and in casing pressure process, pressure is 100 MPa, obtains blank, and the blank piece obtaining can not have damaged, crackle;
Described sintering process refers to that the blank that blank-making technology is obtained is placed in 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, make this half-finished technical parameter reach following standard: bending strength 7800MPa, compression strength 4000MPa, fracture toughness 8-9MPa, in heatproof impact test, after 2 seconds, be raised to 1300 ℃ (surface temperatures) by room temperature and do not ftracture for 200 times, hardness HRA91-93;
Described technique for grinding refers to the semi-finished product polishing processing making in sintering process, obtains surface smoothness and reaches 0.8 heating plate,
Described welding procedure refers to after the lead end CVD technique sputtered with Ti ion of heating plate after polishing, use again CVD technique sputter Ni ion on Ti sheath, then to lead end electroplated Ni layer, Ni layer thickness is 0.2 μ m, finally in hydrogen furnace to lead end welding lead, obtain finished product, in the present invention, can bear the pulling force of 20Kg through the lead-in wire of welding procedure welding; The finished product obtaining through welding procedure can use after the test of energising number of times, gross power, leakage current, heat are shaken the detections such as test again.
The present invention compared with prior art, by using 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 prior art, poor with the sintering integrated property of body, the shortcomings such as finished product rate is low, serviceability is unstable, have that stable performance, production efficiency are high, the high significant advantage of power.
Claims (6)
1. a silicon nitride heating sheet, comprise body and be positioned at intrinsic calandria, body is fired and is formed by silicon nitride powder, it is characterized in that calandria is made up of hot zone and the not hot zone for welding lead that is positioned at calandria end, 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
4powder mixed sintering forms.
2. a kind of silicon nitride heating sheet according to claim 1, is characterized in that the not hot zone of described calandria is by nickel powder, titanium carbide TiC powder, chromium Cr powder, molybdenum Mo powder and silicon nitride Si
3n
4powder mixed sintering forms.
3. a kind of silicon nitride heating sheet according to claim 2, the each component proportion that it is characterized in that the not hot zone of described 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%.
4. the manufacture method of silicon nitride heating sheet as claimed in claim 1, its step is followed successively by flouring technology, blank-making technology, sintering process, technique for grinding, welding procedure and finished product detection, it is characterized in that described blank-making technology comprises the steps: calculating body length, calandria powder thickness, and make after corresponding mould, first make respectively the powder base of He Bu hot zone in hot zone in calandria, wherein tonnage is 2MPa, then produces upper and lower two Si
3n
4powder base, tonnage is 10 MPa, finally above-mentioned three kinds of powder base covers is pressed into blank piece, in casing pressure process, pressure is 100 MPa, obtains blank.
5. the manufacture method of silicon nitride heating sheet according to claim 4, it is characterized in that described sintering process refers to that the blank that blank-making technology is obtained is placed in 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.
6. the manufacture method of silicon nitride heating sheet according to claim 4, it is characterized in that described welding procedure refers to after the lead end CVD technique sputtered with Ti ion of heating plate after polishing, use again CVD technique sputter Ni ion on Ti sheath, then to lead end electroplated Ni layer, Ni layer thickness is 0.2 μ m, finally in hydrogen furnace to 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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|---|---|---|---|---|
| CN104030691B (en) * | 2013-09-09 | 2016-03-23 | 昆山申嘉特种陶瓷有限公司 | A kind of take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material |
| CN104897460B (en) * | 2015-05-19 | 2018-06-01 | 吉林大学 | The piece fixture of multi-load coupling loading and its multiple physical field coupling loading 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 |
| 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 |
| CN112321330B (en) * | 2019-07-31 | 2022-06-07 | 湖北中烟工业有限责任公司 | Ceramic heating element based on multiple subgroup elements and preparation method and application thereof |
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2012
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| US4912305A (en) * | 1988-06-09 | 1990-03-27 | Ngk Spark Plug Co., Ltd. | Silicon nitride base ceramic heater element and method of producing same |
| JPH04187566A (en) * | 1990-11-19 | 1992-07-06 | Riken Corp | Sintered silicon nitride and its production |
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Denomination of invention: Silicon nitride heating element and its manufacturing method Effective date of registration: 20230524 Granted publication date: 20140709 Pledgee: Weihai Commercial Bank Co.,Ltd. Xicheng Branch Pledgor: Weihai Xingtai Precision Technology Co.,Ltd. Registration number: Y2023980041525 |