CN109305811A - A kind of microwave-assisted zinc oxide ceramics sintering method - Google Patents
A kind of microwave-assisted zinc oxide ceramics sintering method Download PDFInfo
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- CN109305811A CN109305811A CN201811240887.6A CN201811240887A CN109305811A CN 109305811 A CN109305811 A CN 109305811A CN 201811240887 A CN201811240887 A CN 201811240887A CN 109305811 A CN109305811 A CN 109305811A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/667—Sintering using wave energy, e.g. microwave sintering
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Abstract
The present invention provides a kind of microwave-assisted zinc oxide ceramics sintering method, the following steps are included: carrying out pre-treatment to Zinc oxide powder using acid solution obtains mixture；Mixture is put into mold, by mold, cooling obtains zinc oxide solid phase ceramics after pressure sintering under microwave environment.The present invention passes through microwave-assisted cold sintering process, in the case where sintering temperature is lower than 300 DEG C, the density of zinc oxide ceramics sample can be more than the 90% of theoretical value, conductivity and the conductivity for the zinc oxide ceramics being sintered under conventional high temperature are very nearly the same, and preparation process is simple and convenient, low energy consumption, and sintering time is short, safe low pollution.
Description
Technical field
The invention belongs to ceramic materials preparation technology fields, and in particular to a kind of microwave-assisted zinc oxide ceramics sintering side
Method.
Background technique
Zinc oxide ceramics refers to that zinc oxide is that one kind electronic ceramics material made of dopant appropriate etc. is added in principal crystalline phase
Material.With excellent nonlinear factor, pressure sensitive voltage range wide (zero point a few volt to tens kilovolts), voltage temperature coefficient it is small, when
Between respond the features such as fast, leakage current is small.Primary raw material is zinc oxide, and dopant has bismuth oxide, cobalt oxide, strontium oxide strontia, titanium oxide
Deng.It can be used for manufacturing voltage stabilizing element and the overvoltage protection element (low voltage varistor in such as integrated circuit in high-tension circuit
Device), it can be also used as arrester.
The manufacturing method of zinc oxide ceramics has the conventional sinterings technique such as normal pressure-sintered method and hot pressing sintering method at present.Tradition pottery
The production technology of ceramic material is a kind of production technology of high energy consumption, especially the sintering process of zinc oxide ceramics material.Due to oxygen
The sintering temperature for changing zinc, which is typically necessary, reaches 1400 DEG C or so, and energy consumption is very big；Though in addition, utilizing additive and sintering aid
So have the advantages that it is certain, but will affect ceramic material consistency and there are leakage current increase, nonlinear factor reduce etc.
A series of problems.
Currently, being added in powder according to the cold-rolled sintered technology that Randall seminar of Pennsylvania State University proposes
Enter a small amount of liquid, in the case where pressurization and heating, powder surface is partly dissolved and resets, and liquid seeps rapidly under stress
Thoroughly in pellet pores, as the temperature rises, dissolve-repreparation process occurs for liquid evaporation, particle surface, to realize
Ceramic densifying.Ceramic sintering temperature greatly reduces in this cold-rolled sintered technique, but can not keep away during ceramic post sintering
It grows up with crystal grain with exempting from, so how to control nano particle growing up during the sintering process, the excellent zinc oxide of processability
Ceramics are that nano zine oxide ceramic material prepares the problem faced, are one of the greatest problems for perplexing researcher.So
We need to improve existing sintering process or develop the sintering that new sintering process is applied to zinc oxide ceramics material.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of microwave-assisted zinc oxide ceramics sintering method, leads to
Cross microwave-assisted, the densification sintering technique of completion zinc oxide ceramics powder in the case where sintering temperature is lower than 300 DEG C.Oxidation
The density of zinc ceramics sample can be more than the 90% of theoretical value, the electricity of conductivity and the zinc oxide ceramics being sintered under conventional high temperature
Conductance is equally matched, and preparation process is simple and convenient, and low energy consumption, and sintering time is short, safe low pollution.
The technical solution of the present invention is as follows:
A kind of microwave-assisted zinc oxide ceramics sintering method, comprising the following steps: using acid solution to Zinc oxide powder
It carries out pre-treatment and obtains mixture；Mixture is put into mold, by mold, cooling is obtained after pressure sintering under microwave environment
Zinc oxide solid phase ceramics.
Further, the Zinc oxide powder partial size is less than 50 μm.
Further, the acid solution includes formic acid solution, acetic acid solution.
Further, the mass concentration of the acid solution is lower than 40%.
Further, the mold is ceramic mold.
Further, the control parameter of the pressure sintering under microwave environment are as follows: microwave power is less than 300W, Microwave Frequency
Rate is 915MHz or 2450MHz, and pressure is no more than 10MPa, and sintering temperature is no more than 300 DEG C, and sintering time is 4~30min.
Further, the relative density of the zinc oxide solid phase ceramics is greater than 90%.
The beneficial effects of the present invention are: the present invention is lower than 300 DEG C by microwave-assisted cold sintering process, in sintering temperature
In the case where, the density of zinc oxide ceramics sample can be more than the 90% of theoretical value, conductivity be sintered under conventional high temperature
The conductivity of zinc oxide ceramics is very nearly the same, and preparation process is simple and convenient, and low energy consumption, and sintering time is short, safe low pollution.
Detailed description of the invention
Fig. 1 is the XRD diagram of zinc oxide ceramics under three kinds of different microwaves in the embodiment of the present invention 3,4,5.
Specific embodiment
In the description of the present invention, it should be noted that the person that is not specified actual conditions in embodiment, according to normal conditions or
The condition that manufacturer suggests carries out.Reagents or instruments used without specified manufacturer is that can be obtained by commercially available purchase
Conventional products.
The present invention is described in further details with specific embodiment with reference to the accompanying drawing, described is to solution of the invention
It releases rather than limits.
Embodiment 1
Zinc oxide powder is uniformly mixed with the aqueous formic acid of 0.1mol/L, the mass ratio of zinc oxide and formic acid solution is
4:1。
Mixture is put into mold, then mold is put into microwave cavity, applies the pressure of 10MPa, microwave power 100W,
Sample is heated to 177 DEG C with the speed of 5 DEG C/min, and is kept for 4 minutes by microwave frequency 915MHz, is then cooled down in air.
After cooling and releasing stress, 0.5 inch of the zinc oxide sample that sintering is completed is obtained, density is as shown in table 1.
Embodiment 2
Zinc oxide powder is uniformly mixed with the aqueous formic acid of 0.1mol/L, the mass ratio of zinc oxide and formic acid solution is
4:1。
Mixture is put into mold, then mold is put into microwave cavity, applies the pressure of 10MPa, microwave power 200W,
Sample is heated to 220 DEG C with the speed of 5 DEG C/min, and is kept for 10 minutes by microwave frequency 915MHz, then cold in air
But.After cooling and releasing stress, 0.5 inch of the zinc oxide sample that sintering is completed is obtained, density is as shown in table 1.
Embodiment 3
Zinc oxide powder is uniformly mixed with the aqueous formic acid of 0.1mol/L, the mass ratio of zinc oxide and formic acid solution is
4:1。
Mixture is put into mold, then mold is put into microwave cavity, applies the pressure of 10MPa, microwave power 250W,
Sample is heated to 300 DEG C with the speed of 5 DEG C/min, and is kept for 20 minutes by microwave frequency 915MHz, then cold in air
But.After cooling and releasing stress, 0.5 inch of the zinc oxide sample that sintering is completed is obtained, density is as shown in table 1,
XRD result is as shown in Figure 1.
Embodiment 4
Zinc oxide powder is uniformly mixed with the aqueous formic acid of 0.1mol/L, the mass ratio of zinc oxide and formic acid solution is
4:1。
Mixture is put into mold, then mold is put into microwave cavity, applies the pressure of 10MPa, microwave power 300W,
Sample is heated to 177 DEG C with the speed of 5 DEG C/min, and is kept for 30 minutes by microwave frequency 915MHz, then cold in air
But.After cooling and releasing stress, 0.5 inch of the zinc oxide sample that sintering is completed is obtained, density is as shown in table 1,
XRD result is as shown in Figure 1.
Embodiment 5
Zinc oxide powder is uniformly mixed with the aqueous formic acid of 0.1mol/L, the mass ratio of zinc oxide and formic acid solution is
4:1。
Mixture is put into mold, then mold is put into microwave cavity, applies the pressure of 10MPa, microwave power 350W,
Sample is heated to 177 DEG C with the speed of 5 DEG C/min, and keeps 4min by microwave frequency 2450MHz, is then cooled down in air.
After cooling and releasing stress, 0.5 inch of the zinc oxide sample that sintering is completed is obtained, density is as shown in table 1, XRD
As a result as shown in Figure 1.
Embodiment 6
Zinc oxide powder is uniformly mixed with the aqueous formic acid of 0.1mol/L, the mass ratio of zinc oxide and formic acid solution is
4:1。
Mixture is put into mold, then mold is put into microwave cavity, applies the pressure of 10MPa, microwave power 200W,
Sample is heated to 220 DEG C with the speed of 5 DEG C/min, and is kept for 10 minutes by microwave frequency 2450MHz, then cold in air
But.After cooling and releasing stress, 0.5 inch of the zinc oxide sample that sintering is completed is obtained, density is as shown in table 1.
Embodiment 7
Zinc oxide powder is uniformly mixed with the acetic acid aqueous solution of 0.1mol/L, the mass ratio of zinc oxide and acetic acid solution is
4:1。
Mixture is put into mold, then mold is put into microwave cavity, applies the pressure of 10MPa, microwave power 250W,
Sample is heated to 300 DEG C with the speed of 5 DEG C/min, and is kept for 20 minutes by microwave frequency 2450MHz, then cold in air
But.After cooling and releasing stress, 0.5 inch of the zinc oxide sample that sintering is completed is obtained, density is as shown in table 1.
Embodiment 8
Zinc oxide powder is uniformly mixed with the acetic acid aqueous solution of 0.1mol/L, the mass ratio of zinc oxide and acetic acid solution is
4:1。
Mixture is put into mold, then mold is put into microwave cavity, applies the pressure of 10MPa, microwave power 300W,
Sample is heated to 177 DEG C with the speed of 5 DEG C/min, and is kept for 30 minutes by microwave frequency 2450MHz, then cold in air
But.After cooling and releasing stress, 0.5 inch of the zinc oxide sample that sintering is completed is obtained, density is as shown in table 1.
Table 1 provides the zinc oxide ceramics density of all embodiment preparations.
Table 1
To sum up, in the specific embodiment of the invention, by microwave-assisted, in the case where sintering temperature is no more than 300 DEG C
Complete the densification sintering technique of zinc oxide ceramics powder.The density of zinc oxide ceramics sample can be more than the 90% of theoretical value.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (7)
1. a kind of microwave-assisted zinc oxide ceramics sintering method, which comprises the following steps: using acid solution to oxygen
Change zinc powder progress pre-treatment and obtains mixture；Mixture is put into mold, by mold after pressure sintering under microwave environment
It is cooling to obtain zinc oxide solid phase ceramics.
2. the microwave-assisted zinc oxide ceramics sintering method of one kind according to claim 1, which is characterized in that the oxidation
Zinc powder partial size is less than 50 μm.
3. the microwave-assisted zinc oxide ceramics sintering method of one kind according to claim 1, which is characterized in that the acid is molten
Liquid includes formic acid solution, acetic acid solution.
4. the microwave-assisted zinc oxide ceramics sintering method of one kind according to claim 1 or 3, which is characterized in that described
The mass concentration of acid solution is lower than 40%.
5. the microwave-assisted zinc oxide ceramics sintering method of one kind according to claim 1, which is characterized in that the mold
For ceramic mold.
6. the microwave-assisted zinc oxide ceramics sintering method of one kind according to claim 1, which is characterized in that described micro-
The control parameter of pressure sintering under wave environment are as follows: microwave power is less than 300W, and microwave frequency is 915MHz or 2450MHz, pressure
Power is no more than 10MPa, and sintering temperature is no more than 300 DEG C, and sintering time is 4~30min.
7. the microwave-assisted zinc oxide ceramics sintering method of one kind according to claim 1, which is characterized in that the oxidation
The relative density of zinc solid phase ceramics is greater than 90%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527082A (en) * | 2021-06-29 | 2021-10-22 | 西安交通大学 | Electronic functional ceramic and manufacturing method and application thereof |
| CN115947596A (en) * | 2023-01-16 | 2023-04-11 | 西安交通大学 | Microwave medium ceramic material based on microwave cold sintering and low-carbon preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786161A (en) * | 2010-01-19 | 2010-07-28 | 武汉科技大学 | Microwave irradiation pressurized sintering equipment and use method thereof |
-
2018
- 2018-10-24 CN CN201811240887.6A patent/CN109305811A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786161A (en) * | 2010-01-19 | 2010-07-28 | 武汉科技大学 | Microwave irradiation pressurized sintering equipment and use method thereof |
Non-Patent Citations (2)
| Title |
|---|
| SHUICHI FUNAHASHI ET AL.: ""Demonstration of the cold sintering process study for the densification and grain growth of ZnO ceramics"", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
| 方可: ""微波烧结纳米氧化锌陶瓷材料研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527082A (en) * | 2021-06-29 | 2021-10-22 | 西安交通大学 | Electronic functional ceramic and manufacturing method and application thereof |
| CN113527082B (en) * | 2021-06-29 | 2022-04-22 | 西安交通大学 | Electronic functional ceramic and manufacturing method and application thereof |
| CN115947596A (en) * | 2023-01-16 | 2023-04-11 | 西安交通大学 | Microwave medium ceramic material based on microwave cold sintering and low-carbon preparation method |
| CN115947596B (en) * | 2023-01-16 | 2023-12-05 | 西安交通大学 | Microwave dielectric ceramic material based on microwave cold sintering and low-carbon preparation method |
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