CN115947596A - Microwave medium ceramic material based on microwave cold sintering and low-carbon preparation method - Google Patents
Microwave medium ceramic material based on microwave cold sintering and low-carbon preparation method Download PDFInfo
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- CN115947596A CN115947596A CN202310065143.XA CN202310065143A CN115947596A CN 115947596 A CN115947596 A CN 115947596A CN 202310065143 A CN202310065143 A CN 202310065143A CN 115947596 A CN115947596 A CN 115947596A
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- 238000005245 sintering Methods 0.000 title claims abstract description 86
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 18
- 239000000919 ceramic Substances 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000007791 liquid phase Substances 0.000 claims abstract description 15
- 238000004321 preservation Methods 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 238000009768 microwave sintering Methods 0.000 claims abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 229910001220 stainless steel Inorganic materials 0.000 claims description 13
- 239000010935 stainless steel Substances 0.000 claims description 13
- 239000004408 titanium dioxide Substances 0.000 claims description 13
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 10
- 238000000280 densification Methods 0.000 abstract description 4
- 239000011812 mixed powder Substances 0.000 description 12
- 238000005303 weighing Methods 0.000 description 10
- NMHMDUCCVHOJQI-UHFFFAOYSA-N lithium molybdate Chemical compound [Li+].[Li+].[O-][Mo]([O-])(=O)=O NMHMDUCCVHOJQI-UHFFFAOYSA-N 0.000 description 5
- MODMKKOKHKJFHJ-UHFFFAOYSA-N magnesium;dioxido(dioxo)molybdenum Chemical compound [Mg+2].[O-][Mo]([O-])(=O)=O MODMKKOKHKJFHJ-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000004891 communication Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910017964 MgMoO4 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010344 co-firing Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000012826 global research Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention discloses a microwave medium ceramic material based on microwave cold sintering and a low-carbon preparation method, which comprises the following steps: mixing the ceramic and the liquid phase for 5-60 minutes, wherein the mass fraction of the ceramic powder is 50% -95% and the balance is the liquid phase content after mixing; step two: tabletting the mixture obtained in the first step; step three: and putting the pressed product into a microwave sintering furnace for sintering, wherein the sintering temperature is 100-1000 ℃, the heating rate is 1-50 ℃/min, and the heat preservation time is 10-300 min, so as to obtain the microwave dielectric ceramic. Compared with the traditional high-temperature sintering, the preparation time of the sample is greatly shortened, the sintering temperature of the sample is reduced, high densification can be achieved, and the microwave dielectric property of the sample can be comparable to or even better than that of the sample prepared by the traditional method.
Description
Technical Field
The invention belongs to the field of electronic information devices, and relates to a microwave medium ceramic material based on microwave cold sintering and a low-carbon preparation method.
Background
The continuous innovation and the vigorous development of the wireless communication technology provide higher requirements on the aspects of miniaturization, integration, low cost, high reliability and the like of microwave components. The low temperature co-fired ceramic/ultra-low temperature co-fired ceramic technology is developed and widely applied. The research on the energy-saving environment-friendly green preparation process with lower sintering temperature, higher sintering efficiency and excellent microwave dielectric property has become one of the global research hotspots.
The microwave dielectric ceramic is an electronic functional ceramic material with a certain function in a microwave frequency band (frequency range: 300MHz to 300GHz, and corresponding wavelength range is 1m-1 mm) circuit, is widely applied to resonators, filters, frequency discriminators, waveguides, antennas and the like, and plays an important role in the fields of communication technology, military and the like. Microwave dielectric ceramics should have low sintering temperature and appropriate relative dielectric constant (epsilon) as one of key materials of low temperature co-fired ceramic technology (LTCC) r ) High quality factor (Q) f ) And a near-zero temperature coefficient of resonance frequency (TCF). Accordingly, microwave dielectric ceramicsThe sintering temperature of the method is also developed in the direction of lower and more energy-saving. The microwave dielectric ceramic prepared by the traditional method usually needs a high temperature of more than 1000 ℃, so that the process period is long, the energy consumption is high, and the integrated co-firing of various material systems is difficult to realize.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a microwave dielectric ceramic material based on microwave cold sintering and a low-carbon preparation method, high densification of the ceramic is achieved at lower temperature in shorter time, a required ceramic finished product is finally obtained, the density of an obtained ceramic sample is higher than 95%, and the microwave dielectric property of the ceramic material is excellent.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a low-carbon preparation method of a microwave dielectric ceramic material based on microwave cold sintering comprises the following steps:
the method comprises the following steps: mixing the ceramic and the liquid phase, wherein the mass fraction of the ceramic powder is 50-95% and the balance is the liquid phase;
step two: tabletting the mixture obtained in the first step;
step three: and sintering the pressed product in a microwave sintering furnace at the sintering temperature of 100-1000 ℃, at the heating rate of 1-50 ℃/min and at the heat preservation time of 10-300 min to obtain the microwave dielectric ceramic.
Preferably, the ceramic in the first step comprises 50-90% by mass of titanium dioxide, and the liquid phase comprises 5-35% by mass of tetrabutyl titanate and 1-20% by mass of deionized water; the sintering temperature in the third step is 900-1000 ℃.
Further, titanium dioxide and tetrabutyl titanate are weighed and mixed, and then deionized water with the mass fraction of 1% -20% is added for full mixing.
Preferably, the ceramic in the first step comprises 80-95% of MgMoO in mass fraction 4 The sintering temperature in the third step is 700-900 ℃.
Preferably, the pottery in the step oneThe porcelain comprises 80 to 95 mass percent of Li 2 MoO 4 And the sintering temperature in the third step is 100-200 ℃.
Preferably, in step one, the ceramic powder and the liquid phase are mixed.
Preferably, the pressure range is 10-500MPa and the dwell time is 1-5 minutes during tabletting treatment.
Preferably, in the second step, the mixture in the first step is placed in a stainless steel mold and then placed on a press for compression molding.
The microwave dielectric ceramic is prepared by the microwave cold sintering-based low-carbon preparation method of the microwave dielectric ceramic material.
Compared with the prior art, the invention has the following beneficial effects:
compared with the traditional high-temperature sintering, the microwave cold sintering process greatly shortens the time for preparing the sample and reduces the temperature for sintering the sample. In the traditional ceramic preparation method, a great deal of time is needed for the steps of granulation, glue discharge and the like, but the steps can be completely omitted by the method provided by the invention. The microwave dielectric ceramic sample prepared by the method can achieve high densification, and the microwave dielectric property of the sample can be comparable to or even better than that of the sample prepared by the traditional method.
The compactness of the titanium dioxide microwave dielectric ceramic, the magnesium molybdate microwave dielectric ceramic and the lithium molybdate microwave dielectric ceramic prepared by the invention can reach more than 95 percent after sintering. The sintered compact titanium dioxide microwave dielectric ceramic has a relative dielectric constant of 103 f Values of 40,000ghz can be achieved. The sintered compact magnesium molybdate microwave dielectric ceramic has the relative dielectric constant of 6 to 8 f The value can reach 150,000GHz, the temperature coefficient of resonance frequency (TCF) is-85 to-50 ppm/DEG C, the relative dielectric constant of the sintered compact lithium molybdate microwave dielectric ceramic is 5 to 7, Q f The value can reach 30,000GHz, and the temperature coefficient of resonance frequency (TCF) is-150 to-100 ppm/DEG C.
Drawings
FIG. 1 is a flow chart of the microwave cold sintering process of the present invention;
FIG. 2 is the evolution of Gibbs free energy during microwave cold sintering and conventional sintering according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments; all other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "front," "back," "left," "right," "upper" and "lower" used in the following description refer to directions in the drawings, and the terms "inner" and "outer" refer to directions toward and away from, respectively, the geometric center of a particular component.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
As shown in figure 1, the microwave cold sintering process adopted by the invention is simple and convenient to operate, and mainly comprises the following steps: the method comprises the steps of fully mixing ceramic powder with a liquid phase with a proper content, then loading the mixed powder into a die for tabletting, and finally placing a sample into a microwave sintering furnace for sintering to finally obtain a highly compact ceramic sample.
As shown in figure 2, the microwave cold sintering process of the invention is compared with the evolution of Gibbs free energy in the traditional sintering process, and can be seen that the microwave cold sintering process of the invention utilizes the intermediate liquid phase to form a layer of liquid phase film on the surface of ceramic particles, thereby increasing the driving force of diffusion and mass transfer of the ceramic particles, putting the pressed block sample into a microwave oven for sintering, and utilizing three physical fields of 'electric field + magnetic field + thermal field' to carry out 'internal and external synchronous heating' on the sample, thereby further promoting the dissolution-precipitation of ceramic and the growth process of crystal grains. Compared with the traditional high-temperature sintering, the microwave cold sintering process greatly shortens the time for preparing the sample and reduces the temperature for sintering the sample. The microwave dielectric ceramic sample prepared by the microwave cold sintering method can achieve high densification, and the microwave dielectric property of the sample can be comparable to or even better than that of the sample prepared by the traditional method.
The invention relates to a low-carbon preparation method of microwave dielectric ceramic based on a microwave cold sintering process, which comprises the following steps of:
the method comprises the following steps: mixing the ceramic powder and the selected liquid phase for 5-60 minutes, wherein the mass fraction of the ceramic powder is 50% -95% and the balance is the liquid phase;
step two: tabletting the mixture obtained in the first step;
step three: and (3) performing microwave sintering on the pressed product, wherein the sintering temperature is 100-1000 ℃, the heating rate is 1-50 ℃/min, and the heat preservation time is 10-300 min, so as to obtain the microwave dielectric ceramic.
When the ceramic powder is titanium dioxide, in the step one, 50-90% by mass of titanium dioxide and 5-35% by mass of tetrabutyl titanate are weighed and mixed. Then deionized water with the mass fraction of 1% -20% is added for mixing. The sintering temperature in the third step is 900-1000 ℃.
When the ceramic powder adopts MgMoO 4 In the first step, 80-95% of MgMoO4 powder and 5-20% of deionized water are weighed, and the sintering temperature in the third step is 700-900 ℃.
When the ceramic powder uses Li 2 MoO 4 Then, 80-95% of Li is weighed 2 MoO 4 The powder and deionized water with the mass fraction of 5-20 percent, and the sintering temperature in the third step is 100-200 ℃.
The first embodiment is as follows:
the method comprises the following steps: weighing 50 mass percent of titanium dioxide and 35 mass percent of tetrabutyl titanate for mixing. Then, deionized water was added thereto in an amount of 15% by mass, and the mixture was mixed for 5 minutes.
Step two: pouring the uniformly mixed powder into a stainless steel mold, then putting the mold filled with the sample on a press, pressurizing under 100MPa for 1 minute, and taking out the massive sample after pressurization.
Step three: and D, putting the blocky sample prepared in the step two into a microwave oven for sintering. The heating rate is 1 ℃/min, the sintering temperature is 800 ℃, and the heat preservation time is 30 minutes.
The properties of the group of ceramic materials reach the following indexes:
after being sintered in air at 800 ℃, the relative density of the sample is about 90 percent, and the microwave dielectric property is epsilon r ＝80，Q f ＝25,000GHz，TCF＝350ppm/℃(25℃-85℃)。
The second embodiment:
the method comprises the following steps: weighing and mixing 90 mass percent of titanium dioxide and 5 mass percent of tetrabutyl titanate. Then, deionized water was added thereto in an amount of 5% by mass, and the mixture was mixed for 15 minutes.
Step two: and pouring the uniformly mixed powder into a stainless steel mold, putting the mold filled with the sample on a press, pressurizing at 500MPa for 5 minutes, and taking out the massive sample after pressurization.
Step three: and D, putting the block sample prepared in the step two into a microwave oven for sintering. The heating rate is 10 ℃/min, the sintering temperature is 1000 ℃, and the heat preservation time is 200 minutes.
The properties of the group of ceramic materials reach the following indexes:
after sintering in the air at 1000 ℃, the relative density of the sample is about 97 percent, and the microwave dielectric property is epsilon r ＝105，Qf＝35,000GHz，TCF＝441ppm/℃(25℃-85℃)。
Example three:
the method comprises the following steps: weighing 89 mass percent of titanium dioxide and 10 mass percent of tetrabutyl titanate for mixing. Then, deionized water was added thereto in an amount of 1% by mass, and the mixture was mixed for 20 minutes.
Step two: pouring the uniformly mixed powder into a stainless steel mold, then putting the mold filled with the sample on a press for pressurization, wherein the pressure is 100MPa, the pressure maintaining time is 1 minute, and taking out the block sample after the pressurization is finished.
Step three: and D, putting the blocky sample prepared in the step two into a microwave oven for sintering. The heating rate is 1 ℃/min, the sintering temperature is 800 ℃, and the heat preservation time is 30 minutes.
The performance of the group of ceramic materials reaches the following indexes:
after sintering in air at 800 ℃, the relative density of the sample is about 92 percent, and the microwave dielectric property is epsilon r ＝95，Q f ＝33,000GHz，TCF＝364ppm/℃(25℃-85℃)。
Example four:
the method comprises the following steps: weighing and mixing 75 mass percent of titanium dioxide and 20 mass percent of tetrabutyl titanate. Then, deionized water was added thereto in an amount of 5% by mass, and the mixture was mixed for 60 minutes.
Step two: pouring the uniformly mixed powder into a stainless steel mold, then putting the mold filled with the sample on a press for pressurization, wherein the pressure is 100MPa, the pressure maintaining time is 1 minute, and taking out the block sample after the pressurization is finished.
Step three: and D, putting the blocky sample prepared in the step two into a microwave oven for sintering. The heating rate is 1 ℃/min, the sintering temperature is 1000 ℃, and the heat preservation time is 300 minutes.
The performance of the group of ceramic materials reaches the following indexes:
after sintering in the air at 1000 ℃, the relative density of the sample is about 93 percent, and the microwave dielectric property is epsilon r ＝92，Q f ＝30,000GHz，TCF＝400ppm/℃(25℃-85℃)。
Example five:
the method comprises the following steps: weighing and mixing 75 mass percent of titanium dioxide and 5 mass percent of tetrabutyl titanate. Then, deionized water was added thereto in an amount of 20% by mass, and the mixture was mixed for 30 minutes.
Step two: pouring the uniformly mixed powder into a stainless steel mold, then putting the mold filled with the sample on a press, pressurizing at 10MPa for 1 minute, and taking out the massive sample after pressurization.
Step three: and D, putting the block sample prepared in the step two into a microwave oven for sintering. The heating rate is 50 ℃/min, the sintering temperature is 900 ℃, and the heat preservation time is 10 minutes.
The properties of the group of ceramic materials reach the following indexes:
after sintering in air at 900 ℃, the relative density of the sample is about 91 percent, and the microwave dielectric property is epsilon r ＝90，Q f ＝27,000GHz，TCF＝387ppm/℃(25℃-85℃)。
Example six:
the method comprises the following steps: weighing 80 mass percent of magnesium molybdate powder and 20 mass percent of deionized water, and mixing for 60 minutes.
Step two: pouring the uniformly mixed powder into a stainless steel mold, then putting the mold filled with the sample on a press, pressurizing under 100MPa for 1 minute, and taking out the massive sample after pressurization.
Step three: and D, putting the block sample prepared in the step two into a microwave oven for sintering. The heating rate is 1 ℃/min, the sintering temperature is 700 ℃, and the heat preservation time is 10 minutes.
The performance of the group of ceramic materials reaches the following indexes:
after sintering in air at 700 ℃, the relative density of the sample is about 85 percent, and the microwave dielectric property is epsilon r ＝6.8，Q f ＝40,000GHz，TCF＝-51ppm/℃(25℃-85℃)。
Example seven:
the method comprises the following steps: weighing 90 mass percent of magnesium molybdate powder and 10 mass percent of deionized water, and mixing for 5 minutes.
Step two: and pouring the uniformly mixed powder into a stainless steel mold, putting the mold filled with the sample on a press, pressurizing at 500MPa for 5 minutes, and taking out the massive sample after pressurization.
Step three: and D, putting the block sample prepared in the step two into a microwave oven for sintering. The heating rate is 30 ℃/min, the sintering temperature is 900 ℃, and the heat preservation time is 200 minutes.
The properties of the group of ceramic materials reach the following indexes:
after sintering in air at 900 ℃, the relative density of the sample is about 95 percent, and the microwave dielectric property is epsilon r ＝7.2，Q f ＝150,000GHz，TCF＝-85ppm/℃(25℃-85℃)。
Example eight:
the method comprises the following steps: weighing magnesium molybdate powder with the mass fraction of 95% and deionized water with the mass fraction of 5%, and mixing for 30 minutes.
Step two: pouring the uniformly mixed powder into a stainless steel mold, then putting the mold filled with the sample on a press for pressurizing at the pressure of 10MPa for 3 minutes, and taking out the massive sample after pressurizing.
Step three: and D, putting the blocky sample prepared in the step two into a microwave oven for sintering. The heating rate is 50 ℃/min, the sintering temperature is 800 ℃, and the heat preservation time is 300 minutes.
Example nine:
the method comprises the following steps: 80 mass percent of lithium molybdate powder and 20 mass percent of deionized water are weighed and mixed for 5 minutes.
Step two: pouring the uniformly mixed powder into a stainless steel mold, then putting the mold filled with the sample on a press for pressurization, wherein the pressure is 100MPa, the pressure maintaining time is 1 minute, and taking out the block sample after the pressurization is finished.
Step three: and D, putting the blocky sample prepared in the step two into a microwave oven for sintering. The heating rate is 1 ℃/min, the sintering temperature is 100 ℃, and the heat preservation time is 10 minutes.
The performance of the group of ceramic materials reaches the following indexes:
after sintering in air at 100 ℃, the relative density of the sample is about 92 percent, and the microwave dielectric property is epsilon r ＝5.4，Q f ＝20,000GHz，TCF＝-103ppm/℃(25℃-85℃)。
Example ten:
the method comprises the following steps: weighing 90 mass percent of lithium molybdate powder and 10 mass percent of deionized water, and mixing for 60 minutes.
Step two: and pouring the uniformly mixed powder into a stainless steel mold, putting the mold filled with the sample on a press, pressurizing at 500MPa for 5 minutes, and taking out the massive sample after pressurization.
Step three: and D, putting the blocky sample prepared in the step two into a microwave oven for sintering. The heating rate is 50 ℃/min, the sintering temperature is 200 ℃, and the heat preservation time is 240 minutes.
The performance of the group of ceramic materials reaches the following indexes:
after sintering in air at 200 ℃, the relative density of the sample is about 95 percent, and the microwave dielectric property is epsilon r ＝6.2，Q f ＝30,000GHz，TCF＝-150ppm/℃(25℃-85℃)。
Example eleven:
the method comprises the following steps: weighing 95 mass percent of lithium molybdate powder and 5 mass percent of deionized water, and mixing for 40 minutes.
Step two: pouring the uniformly mixed powder into a stainless steel mold, then putting the mold filled with the sample on a press, pressurizing at 10MPa for 3 minutes, and taking out the massive sample after pressurization.
Step three: and D, putting the blocky sample prepared in the step two into a microwave oven for sintering. The heating rate is 30 ℃/min, the sintering temperature is 150 ℃, and the heat preservation time is 300 minutes.
The performance of the group of ceramic materials reaches the following indexes:
after sintering in air at 150 ℃, the relative density of the sample is about 94 percent, and the microwave dielectric property is epsilon r ＝5.7，Q f ＝24,000GHz，TCF＝-127ppm/℃(25℃-85℃)。
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
It is to be understood that the above description is intended to be illustrative, and not restrictive. Many embodiments and many applications other than the examples provided would be apparent to those of skill in the art upon reading the above description. The scope of the patent should, therefore, be determined not with reference to the above description, but instead should be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled. The disclosures of all articles and references, including patent applications and publications, are hereby incorporated by reference for all purposes. The omission in the foregoing claims of any aspect of subject matter that is disclosed herein is not intended to forego such subject matter, nor should the applicant consider that such subject matter is not considered part of the disclosed subject matter.
Claims (9)
1. A low-carbon preparation method of a microwave dielectric ceramic material based on microwave cold sintering is characterized by comprising the following steps:
the method comprises the following steps: mixing the ceramic and the liquid phase, wherein the mass fraction of the ceramic powder is 50-95% and the balance is the liquid phase;
step two: tabletting the mixture obtained in the first step;
step three: and putting the pressed product into a microwave sintering furnace for sintering, wherein the sintering temperature is 100-1000 ℃, the heating rate is 1-50 ℃/min, and the heat preservation time is 10-300 min, so as to obtain the microwave dielectric ceramic.
2. The microwave cold sintering-based low-carbon preparation method of the microwave dielectric ceramic material as claimed in claim 1, wherein the ceramic in the first step comprises 50-90% by mass of titanium dioxide, and the liquid phase comprises 5-35% by mass of tetrabutyl titanate and 1-20% by mass of deionized water; the sintering temperature in the third step is 900-1000 ℃.
3. The microwave cold sintering-based low-carbon preparation method of the microwave dielectric ceramic material as claimed in claim 2, wherein the titanium dioxide and the tetrabutyl titanate are weighed and mixed, and then deionized water with the mass fraction of 1% -20% is added for full mixing.
4. The microwave dielectric ceramic material low-carbon preparation method based on microwave cold sintering as claimed in claim 1, wherein the ceramic in the first step comprises 80% -95% of MgMoO by mass 4 The sintering temperature in the third step is 700-900 ℃.
5. The microwave cold sintering-based low-carbon preparation method for the microwave dielectric ceramic material as claimed in claim 1, wherein the ceramic in the first step comprises 80-95% by mass of Li 2 MoO 4 And the sintering temperature in the third step is 100-200 ℃.
6. The microwave cold sintering-based low-carbon preparation method of the microwave dielectric ceramic material as claimed in claim 1, wherein in the first step, ceramic powder and liquid phase are mixed.
7. The microwave cold sintering-based low-carbon preparation method of the microwave dielectric ceramic material as claimed in claim 1, wherein during the tabletting process, the pressure range is 10-500MPa, and the pressure-holding time is 1-5 minutes.
8. The microwave cold sintering-based low-carbon preparation method of the microwave dielectric ceramic material as claimed in claim 1, wherein in the second step, the mixture in the first step is placed in a stainless steel mold and then placed on a press for press forming.
9. A microwave dielectric ceramic prepared by the microwave cold sintering-based microwave dielectric ceramic material low-carbon preparation method according to any one of claims 1 to 8.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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