CN101765253B - Method for preparing SiC heating element having long service life - Google Patents
Method for preparing SiC heating element having long service life Download PDFInfo
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- CN101765253B CN101765253B CN2010101042130A CN201010104213A CN101765253B CN 101765253 B CN101765253 B CN 101765253B CN 2010101042130 A CN2010101042130 A CN 2010101042130A CN 201010104213 A CN201010104213 A CN 201010104213A CN 101765253 B CN101765253 B CN 101765253B
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Abstract
The invention discloses a method for preparing a SiC (silicon carbide) heating element having long service life. The method comprises the following steps: proportioning the following components by mass percentage: 75% to 90% of SiC, 1% to 5% of Al2O3, 1% to 5% of ZrO2, 1% to 3% SiO2, 4% to 10% of Si and 1% to 5% of C; preparing the components into a hollow pipe by using the extrusion molding process; drying at 80 to 300 DEG C; sintering at 1,450 to 1,650 DEG C in the presence of protective nitrogen, cutting into a heating part, and testing the resistance of the heating part for later use; proportioning the following components by mass percentage: 70% to 90% of SiC, 1% to 5% of Ni, 1% to 5% of Mo, 1% to 5% of Ti, 1% to 5% of TiC, 5% to 10% of Si and 1% to 5% of C; sintering the components by using the same process of forming and sintering as the heating part, cutting into a cold-side part, testing the resistance of the cold-side part for later use; and welding the cold-side parts at two ends of the heating part at the local-welding temperature of 1,500 to 1,600 DEG C, to complete the preparation of the entire heating element.
Description
Technical field
The present invention relates to a kind of preparation method of heater element, particularly a kind of preparation method of SiC heater element.
Background technology
SiC (carborundum) heater element is claimed Elema again, forms (Fig. 1) by heat generating part and cold end two parts usually.Heat generating part generally forms through SiC recrystallization sintering, and sintering temperature is usually about 2200 ℃.The porosity reaches 15～20%, and intensity is 75～100Mpa; Resistivity is bigger, is generally 15～20 times of cold end.The cold end material is at present main to be adopted reaction-sintered to ooze Si to handle, and the porosity is less than 1%, fine and close, intensity is little up to 250MPa, resistivity.The best serviceability temperature of Elema is generally at 800 ℃～1350 ℃, heat generating part at high temperature, the SiC surface produces oxidation reaction: 2SiC+3O with oxygen
2→ 2SiO
2+ 2CO ↑, SiO
2Generate diaphragm at the SiC particle surface, the further oxidation of protection SiC has realized the ceramic high-temperature oxidation resistance of SiC.But when using for a long time, on the one hand, because heat generating part contains 15～20% the porosity, oxygen can be in the free flow of SiC material internal; On the other hand, SiO
2Though generation the SiC particle is had the certain protection effect, local electrical resistance is raise, cause this place local temperature to raise, make the selective oxidation aggravation again, cause the excellent limited service life of SiC.
The high porosity (about 20%) that changes heat generating part is 0% fine and close SiC, and oxidized area is reduced greatly, thereby improves the life-span.How to obtain low-cost fine and close SiC: the technology that the simplest at present industrial method employing reaction-sintered oozes Si.Subject matter be gained reaction-sintered SiC (Si) though densification (0% porosity), resistivity is little, should not be used for heat generating part.
Summary of the invention
The present invention is directed to short problem of traditional silicon carbon-point life-span, a kind of preparation method of SiC heating element having long service life is provided.
For reaching above purpose, the present invention takes following technical scheme to be achieved:
A kind of preparation method of SiC heating element having long service life is characterized in that, comprises the steps:
(1) preparation of heat generating part: following component is prepared burden by mass percentage: SiC, 75～90%; Al
2O
3, 1～5%; ZrO
2, 1～5%; SiO
2, 1～3%; Si, 4～10%; C, 1～5%; Adopt extrusion forming process to process hollow pipe; 80～300 ℃ of oven dry; Nitrogen protection, 1550～1650 ℃ are burnt till, subsequent use after cutting, the check resistance value;
(2) preparation of cold end: following component is prepared burden by mass percentage: SiC, 70～90%, Ni, 1～5%; Mo, 1～5%; Ti, 1～5%; TiC, 1～5%; Si, 5～10%; C, 1～5%; Adopt moulding and the sintering process identical to burn till with step (1), subsequent use after cutting, the check resistance value;
(3) welding: cold end is gone up in the two ends welding of heat generating part, accomplishes the preparation of whole heater element, and wherein the resistance ratio of heat generating part and cold end is chosen in 15～20, and welding temperature is 1500～1600 ℃.
In the said method, the resistance ratio of heat generating part and cold end preferably is chosen in 20.The temperature of said check resistance value is 1100 ℃.
Compared with prior art, the present invention adopts and adds oxide ceramics additive (ZrO in fine and close SiC (Si) material
2, SiO
2, Al
2O
3) improve the resistivity of this material, as the heat generating part of Elema, this heat generating part material is because the porosity is near zero.Air can't pass through at material internal.Have only the surface can oxidation, the oxidation area be very little, and local electrical resistance changes very little after the oxidation.Thereby can significantly improve the useful life of Elema.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed description.
Fig. 1 is the structure chart of SiC heater element.Among the figure: 1, heat generating part; 2, cold end.
Fig. 2 is a process chart of the present invention.
Embodiment
Referring to Fig. 2 SiC heater element of the present invention preparation technology flow chart, heat generating part 1 and cold end 2 all relate to wherein batching, mixing, moulding, dry, burn till and check 1 operation.The specific embodiment of heat generating part is as shown in table 1.The specific embodiment of cold end is as shown in table 2.
The prescription of table 1 heat generating part is formed and technological parameter
The prescription of table 2 cold end is formed and technological parameter
In operation shown in Figure 2, checking 1 operation is that detected temperatures is 1100 ℃ to the hot detection of the resistance value (resistivity) of the heat generating part 1 that sinters or cold end 2.
Welding sequence is to be welded as integral body to the heat generating part 1 through check 1 operation with cold end 2, and the local welding temperature of weld is 1500～1600 ℃.The resistance ratio of heat generating part and cold end is chosen in 15～20, preferably is chosen in 20.Checking 2 operations is that the resistance of the whole heater element after welding is finished is measured.
The heat generating part that the present invention forms code name for heat 1 and code name are that cold 4 cold end formed are welded and processed Elema A; The heat generating part that code name is formed for heat 2 and code name are that cold 3 cold end formed are welded and processed Elema B; The heat generating part that code name is formed for heat 3 and code name are that cold 2 cold end formed are welded and processed Elema C; The heat generating part that code name is formed for heat 4 and code name are that cold 1 cold end formed is welded and processed Elema D; Its performance is listed in table 3
The Elema performance of table 3 the present invention preparation
| Code name | Elema A | Elema B | Elema C | Elema D |
| Applicable temperature (℃) | 800～1200 | 900～1300 | 900～1350 | 900～1350 |
| The hot junction porosity (%) | 1 | 0.65 | 0.32 | 0.06 |
| Useful life (moon) | ＞12 | ＞18 | ＞18 | ＞18 |
Existing Elema heat generating part lost efficacy or the reason damaged is: the best serviceability temperature of Elema is generally at 800 ℃～1350 ℃, heat generating part at high temperature, the SiC surface produces oxidation reaction, the SiO of generation with oxygen
2Form diaphragm at the SiC particle surface,, local electrical resistance is raise though can protect the further oxidation of SiC; Cause this place's local temperature to raise; Because the recrystallization SiC porosity that uses at present is high, inside and outside being prone to of oxygen flowed and passes through, and causes Elema selective oxidation aggravation in addition; Oxide film breakdown, overheated and fracture and aging.
Innovative point of the present invention is:
1, the high porosity (about 20%) that at first changes heat generating part reduces oxidized area greatly, thereby improves the life-span near 0% fine and close SiC.
2, through respectively heat generating part and cold end material being added the composition of suitable increase resistance, like ZrO
2, Al
2O
3, SiO
2Deng and reduce the component of resistance, like Ni, Mo, Ti, TiC etc. significantly increase heat generating part resistance, cold end resistance significantly reduces, thereby satisfies the specification requirement of the two resistance ratio 15～20.
Claims (1)
1. the preparation method of a SiC heating element having long service life is characterized in that, comprises the steps:
(1) preparation of heat generating part: following component is prepared burden by mass percentage: SiC, 75～90%; Al
2O
3, 1～5%; ZrO
2, 1～5%; SiO
2, 1～3%; Si, 4～10%; C, 1～5%; Adopt extrusion forming process to process hollow pipe; 80～300 ℃ of oven dry; Nitrogen protection, 1550～1650 ℃ are burnt till, subsequent use after cutting, the check resistance value;
(2) preparation of cold end: following component is prepared burden by mass percentage: SiC, 70～90%, Ni, 1～5%; Mo, 1～5%; Ti, 1～5%; TiC, 1～5%; Si, 5～10%; C, 1～5%; Adopt moulding and the sintering process identical to burn till with step (1), subsequent use after cutting, the check resistance value;
(3) welding: cold end is gone up in the two ends welding of heat generating part, accomplishes the preparation of whole heater element, and wherein the resistance ratio of heat generating part and cold end is chosen in 15～20, and welding temperature is 1500～1600 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101042130A CN101765253B (en) | 2010-02-02 | 2010-02-02 | Method for preparing SiC heating element having long service life |
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|---|---|---|---|
| CN2010101042130A CN101765253B (en) | 2010-02-02 | 2010-02-02 | Method for preparing SiC heating element having long service life |
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| CN101765253A CN101765253A (en) | 2010-06-30 |
| CN101765253B true CN101765253B (en) | 2012-01-04 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173812B (en) * | 2011-01-29 | 2013-10-30 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of molybdenum silicide type heating component |
| CN103152847A (en) * | 2013-02-28 | 2013-06-12 | 包头稀土研究院 | Method for manufacturing lanthanum chromite electric heating element in welding manner |
| CN105934005A (en) * | 2016-05-06 | 2016-09-07 | 武汉航空仪表有限责任公司 | Novel heater of icing detector |
| KR102137032B1 (en) | 2017-05-10 | 2020-07-23 | 엘지전자 주식회사 | A composition for carbon composite and a carbon heater manufactured by using the same |
| KR102004035B1 (en) * | 2017-05-26 | 2019-07-25 | 엘지전자 주식회사 | A carbon heating element |
| KR102079363B1 (en) * | 2017-05-26 | 2020-02-19 | 엘지전자 주식회사 | A manufacturing method for carbon heater |
| CN109288140B (en) * | 2018-12-06 | 2021-08-27 | 广东国研新材料有限公司 | Porous ceramic heating element for electronic cigarette and preparation method thereof |
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