CN108395241B - Preparation method of low-resistance zinc oxide ceramic - Google Patents
Preparation method of low-resistance zinc oxide ceramic Download PDFInfo
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- CN108395241B CN108395241B CN201810255458.XA CN201810255458A CN108395241B CN 108395241 B CN108395241 B CN 108395241B CN 201810255458 A CN201810255458 A CN 201810255458A CN 108395241 B CN108395241 B CN 108395241B
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Abstract
The invention belongs to the technical field of zinc oxide energy-releasing ceramics, and particularly relates to a preparation method of low-resistance zinc oxide ceramics. According to the invention, the samples are placed in a sample stacking manner, so that the surface integrity is improved, the growth of crystal grains is facilitated, and the electrical property of the product is better; sintering is carried out by combining a sectional heating and heat preservation mode, so that the sintering completeness of the ceramic is promoted, uniform and compact ceramic is obtained, and the yield, stability and electrical performance of the zinc oxide ceramic are improved. The low-resistance zinc oxide ceramic prepared by the invention has the resistivity as low as 0.54 omega cm and the energy density higher than 700J/cm3The nonlinear coefficient is less than 1.1, and the relative density is as high as 97%. The energy density is further obviously improved while the resistivity is lower, and the surface cleanliness of the final finished product is higher due to the stacking mode.
Description
Technical Field
The invention belongs to the technical field of zinc oxide energy-releasing ceramics, and relates to an improvement on a preparation method of a conventional zinc oxide ceramic resistor disc, in particular to a preparation method of low-resistance zinc oxide ceramic.
Background
In recent years, the application of high power has been increasingly limited due to the low resistivity and poor reliability of conventional general-purpose wires. Therefore, there is a strong need for a linear resistor that is small, lightweight, simple to manufacture, and can withstand large amounts of energy. The resistance of ZnO conductive ceramics is produced under the background. The high-energy zinc oxide conductive ceramic resistor is a newly developed electric appliance element, and fully exerts the characteristics of easy manufacturing and easy control of resistivity of the zinc oxide ceramic. The zinc oxide conductive ceramic has wide resistivity adjustable range, large energy density and good linearity, and the temperature coefficient of resistance can be controlled to be positive, thereby bringing advantages to series-parallel combination and being applied to various energy absorption occasions.
The preparation process of the low-resistance zinc oxide ceramic is basically the same as that of the common electronic ceramic, but the electrical performance of the low-resistance zinc oxide ceramic has high dependence on the process due to the special low-resistance characteristic, wherein the component proportion and sintering are the two most critical processes in the manufacturing process, and the micro-morphology structure, the grain components, the defects and the like of the ceramic are controlled by the raw material formula, so that the physical and chemical properties, such as conductivity and stability, of the ceramic are influenced; the sintering aims to control the conditions and the process of various physical and chemical reactions in the ceramic body, form an expected chemical composition and promote the homogenization and densification of a microstructure, thereby playing an important role in the electrical performance of the zinc oxide ceramic, and having unsatisfactory yield, conductivity and stability.
Disclosure of Invention
Aiming at the problems or the defects, the method aims to solve the problems of yield, conductivity and stability of the existing low-resistance zinc oxide ceramic sintering process. The invention provides a preparation method of low-resistance zinc oxide ceramic.
The specific technical scheme is as follows:
and 3, stacking the sheet green bodies prepared in the step 2, and sintering according to a preset sintering curve.
Further, the thickness of the sheet-shaped green body in the step 2 is 1 mm-3 mm;
further, the total thickness of the stacked sheet green bodies in the step 3 is 3-12 mm; the stacked sheet-like green bodies are sintered while being held at both ends by a brown body.
Further, the preset sintering curve in step 3 is as follows: firstly, heating from room temperature to 350 ℃ at the speed of 40-80 ℃ per hour; heating to 450 deg.C at a rate of 80-150 deg.C per hour, and maintaining for 30-60 min; then heating to 600 ℃ within 60-120min, and preserving heat for 1-2 hours; then raising the temperature to 1000 ℃ at the speed of 100-; then heating to 1350 ℃ within 50-150min, and preserving heat for 1-2 hours; finally, the low-resistance zinc oxide ceramic can be prepared by furnace cooling.
According to the invention, the samples are placed in a sample stacking manner, so that the surface integrity is improved, the growth of crystal grains is facilitated, and the electrical property of the product is better; sintering is carried out by combining a sectional heating and heat preservation mode, so that the sintering completeness of the ceramic is promoted, uniform and compact ceramic is obtained, and the yield, stability and electrical performance of the zinc oxide ceramic are improved.
The resistivity of the existing zinc oxide ceramic is 2 omega cm, and the energy density is 400J/cm3The low-resistance zinc oxide ceramic prepared by the invention has the resistivity as low as 0.54 omega cm and the energy density higher than 700J/cm3The nonlinear coefficient is less than 1.1, and the relative density is as high as 97%.
In conclusion, the zinc oxide ceramic is sintered by a stacking mode and a sectional sintering method, so that the obtained low-resistance zinc oxide ceramic has lower resistivity, the energy density is also obviously improved, and the surface cleanliness of the final finished product is higher by the stacking mode.
Drawings
FIG. 1 is a sample placement diagram of a low resistance zinc oxide ceramic of the present invention as sintered;
FIG. 2 is a sintering curve of a low-resistance zinc oxide ceramic (T in the figure is temperature, T is time);
FIG. 3 is a graph showing the relative densities of ZnO ceramics with different Al doping concentrations;
FIG. 4 is the resistivity of ZnO ceramics with different Al doping concentrations;
FIG. 5 shows the energy absorption density of ZnO released energy at different Al doping concentrations.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1:
weighing 0.5 at% (Al/Al + Zn) of aluminum oxide and zinc oxide, mixing, putting into a ball mill, wet grinding for 4 hours, granulating, forming, stacking and placing into a furnace, heating from room temperature to 350 ℃ at 60 ℃ per hour, heating to 450 ℃ at 100 ℃ per hour, preserving heat for 30min, heating to 600 ℃ at 80min, preserving heat for 1 hour, heating to 1000 ℃ at 120 ℃ per hour, preserving heat for 1 hour, heating to 1350 ℃ at 110min, preserving heat for 1 hour, and finally slowly cooling along with the furnace to obtain a sintered product with the relative density of 90-97%.
Example 2:
weighing 0.5 at% (Al/Al + Zn) of aluminum oxide and zinc oxide, mixing, putting into a ball mill, wet grinding for 4 hours, granulating, forming, stacking and placing into a furnace, heating from room temperature to 350 ℃ at 60 ℃ per hour, heating to 450 ℃ at 150 ℃ per hour, preserving heat for 45min, heating to 600 ℃ at 60min, preserving heat for 2 hours, heating to 1000 ℃ at 160 ℃ per hour, preserving heat for 1 hour, heating to 1350 ℃ at 80min, preserving heat for 2 hours, and finally slowly cooling along with the furnace to obtain a sintered product with the relative density of 90-97%.
Example 3:
weighing 1.0 at% (Al/Al + Zn) of aluminum oxide and zinc oxide, mixing, putting into a ball mill, wet-milling for 4 hours, granulating, forming, stacking and placing into a furnace, heating from room temperature to 350 ℃ at 60 ℃ per hour, heating to 450 ℃ at 100 ℃ per hour, preserving heat for 30min, heating to 600 ℃ at 80min, preserving heat for 1 hour, heating to 1000 ℃ at 120 ℃ per hour, preserving heat for 1 hour, heating to 1350 ℃ at 110min, preserving heat for 1 hour, and finally slowly cooling along with the furnace to obtain a sintered product with a relative density of 90-97%.
Example 4:
weighing 1.0 at% (Al/Al + Zn) of aluminum oxide and zinc oxide, mixing, putting into a ball mill, wet grinding for 4 hours, granulating, forming, stacking and placing into a furnace, heating from room temperature to 350 ℃ at 60 ℃ per hour, heating to 450 ℃ at 150 ℃ per hour, preserving heat for 45min, heating to 600 ℃ at 60min, preserving heat for 2 hours, heating to 1000 ℃ at 160 ℃ per hour, preserving heat for 1 hour, heating to 1350 ℃ at 80min, preserving heat for 2 hours, and finally slowly cooling along with the furnace to obtain a sintered product with a relative density of 90-97%.
FIG. 3 is a graph showing the relative densities of ZnO ceramics with different Al doping concentrations; FIG. 4 is the resistivity of ZnO ceramics with different Al doping concentrations; FIG. 5 shows the energy absorption density of ZnO released energy at different Al doping concentrations. As can be seen from the above examples and the attached drawings, the low-resistance zinc oxide ceramic prepared by the invention has the resistivity as low as 0.54 omega cm and the energy density higher than 700J/cm3The nonlinear coefficient is less than 1.1, and the relative density is as high as 97%. Has lower resistivity and obviously improved energy density.
Claims (3)
1. A preparation method of low-resistance zinc oxide ceramic comprises the following specific steps:
step 1, zinc oxide is used as a main material, aluminum oxide is used as an additive, the materials are mixed according to the atomic mass ratio of Al/(Al + Zn) of 0.5-4.0 at%, then ball milling and mixing are carried out uniformly, and drying is carried out;
step 2, adding a binder into the product obtained in the step 1 for granulation, and pressing into a sheet green body;
step 3, stacking the sheet green bodies prepared in the step 2, and sintering according to a preset sintering curve;
the preset sintering curve is as follows: firstly, heating from room temperature to 350 ℃ at the speed of 40-80 ℃ per hour; heating to 450 deg.C at a rate of 80-150 deg.C per hour, and maintaining for 30-60 min; then heating to 600 ℃ within 60-120min, and preserving heat for 1-2 hours; then raising the temperature to 1000 ℃ at the speed of 100-; then heating to 1350 ℃ within 50-150min, and preserving heat for 1-2 hours; finally, cooling along with the furnace to obtain the low-resistance zinc oxide ceramic;
and (3) clamping two ends of the sheet green compact stacked in the step 3 by using a mature compact for sintering.
2. The method for preparing the low-resistance zinc oxide ceramic according to claim 1, wherein: the thickness of the sheet green body in the step 2 is 1 mm-3 mm.
3. The method for preparing the low-resistance zinc oxide ceramic according to claim 1, wherein: and 3, the total thickness of the stacked sheet green bodies is 3-12 mm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07130503A (en) * | 1993-11-02 | 1995-05-19 | Hitachi Ltd | Manufacture of ceramic resisting body |
| CN103496966A (en) * | 2013-09-16 | 2014-01-08 | 电子科技大学 | Preparation method of low-resistivity zinc oxide ceramic material |
| CN103693954A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院福建物质结构研究所 | High conductivity zinc oxide ceramic and preparation method thereof |
| CN103896578A (en) * | 2014-03-19 | 2014-07-02 | 桂林电子科技大学 | Method for preparing high-density and low-resistivity zinc oxide ceramic target |
| CN106278239A (en) * | 2016-08-11 | 2017-01-04 | 广西新未来信息产业股份有限公司 | A kind of superelevation gradient zinc oxide piezoresistive and preparation method thereof |
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2018
- 2018-03-23 CN CN201810255458.XA patent/CN108395241B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07130503A (en) * | 1993-11-02 | 1995-05-19 | Hitachi Ltd | Manufacture of ceramic resisting body |
| CN103496966A (en) * | 2013-09-16 | 2014-01-08 | 电子科技大学 | Preparation method of low-resistivity zinc oxide ceramic material |
| CN103693954A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院福建物质结构研究所 | High conductivity zinc oxide ceramic and preparation method thereof |
| CN103896578A (en) * | 2014-03-19 | 2014-07-02 | 桂林电子科技大学 | Method for preparing high-density and low-resistivity zinc oxide ceramic target |
| CN106278239A (en) * | 2016-08-11 | 2017-01-04 | 广西新未来信息产业股份有限公司 | A kind of superelevation gradient zinc oxide piezoresistive and preparation method thereof |
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