CN103319161B - Composite aluminum oxide ceramic resistance material for large-power resistance element and preparation method thereof - Google Patents
Composite aluminum oxide ceramic resistance material for large-power resistance element and preparation method thereof Download PDFInfo
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- CN103319161B CN103319161B CN201310237907.5A CN201310237907A CN103319161B CN 103319161 B CN103319161 B CN 103319161B CN 201310237907 A CN201310237907 A CN 201310237907A CN 103319161 B CN103319161 B CN 103319161B
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Abstract
The invention provides a composite aluminum oxide ceramic resistance material for a large-power resistance element and a preparation method thereof. The preparation method comprises the following steps of: stirring, ball milling, granulating and tabletting the following components: 35 to 70 percent of aluminum oxide, 25 to 55 percent of molybdenum, 0 to 10 percent of nickel and 5 to 10 percent of a multi-element additive such as calcium oxide, mullite and spinel, and sintering the mixture in a vacuum furnace at the temperature of 1500 to 1600 DEG C. Prepared resistance ceramic can resist the high temperature and large-current impact and is easily welded with metal; moreover, the volt-ampere characteristic can satisfy the linear relation, and the prepared resistance ceramic can be widely applied to the fields such as large-power resistance elements.
Description
Technical field
The present invention relates to a kind of compound alumina ceramic resistive material for large power, electrically resistance element and preparation method thereof.
Background technology
The stupalith that is usually used in resistance element has silicon carbide ceramics, zinc oxide ceramics, clay carbon black pottery and carbon film pottery etc.The high temperature resistant resistance to heavy current impact of silicon carbide ceramics wherein, but that its volt-ampere characteristic is difficult to realize is linear, and its resistivity-temperature characteristics is difficult to control; Zinc oxide ceramics is as the open Zinc oxide linear resistance material of CN1395258A, its crystal grain is semi-conductor, through Composition Design, change the resistance of its grain boundary layer, can meet the controlled requirement of linear resistance and resistance, but its grain boundary layer through-current capability is poor, very easily bursts, be not suitable for the large electric current environment of high temperature under heavy current impact; Clay carbon black pottery is as the open patent of CN102250654A, prepared by its cheap being easy to, but graphite is at high temperature easy to oxidation, cannot meet the requirement of applied at elevated temperature in air atmosphere, carbon film pottery is due to its through-flow mechanism (electric current only passes through from ceramic surface carbon film) simultaneously, cannot weld with metal, limit range of application.
Alumina-ceramic can tolerate higher temperature, is also easy to carry out surface metalation and and metal solder.But itself be dielectric, need to be by doping vario-property to reduce resistivity.Patent CN101350237A discloses aluminum oxide/molybdenum composite material, although reduced ceramic resistance by doping, but this patent is used for dielectric material but not large power, electrically resistance element, and the resistivity that is greater than pottery after certain threshold value due to doping just equals the resistivity of doping metals, and single molybdenum doping is difficult to obtain the composite ceramic resistor material of expection resistivity.
Summary of the invention
The object of the present invention is to provide a kind of volt-ampere characteristic meet linear relationship, for compound alumina ceramic resistive material of large power, electrically resistance element and preparation method thereof.
For achieving the above object, the present invention has adopted following technical scheme:
A kind of compound alumina ceramic resistive material for large power, electrically resistance element, this compound alumina ceramic resistive material is by weight percentage by the aluminum oxide of 35-70%, the molybdenum of 25-55%, the nickel of 0-10% and the multielement additive of 5-10% form, and described multielement additive is the mixture of calcium oxide, mullite and spinel.
Described compound alumina ceramic resistive material is by weight percentage by the aluminum oxide of 35-70%, the molybdenum of 25-55%, and the nickel of 0.1-10% and the multielement additive of 5-10% form.
Described calcium oxide: mullite: the mass ratio of spinel is 1:(1-2): (1-2).
The preparation method of the above-mentioned compound alumina ceramic resistive material for large power, electrically resistance element, comprises the following steps:
1) raw material being comprised of described aluminum oxide, molybdenum, nickel and multielement additive is packed in ball mill, 12-48h then dry grinds;
2) raw material after dry grinding is crossed to 100 mesh sieves and obtained powder, to adding in powder, grind granulation after the polyvinyl alcohol water solution of powder weight 5-10% and obtain granulation material, the massfraction of polyvinyl alcohol water solution is 5-10%;
3) pack granulation material into mould, then on isostatic pressing machine, the granulation material that packs mould into is pressed into base substrate;
4) the base substrate demoulding is placed in vacuum oven, then under nitrogen atmosphere, in 1500-1600 ℃, is incubated 1-3 hour, furnace cooling after insulation.
Described ball mill is drum ball mill or planetary ball mill.
The pressure that described isostatic pressing machine adopts when pressing blank is 100-200MPa.
Beneficial effect of the present invention is:
The prepared compound alumina ceramic resistive material of the present invention has kept the original resistance to elevated temperatures of alumina-ceramic, and the integrity of existing technique, can tolerate heavy current impact simultaneously, surface be easy to metallization and and metal solder, can be used for the aluminum oxide conductive and heat-conductive medium under the large electric current environment of high temperature, there is preparation technology simple, cost is low, be suitable for the advantages such as large-scale industrial production, and through overdoping, the volt-ampere characteristic of stupalith meets linear relationship, overcome common carbon film pottery, the shortcoming of the linear pottery of zinc oxide, therefore can be widely used in the fields such as large power, electrically resistance element.
Further, the present invention adds two kinds of metals (molybdenum and nickel) in alumina-ceramic simultaneously, due to after two kinds of metals add, in material, the neat degree of crystal reduces, defect increases, and has affected the motion of electronics, therefore adds after two kinds of metals simultaneously, keeping under the prerequisite of linear resistive performance, the more single doping of resistivity of pottery increases to some extent.Due to after single metal-doped amount surpasses certain threshold value, the resistivity of pottery just equals the resistivity of metal, and the Changing Pattern of doping and resistivity is non-linear, be therefore difficult to measure by controlled doping the ceramic resistor material of a certain expection resistivity.The present invention is by regulating the doping ratio of two kinds of metals, can on the basis of single molybdenum doped aluminium ceramic resistor material, its steady resistance rate be improved slightly, than regulating molybdenum doping to control stupalith resistivity, more simple effective, can meet the requirement of concrete application.
Accompanying drawing explanation
Fig. 1 is the current voltage characteristic (embodiment 1 sample 3) of mixing molybdenum 35wt.%, mixing nickel 5wt.% alumina-ceramic;
Fig. 2 is the current voltage characteristic (embodiment 2 samples 3) of mixing molybdenum 35wt.% alumina-ceramic.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1
(1). first carry out proportioning raw materials, by oeverall quality per-cent, prepare to have respectively the raw material style of following component, style numbering and proportioning are in Table 1.
(2). pack raw material into ball grinder, according to the mass ratio of material: ball=1:2, in ball grinder, add alumina balls, then on planetary ball mill with the rotating speed dry grinding 24h of 600r/min;
(3). raw material after ball milling is taken out, cross 100 mesh sieves and obtain powder, to adding in powder, massfraction is 5%, quality is the PVA(polyvinyl alcohol of powder weight 5%) aqueous solution, then grind granulation and obtain granulation material;
(4). pack granulation material into mould, on isostatic pressing machine, with 150MPa, be pressed into cylinder base substrate;
(5). by the above-mentioned base substrate demoulding, under nitrogen atmosphere, (in vacuum oven) rises to 1550 ℃ with the speed of 700 ℃/h, and furnace cooling after insulation 2h, obtains compound alumina ceramic;
(6). the measurements resistivity of the compound alumina ceramic of preparation is in Table 1.
As can be seen from Table 1, when the add-on of molybdenum is greater than 35wt.%, the resistivity of pottery sharply declines, and along with the increase of molybdenum add-on, the resistivity of stupalith is stabilized in 3 * 10
-3Ω cm.
When molybdenum doping is more than or equal to 35wt.%, the current voltage characteristic of pottery is straight line, referring to Fig. 1.
Table 1 style forms and performance test
Embodiment 2
(1). first carry out proportioning raw materials, by oeverall quality per-cent, prepare to have respectively the raw material style of following component, style numbering and proportioning are in Table 2.
(2). pack raw material into ball grinder, according to the mass ratio of material: ball=1:2, in ball grinder, add alumina balls, then on planetary ball mill with the rotating speed dry grinding 24h of 600r/min;
(3). raw material after ball milling is taken out, cross 100 mesh sieves and obtain powder, to adding in powder, massfraction is 5%, quality is the PVA(polyvinyl alcohol of powder weight 5%) aqueous solution, then grind granulation and obtain granulation material;
(4). pack granulation material into mould, on isostatic pressing machine, with 150MPa, be pressed into cylinder base substrate;
(5). by the above-mentioned base substrate demoulding, under nitrogen atmosphere, (in vacuum oven) rises to 1550 ℃ with the speed of 700 ℃/h, and furnace cooling after insulation 2h, obtains compound alumina ceramic;
(6). the measurements resistivity of the compound alumina ceramic of preparation is in Table 2.
As can be seen from Table 2, when the doping of molybdenum is greater than 35wt%, the resistivity of stupalith sharply declines, and in the absence of nickel doping, the resistivity of pottery is lower, can meet the environment for use of larger electric current.
When molybdenum doping is more than or equal to 35wt.%, the current voltage characteristic of pottery is straight line, referring to Fig. 2.
Table 2 style forms and performance test
Claims (5)
1. the compound alumina ceramic resistive material for large power, electrically resistance element, it is characterized in that: this compound alumina ceramic resistive material is by weight percentage by the aluminum oxide of 35-70%, the molybdenum of 25-55%, the nickel of 0.1-10% and the multielement additive of 5-10% form, and described multielement additive is the mixture of calcium oxide, mullite and spinel.
2. a kind of compound alumina ceramic resistive material for large power, electrically resistance element according to claim 1, is characterized in that: described calcium oxide: mullite: the mass ratio of spinel is 1:(1-2): (1-2).
3. as claimed in claim 1 for a preparation method for the compound alumina ceramic resistive material of large power, electrically resistance element, it is characterized in that: comprise the following steps:
1) raw material being comprised of described aluminum oxide, molybdenum, nickel and multielement additive is packed in ball mill, 12-48h then dry grinds;
2) raw material after dry grinding is crossed to 100 mesh sieves and obtained powder, to adding in powder, grind granulation after the polyvinyl alcohol water solution of powder weight 5-10% and obtain granulation material, the massfraction of polyvinyl alcohol water solution is 5-10%;
3) pack granulation material into mould, then on isostatic pressing machine, the granulation material that packs mould into is pressed into base substrate;
4) the base substrate demoulding is placed in vacuum oven, then under nitrogen atmosphere, in 1500-1600 ℃, is incubated 1-3 hour, furnace cooling after insulation.
4. a kind of preparation method of the compound alumina ceramic resistive material for large power, electrically resistance element according to claim 3, is characterized in that: described ball mill is drum ball mill or planetary ball mill.
5. a kind of preparation method of the compound alumina ceramic resistive material for large power, electrically resistance element according to claim 3, is characterized in that: the pressure that described isostatic pressing machine adopts when pressing blank is 100-200MPa.
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| CN110981522B (en) * | 2019-12-12 | 2022-03-18 | 西安建筑科技大学 | Resistivity-controllable high-power-density metal ceramic resistor material and preparation method thereof |
| CN112824345A (en) * | 2020-07-31 | 2021-05-21 | 北京七一八友晟电子有限公司 | Pulse-resistant and surge-resistant ceramic resistor and manufacturing process thereof |
| CN114141458B (en) * | 2021-11-30 | 2023-07-18 | 尧中华 | High-stability high-power ceramic resistor and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0907621B1 (en) * | 1996-05-30 | 2001-04-11 | Fraunhofer-Gesellschaft Zur Förderung Der Angewandten Forschung E.V. | Open-cell expanded ceramic with a high level of strength, and process for the production thereof |
| CN101023194B (en) * | 2004-07-15 | 2011-04-13 | 通用电气公司 | Electrically conductive cermet and method of making |
| CN102219517A (en) * | 2010-04-14 | 2011-10-19 | 浙江晟翔电子科技有限公司 | Multiphase ceramic material with adjustable resistivity and preparation technology thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0907621B1 (en) * | 1996-05-30 | 2001-04-11 | Fraunhofer-Gesellschaft Zur Förderung Der Angewandten Forschung E.V. | Open-cell expanded ceramic with a high level of strength, and process for the production thereof |
| CN101023194B (en) * | 2004-07-15 | 2011-04-13 | 通用电气公司 | Electrically conductive cermet and method of making |
| CN102219517A (en) * | 2010-04-14 | 2011-10-19 | 浙江晟翔电子科技有限公司 | Multiphase ceramic material with adjustable resistivity and preparation technology thereof |
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