CN103693954A - High conductivity zinc oxide ceramic and preparation method thereof - Google Patents
High conductivity zinc oxide ceramic and preparation method thereof Download PDFInfo
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- CN103693954A CN103693954A CN201310656957.7A CN201310656957A CN103693954A CN 103693954 A CN103693954 A CN 103693954A CN 201310656957 A CN201310656957 A CN 201310656957A CN 103693954 A CN103693954 A CN 103693954A
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- zinc oxide
- sintering
- oxide ceramics
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- conductivity
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Abstract
The invention relates to a method for preparing high conductivity zinc oxide ceramic through sintering in high pressure oxygen. The zinc oxide ceramic is prepared by taking zinc oxide as the main component added with aluminum oxide and gallium oxide through the steps of dispersing, grinding, smashing, pressing and sintering, wherein the sintering temperature is 700-900 DEG C, the carrier concentration of the sintered ceramic is 1.137*10<19>cm<-3>, the resistivity is 0.063(ohm cm), the carrier mobility is 8.712cm<2> V<-1> s<-1>, and the heat conductivity is 32.171W/(m*K).
Description
Technical field
The present invention relates to sintering under a kind of hyperbaric oxygen atmosphere and prepare the method for high conductivity zinc oxide ceramics, belong to field of inorganic nonmetallic material.
Background technology
Conducting ceramic material refers to a kind of new function material that possesses ionic conduction, electrons conduction in stupalith.ZnO conductivity ceramics has linear V-I characteristic, adjustable resistivity, can be used as high-power linear resistance for power transmission lines neutral point grounding resistor, can and bear very high energy by sizable electric current.[1] due to ZnO native defect, as Zn occupies O position (ZnO), calking zinc atom (Zn
i) or oxygen room (V
o) existence, make it depart from desirable stoicheiometry, ZnO presents N-shaped conductive characteristic at normal temperatures.For improving the conductive capability of conductivity ceramics, often adopt formation donor dopings such as mixing trivalent metal ion in zinc oxide, improve carrier concentration.[2] conventional ZnO conductivity ceramics preparation method has solid sintering technology.Yet adopt solid sintering technology must be at very high temperature sintering, its sintering range is 1100-2000 ℃.Because Zn and O in ZnO at high temperature easily escape, cause after sintering the physical strength of product not high and unstable.Thereby in the urgent need to a kind of method that obtains high conductivity and density zinc oxide ceramics.
Summary of the invention
The shortcoming that the object of the invention is to overcome prior art is prepared lower, the finer and close Zinc oxide-base conductivity ceramics of resistivity.The invention has the advantages that preparation, containing the pottery in Treatment with High Concentration Zinc room, adds aluminum oxide to wait, Al under strong oxidizing property atmosphere
3+after insert zinc room, a large amount of electronics are provided, improved ceramic specific conductivity.When simultaneously hyperbaric oxygen atmosphere sintering is avoided high temperature, the escape of O in zinc oxide, does not depart from the stoicheiometry of Zn and O, and perfect lattice improves the density degree of sintering, crystal grain thinning, thus improve ceramic mass.Ceramic density and specific conductivity after this processes have all obtained great lifting.
Technical scheme of the present invention comprises as follows:
In this high conductivity zinc oxide ceramics, mixed that valency is higher, ionic radius and the more approaching donor impurity of zine ion, doping quality percentage composition is 3%～5%.Wherein, donor impurity is preferably Al
3+, Ga
3+.The carrier concentration of this zinc oxide ceramics is greater than 10
19cm
-3, resistivity is less than 0.065 (Ω cm), and carrier mobility is greater than 8 (cm
2v
-1s
-1), thermal conductivity 32.171W/ (mK).
The preparation method of this zinc oxide ceramics carries out sintering in high pressure oxygen atmosphere.It is 20～60 normal atmosphere that described high pressure oxygen atmosphere pressures is preferably.
Zinc oxide conductivity ceramics prepared by present method has obvious advantage with traditional pure zinc oxide ceramic phase ratio: significantly improve its conductivity, thus the requirement of the original paper that generates heat in the oxidation that reaches a high temperature, for making high-power fixed resistor; Otherwise address the too high difficult problem of pure zinc oxide ceramic sintering temperature, the zinc oxide ceramics of doping prepared by this method, its sintering temperature only has 800 ℃.
Accompanying drawing explanation
Accompanying drawing is the ZnO pottery X-ray powder diffraction figure that sintering goes out.
Concrete steps are as follows:
1) selecting purity is that alumina powder jointed that 99.99% Zinc oxide powder, purity are 99.99% is raw material, presses: ZnO+x wt%Al
2o
3proportion ingredient, adds appropriate distilled water and alcohol dispersant, grinds 2 hours, is fully pulverized and mixed rear being dried, and with 150MPa pressure, granulation material is pressed into disk green compact;
2) disk green compact are put into sintering oven;
3) utilize mechanical pump to vacuumize annealing furnace.
4) oxygen is passed in annealing furnace to sintering in stressed situation;
5) process that sintering temperature is controlled is set.First, from normal temperature, through 10 hours to 400 ℃ left and right sintering for some time, be incubated 3 hours, throw out steam in stove, then be raised to 800 ℃ through 12 hours, at 800 ℃, maintain 12 hours, from 800 ℃, through 2 hours, reduce by 500 ℃ again, then at 500 ℃, maintain 6 hours, last cooling naturally;
Described proportion ingredient Al
2o
3addition x=3%～5%(massfraction).
Described annealing furnace, the vacuum tightness reaching is 4～5Pa.
Described passing in oxygen sintering process, the pressure of sintering oven is 20～60 normal atmosphere.
Described sintering process adopts distribution lifting warm therapy passable, reduces the temperature difference in stove, contributes to improve the compactness of material.
Beneficial effect of the present invention: oxygen atmosphere sintering makes the carrier concentration of ZnO pottery obtain greatly lifting, resistivity declines, density through high-pressure sinter also increases greatly, sample relative density is reached for 95%, film after sintering was placed in 100 ℃ of air through 4 weeks, and resistivity maintains 0.063 Ω cm without any variation.
Embodiment:
Embodiment 1:
ZnO+x wt%Al
2o
3, passing into oxygen atmosphere pressure is that 20 normal atmosphere carry out sintering, adopts vanderburg four electrode method to measure resistivity, mobility and the carrier concentration of film.At Al
2o
3content is that in 2% situation, passing into oxygen atmosphere pressure is that 20 normal atmosphere carry out sintering, again by vanderburg four electrode method, measures resistivity, mobility and the carrier concentration of film.Electric property after sintering is as shown in table 1.
The electric property of table 1 zinc oxide ceramics
Claims (5)
1. a high conductivity zinc oxide ceramics, is characterized in that: in this zinc oxide ceramics pottery, mix that valency is higher, ionic radius and the more approaching donor impurity of zine ion, doping quality percentage composition is 3%～5%.
2. zinc oxide ceramics according to claim 1, is characterized in that: described donor impurity is Al
3+, Ga
3+.
3. zinc oxide ceramics according to claim 1, is characterized in that: its carrier concentration is greater than 10
19cm
-3, resistivity is less than 0.065 (Ω cm), and carrier mobility is greater than 8 (cm
2v
-1s
-1), thermal conductivity 32.171W/ (mK).
4. the preparation method of zinc oxide ceramics described in claim 1, is characterized in that: this pottery carries out sintering in high pressure oxygen atmosphere.
5. method according to claim 3, is characterized in that: described high pressure oxygen atmosphere pressures is 20～60 normal atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310656957.7A CN103693954A (en) | 2013-12-09 | 2013-12-09 | High conductivity zinc oxide ceramic and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310656957.7A CN103693954A (en) | 2013-12-09 | 2013-12-09 | High conductivity zinc oxide ceramic and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103693954A true CN103693954A (en) | 2014-04-02 |
Family
ID=50355649
Family Applications (1)
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| CN201310656957.7A Pending CN103693954A (en) | 2013-12-09 | 2013-12-09 | High conductivity zinc oxide ceramic and preparation method thereof |
Country Status (1)
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|---|---|
| CN (1) | CN103693954A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108395241A (en) * | 2018-03-23 | 2018-08-14 | 电子科技大学 | A kind of preparation method of low-resistance zinc oxide ceramics |
| CN108821762A (en) * | 2018-06-28 | 2018-11-16 | 中山市武汉理工大学先进工程技术研究院 | A kind of antistatic Al-Doped ZnO conducting powder and its preparation method and application |
| CN115010482A (en) * | 2022-05-11 | 2022-09-06 | 内蒙古大学 | Preparation method of high-conductivity zinc oxide-based ceramic for high power |
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| CN102747334A (en) * | 2012-07-30 | 2012-10-24 | 中国科学院宁波材料技术与工程研究所 | Zinc-oxide-based transparent conductive film and preparation method thereof |
| CN103046133A (en) * | 2011-10-17 | 2013-04-17 | 中国科学院福建物质结构研究所 | Annealing method for increasing resistivity of ZnO single crystal |
| CN103193475A (en) * | 2013-03-28 | 2013-07-10 | 杭州碳诺光伏材料有限公司 | Study of preparation technology of AZO composite target material with high performance and low cost |
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2013
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103046133A (en) * | 2011-10-17 | 2013-04-17 | 中国科学院福建物质结构研究所 | Annealing method for increasing resistivity of ZnO single crystal |
| CN102747334A (en) * | 2012-07-30 | 2012-10-24 | 中国科学院宁波材料技术与工程研究所 | Zinc-oxide-based transparent conductive film and preparation method thereof |
| CN103193475A (en) * | 2013-03-28 | 2013-07-10 | 杭州碳诺光伏材料有限公司 | Study of preparation technology of AZO composite target material with high performance and low cost |
Non-Patent Citations (2)
| Title |
|---|
| WENWEN LIN ET AL.: "The growth and investigation on Ga-doped ZnO single crystals with high thermal stability and high carrier mobility", 《CRYSTENGCOMM》 * |
| ZHIBING ZHAN ET AL.: "Strategy for Preparing Al-Doped ZnO Thin Film with High Mobility and High Stability", 《CRYSTAL GROWTH & DESIGN》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108395241A (en) * | 2018-03-23 | 2018-08-14 | 电子科技大学 | A kind of preparation method of low-resistance zinc oxide ceramics |
| CN108395241B (en) * | 2018-03-23 | 2021-02-05 | 电子科技大学 | Preparation method of low-resistance zinc oxide ceramic |
| CN108821762A (en) * | 2018-06-28 | 2018-11-16 | 中山市武汉理工大学先进工程技术研究院 | A kind of antistatic Al-Doped ZnO conducting powder and its preparation method and application |
| CN108821762B (en) * | 2018-06-28 | 2021-07-13 | 中山市武汉理工大学先进工程技术研究院 | Anti-static aluminum-doped zinc oxide conductive powder and preparation method and application thereof |
| CN115010482A (en) * | 2022-05-11 | 2022-09-06 | 内蒙古大学 | Preparation method of high-conductivity zinc oxide-based ceramic for high power |
| CN115010482B (en) * | 2022-05-11 | 2023-10-24 | 内蒙古大学 | Preparation method of high-conductivity zinc oxide-based ceramic for high power |
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