CN104108937A - Zirconium carbide ceramic heating unit and preparation method thereof - Google Patents
Zirconium carbide ceramic heating unit and preparation method thereof Download PDFInfo
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- CN104108937A CN104108937A CN201410333354.8A CN201410333354A CN104108937A CN 104108937 A CN104108937 A CN 104108937A CN 201410333354 A CN201410333354 A CN 201410333354A CN 104108937 A CN104108937 A CN 104108937A
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- zirconium carbide
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Abstract
The invention relates to a zirconium carbide ceramic heating unit and a preparation method thereof. The heating unit material is composed of 50-99.5% of zirconium carbide and the balance of additive composed of graphite, ZrB2, ZrO2, Zr, SiC, Mo or MoSi2. The preparation method comprises the following steps: (1) taking zirconium carbide powder and proper amounts of additive and solvent, and carrying out ball milling in a ball mill; (2) drying the mixture subjected to ball milling in a rotary evaporator, and passing through a 50-200-mesh screen; and (3) sintering the screened mixed powder in a vacuum or inert atmosphere, and machining to obtain the heating unit with required size and shape. The heating unit has the advantges of high mechanical strength, low deformation tendency and volatility at high temperature, and stable electric properties. In a vacuum or protective atmosphere, the heating unit can provide a high-temperature environment of 3000 DEG C to the maximum.
Description
Technical field
The present invention relates to electric heating material technical field, be specifically related to the preparation method of a kind of zirconium carbide ceramics heating element and heating element.
Background technology
At present, can produce 3000 DEG C of high temperature and the heating element that is applied is mainly graphite matter heating element.Be characterized in thering is good conduction and heat conductivility, and cheap.Shortcoming is at high temperature yielding, and thermal stresses is poor, and in order to prevent distortion, the normal methods such as becoming large heating element size that adopts solves, and this certainly will cause body of heater volume to become large, and energy consumption increases.Another shortcoming of graphite heater is that the vapour pressure under hot conditions (is 1.8 × 10 greatly in the time of 2227 DEG C
-7pa), as carbon when the high temperature of 2227 DEG C will be with 1.16 × 10
-2the speed evaporation of g/cm3h.Therefore, graphite heater not only can run into because carbon component evaporates the graphite heater endurance issues of drawing in the time that long-time continuous is used, and, if heating element causes the consumption of carbon because of evaporation, its resistance value is inevitable correspondingly to be increased, and this will further encourage the evaporation of carbon.Although have been reported demonstration, suppress the evaporation of above-mentioned carbon by adding carbon fiber, difficulty fundamentally solves evaporation problems.
Summary of the invention
The object of the invention is the deficiency for solving the problems of the technologies described above; the preparation method of a kind of zirconium carbide ceramics heating element and heating element is provided; this heating element mechanical strength is high; at high temperature not yielding and difficult volatilization; stable electrical properties; under vacuum or protective atmosphere, can provide the hot environment that is up to 3000 DEG C.
The present invention is for solving the problems of the technologies described above, and the technical scheme providing is: a kind of zirconium carbide ceramics heating material, made by the raw material of following weight per-cent: zirconium carbide 50～99.5% and additive 0.5～50%.
Described additive is graphite, ZrB
2, ZrO
2, Zr, SiC, Mo or MoSi
2in one or arbitrary composition.
A preparation method for zirconium carbide ceramics heating element, comprises the following steps:
(1) get, by weight percentage zirconium carbide powder 50～99.5% and additive 0.5～50%, insert in ball mill and carry out ball milling, ball mill travelling speed is 150～250 revs/min, and Ball-milling Time is 20～40 hours;
(2) compound, by step (1) after ball milling is dried in rotatory evaporator, and controlling bath temperature is 65～85 DEG C, and revolving bottle rotating speed is 20～70 revs/min, and drying time is 2～5 hours, after oven dry, is crossing 50～200 mesh sieves;
(3) powder mix, after step (2) is sieved carries out sintering in vacuum or inert atmosphere, after sintering completes, is machined into desired size, is shaped as straight shape heating element or U-shaped heating element.
Described additive is graphite, ZrB
2, ZrO
2, Zr, SiC, Mo or MoSi
2in one or arbitrary composition.
The particle diameter of zirconium carbide powder is 0.1～2 μ m, and the particle diameter of additive powder is 0.1～30 μ m.
In described step (3), the concrete grammar of sintering is: powder mix is packed in mould, carry out hot pressed sintering in vacuum or inert atmosphere, temperature is 1900～2600 DEG C, and pressure is 15～50MPa.
The concrete grammar of sintering is in described step (3): powder mix and bonding agent and solvent are mixed, then through oven dry, granulation, cold isostatic compaction, pressure is 200～300 MPa, then in vacuum or inert atmosphere, carries out pressureless sintering, and temperature is 2200～2800 DEG C.
Described solvent is ethanol, acetone or toluene etc., and bonding agent is resol, polyvinyl alcohol, methylcellulose gum, starch or dextrin, and the add-on of bonding agent is 2～5% of powder mix weight.
beneficial effect
Heating element mechanical strength of the present invention is high, at high temperature not yielding and difficult volatilization, and stable electrical properties, under vacuum or protective atmosphere, can provide the hot environment that is up to 3000 DEG C.
Brief description of the drawings
Fig. 1 is the structural representation of the straight shape heating element that makes of the present invention;
Fig. 2 is the structural representation of the U-shaped heating element that makes of the present invention;
In figure: 1, cold junction, 2, hot junction.
Embodiment
embodiment 1
A preparation method for zirconium carbide ceramics heating element, comprises the following steps:
(1) get, by weight percentage zirconium carbide (particle diameter be 0.1～2 μ m) 90%, (particle diameter is 0.1～30 μ m) 10% to Graphite Powder 99, inserts in ball mill and carries out ball milling, and ball mill travelling speed is 150 revs/min, and Ball-milling Time is 40 hours;
(2) compound, by step (1) after ball milling is dried in rotatory evaporator, and controlling bath temperature is 65 DEG C, and revolving bottle rotating speed is 70 revs/min, and drying time is 5 hours, after oven dry, is crossing 50 mesh sieves;
(3) powder mix, after step (2) is sieved packs in mould, carries out hot pressed sintering in vacuum or inert atmosphere, and temperature is 2100 DEG C, and pressure is 40MPa, after sintering completes, is machined into the heating element of desired size, shape.
As shown in Figure 1, can be processed into straight shape heating element (comprising cold junction 1 and hot junction 2), as shown in Figure 2, also can be processed into U-shaped heating element (comprising cold junction 1 and hot junction 2).
embodiment 2
A preparation method for zirconium carbide ceramics heating element, comprises the following steps:
(1) get, by weight percentage zirconium carbide (particle diameter be 0.1～2 μ m) 85%, (particle diameter is 0.1～30 μ m) 15% to Graphite Powder 99, inserts in ball mill and carries out ball milling, and ball mill travelling speed is 150 revs/min, and Ball-milling Time is 40 hours;
(2) compound, by step (1) after ball milling is dried in rotatory evaporator, and controlling bath temperature is 65 DEG C, and revolving bottle rotating speed is 70 revs/min, and drying time is 5 hours, after oven dry, is crossing 50 mesh sieves;
(3) powder mix, after step (2) is sieved packs in mould, carries out hot pressed sintering in vacuum or inert atmosphere, and temperature is 2200 DEG C, and pressure is 30MPa, after sintering completes, is machined into the heating element of desired size, shape.
embodiment 3
A preparation method for zirconium carbide ceramics heating element, comprises the following steps:
(1), get by weight percentage zirconium carbide (particle diameter be 0.1～2 μ m) 75%, Graphite Powder 99 (particle diameter be 0.1～30 μ m) 5%, Zr powder (particle diameter be 0.1～30 μ m) 10% and Mo powder (particle diameter is 0.1～30 μ m) 1% and MoSi
2(particle diameter is 0.1～30 μ m) 9% to powder, inserts in ball mill and carries out ball milling, and ball mill travelling speed is 250 revs/min, and Ball-milling Time is 20 hours;
(2) compound, by step (1) after ball milling is dried in rotatory evaporator, and controlling bath temperature is 80 DEG C, and revolving bottle rotating speed is 50 revs/min, and drying time is 4 hours, after oven dry, is crossing 200 mesh sieves;
(3), powder mix and the polyvinyl alcohol after step (2) is sieved mixes, then through drying, granulation, cold isostatic compaction, pressure is 300 MPa, then in vacuum or inert atmosphere, carries out pressureless sintering, and temperature is 2400 DEG C, after sintering completes, be machined into the heating element of desired size, shape.
embodiment 4
A preparation method for zirconium carbide ceramics heating element, comprises the following steps:
(1), get by weight percentage zirconium carbide (particle diameter be 0.1～2 μ m) 75%, Graphite Powder 99 (particle diameter be 0.1～30 μ m) 15%, Zr powder (particle diameter be 0.1～30 μ m) 2% and Mo powder (particle diameter be 0.1～30 μ m) 2%, ZrO
2powder (particle diameter be 0.1～30 μ m) 2%, (particle diameter is 0.1～30 μ m) 2% and MoSi to SiC powder
2(particle diameter is 0.1～30 μ m) 2% to powder, inserts in ball mill and carries out ball milling, and ball mill travelling speed is 250 revs/min, and Ball-milling Time is 20 hours;
(2) compound, by step (1) after ball milling is dried in rotatory evaporator, and controlling bath temperature is 80 DEG C, and revolving bottle rotating speed is 50 revs/min, and drying time is 4 hours, after oven dry, is crossing 200 mesh sieves;
(3), the powder mix after step (2) is sieved and resol and ethanol mix, then through drying, granulation, cold isostatic compaction, pressure is 300 MPa, then in vacuum or inert atmosphere, carries out pressureless sintering, and temperature is 2400 DEG C, after sintering completes, be machined into the heating element of desired size, shape.
performance test
Claims (8)
1. a zirconium carbide ceramics heating element, is characterized in that: the raw material by following weight per-cent is made: zirconium carbide 50～99.5% and additive 0.5～50%.
2. a kind of zirconium carbide ceramics heating element as claimed in claim 1, is characterized in that: described additive is graphite, ZrB
2, ZrO
2, Zr, SiC, Mo or MoSi
2in one or arbitrary composition.
3. a preparation method for zirconium carbide ceramics heating element, is characterized in that: comprise the following steps:
(1) get, by weight percentage zirconium carbide powder 50～99% and additive powder 0.5～50%, insert in ball mill and carry out ball milling, ball mill travelling speed is 150～250 revs/min, and Ball-milling Time is 20～40 hours;
(2) compound, by step (1) after ball milling is dried in rotatory evaporator, and controlling bath temperature is 65～85 DEG C, and revolving bottle rotating speed is 20～70 revs/min, and drying time is 2～5 hours, after oven dry, is crossing 50～200 mesh sieves;
, powder mix after step (2) is sieved carries out sintering in vacuum or inert atmosphere, after sintering completes, is machined into the heating element of desired size, shape.
4. as the preparation method of a claim 3 zirconium carbide ceramics heating element, it is characterized in that: described additive is graphite, ZrB
2, ZrO
2, Zr, SiC, Mo or MoSi
2in one or arbitrary composition, the particle diameter of zirconium carbide powder is 0.1～2 μ m, the particle diameter of additive powder is 0.1～30 μ m.
5. as the preparation method of a claim 3 zirconium carbide ceramics heating element, it is characterized in that: the heating element making is straight shape heating element or U-shaped heating element.
6. as the preparation method of a claim 3 zirconium carbide ceramics heating element, it is characterized in that: in described step (3), the concrete grammar of sintering is: powder mix is packed in mould, in vacuum or inert atmosphere, carry out hot pressed sintering, temperature is 1900～2600 DEG C, and pressure is 15～50MPa.
7. as the preparation method of a claim 3 zirconium carbide ceramics heating element, it is characterized in that: the concrete grammar of sintering is in described step (3): powder mix and bonding agent and solvent are mixed, then through drying, granulation, cold isostatic compaction, pressure is 200～300 MPa, then in vacuum or inert atmosphere, carries out pressureless sintering, and temperature is 2200～2800 DEG C.
8. as the preparation method of a claim 7 zirconium carbide ceramics heating element, it is characterized in that: described solvent is ethanol, acetone or toluene, bonding agent is resol, polyvinyl alcohol, methylcellulose gum, starch or dextrin, and the add-on of bonding agent is 2～5% of powder mix weight.
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| CN201410333354.8A CN104108937A (en) | 2014-07-14 | 2014-07-14 | Zirconium carbide ceramic heating unit and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104829227A (en) * | 2015-04-24 | 2015-08-12 | 河南科技大学 | Zirconia-zirconium boride double-layer composite ceramic heating element and preparation method thereof |
| CN106495697A (en) * | 2016-10-21 | 2017-03-15 | 过冬 | A kind of zirconium carbide ceramics heater and the preparation method of heater |
| CN109185372A (en) * | 2018-10-29 | 2019-01-11 | 海宁易达自动化设备有限公司 | Hydraulic brake liner and preparation method thereof |
| WO2019119612A1 (en) * | 2017-12-21 | 2019-06-27 | 深圳市卓力能电子有限公司 | Preparation process for novel porous ceramic heating body |
| CN110330340A (en) * | 2019-07-18 | 2019-10-15 | 平顶山市信瑞达石墨制造有限公司 | A kind of ceramics-graphite composite material cooker and its preparation process |
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| JPS62102501A (en) * | 1985-10-30 | 1987-05-13 | ティーディーケイ株式会社 | Resistance heating element |
| CN1453799A (en) * | 2003-06-03 | 2003-11-05 | 段曦东 | Composite conducting ceramic and its prepn |
| CN102503427A (en) * | 2011-11-10 | 2012-06-20 | 哈尔滨工业大学 | Preparation method of high-toughness boride-carbide composite ceramic |
-
2014
- 2014-07-14 CN CN201410333354.8A patent/CN104108937A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62102501A (en) * | 1985-10-30 | 1987-05-13 | ティーディーケイ株式会社 | Resistance heating element |
| CN1453799A (en) * | 2003-06-03 | 2003-11-05 | 段曦东 | Composite conducting ceramic and its prepn |
| CN102503427A (en) * | 2011-11-10 | 2012-06-20 | 哈尔滨工业大学 | Preparation method of high-toughness boride-carbide composite ceramic |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104829227A (en) * | 2015-04-24 | 2015-08-12 | 河南科技大学 | Zirconia-zirconium boride double-layer composite ceramic heating element and preparation method thereof |
| CN104829227B (en) * | 2015-04-24 | 2017-03-01 | 河南科技大学 | A kind of zirconium oxide zirconium boride two-layer compound ceramic heating element and preparation method thereof |
| CN106495697A (en) * | 2016-10-21 | 2017-03-15 | 过冬 | A kind of zirconium carbide ceramics heater and the preparation method of heater |
| WO2019119612A1 (en) * | 2017-12-21 | 2019-06-27 | 深圳市卓力能电子有限公司 | Preparation process for novel porous ceramic heating body |
| CN109185372A (en) * | 2018-10-29 | 2019-01-11 | 海宁易达自动化设备有限公司 | Hydraulic brake liner and preparation method thereof |
| CN110330340A (en) * | 2019-07-18 | 2019-10-15 | 平顶山市信瑞达石墨制造有限公司 | A kind of ceramics-graphite composite material cooker and its preparation process |
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Address after: Three Yuan Industrial Park, Xindian town high tech Zone 471000 Luoyang city in Henan Province Applicant after: LUOYANG SIGMA FURNACE STOCK INDUSTRY CO., LTD. Address before: Three Yuan Industrial Park, Xindian town high tech Zone 471000 Luoyang city in Henan Province Applicant before: Luoyang Sigma Furnace Industry Co., Ltd. |
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Application publication date: 20141022 |