CN105130421A - Ti-position high-valence substituted SrTiO3 giant dielectric ceramic and preparation method thereof - Google Patents
Ti-position high-valence substituted SrTiO3 giant dielectric ceramic and preparation method thereof Download PDFInfo
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- CN105130421A CN105130421A CN201510566377.8A CN201510566377A CN105130421A CN 105130421 A CN105130421 A CN 105130421A CN 201510566377 A CN201510566377 A CN 201510566377A CN 105130421 A CN105130421 A CN 105130421A
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Abstract
The invention relates to a Ti-position high-valence substituted SrTiO3 giant dielectric ceramic material and a preparation method thereof. The ceramic is prepared by substituting high-valence Nb for Ti and expressed in a general formula of SrNbxTi<1-x>O3, wherein x is more than or equal to 0.003 and less than or equal to 0.006. The preparation method comprises the following steps: mixing SrCO3, Nb2O5 and TiO2 according to a stoichiometric ratio of the general formula SrNbxTi<1-x>O3 at 1 to x/2 to (1-x) to obtain a mixture, ball milling the mixture, drying, per-burning at the temperature of 1140 to 1180 DEG C, and secondarily ball milling to obtain pre-burned powder, adding adhesive into the pre-burned powder, granulating, screening, forming, batching out to obtain a ceramic green body, preserving the heat of the ceramic green body in a nitrogen atmosphere at the temperature of 1500 to 1600 DEG C and sintering, and naturally cooling along with the furnace to obtain the giant dielectric ceramic. The prepared Ti-position high-valence-substituted SrTiO3 giant dielectric ceramic is high in dielectric constant, low in dielectric loss, good in electric constant temperature/frequency stability, simple in preparation method, good in repeatability, high in rate of finished product and easy to produce.
Description
Technical field
The invention belongs to dielectric ceramic material technical field, be specifically related to a kind of Ti position high price and replace SrTiO
3base giant dielectric pottery and preparation method thereof.
Background technology
Along with microelectronics market is to practical device miniaturization, integrated, intelligentized demands such as ceramic condenser and microwave-medium components and parts, more and more get more and more people's extensive concerning to the research with the good dielectric ceramic of high-k, low-dielectric loss and temperature/frequency stability, particularly it stores at dynamic random and has a wide range of applications in high dielectric capacitor.At present, high dielectric constant material mainly concentrates on the stupalith of transition metal oxide, rare earth oxide and perovskite structure.The barium titanate series of perovskite structure and lead titanate based material, specific inductivity is greater than 1000 usually, but its high-k is mainly derived from ferroelectric phase transition and nonlinear dielectric phenomenon, because ferroelectrics, at Curie temperature place, the transformation of ferroelectric phase to paraelectric phase occurs, make the specific inductivity of ferroelectric material be subject to the impact of temperature consumingly, thus cause the bad stability of device.And containing environmentally harmful Element Lead in lead system uhligite high dielectric material, volatile during high temperature, be unfavorable for environment protection.Another kind of CaCu
3ti
4o
12(being called for short CCTO) stupalith is one of high dielectric material received publicity in recent years, not only there is high specific inductivity, and specific inductivity can remain unchanged in quite wide temperature range, but, research finds that CCTO material dielectric loss while having high-k is also very high, and being difficult to be widely used in electrical condenser, storer etc. needs in the electron device of high-k.So find and a kind ofly both had high specific inductivity, have again low dielectric loss, the temperature also had and the material of frequency stability just have obvious practical significance.
SrTiO
3it is at room temperature paraelectric phase cubic structure, Curie temperature is very low, phase transformation is not had more than Curie temperature, and temperature stability is fine, compared with CCTO high-permitivity ceramics, the very low and excellent in stability of dielectric loss, can not cause fatigue and problem of aging, receive concern for many years in dielectric ceramic field compared with barium titanate system.
Summary of the invention
A technical problem to be solved by this invention is to provide a kind of huge dielectric constant, the Ti position high price of low-dielectric loss and good temperature stability and frequency stability replaces SrTiO
3giant dielectric stupalith.
Another technical problem to be solved by this invention is to provide a kind of Ti position high price to replace SrTiO
3the preparation method of giant dielectric stupalith.
For solving the problems of the technologies described above the technical solution adopted in the present invention be:
A kind of Ti position high price is provided to replace SrTiO
3giant dielectric stupalith, replaces Ti by Nb high price and obtains, using general formula SrNb
xti
1-xo
3represent, 0.003≤x≤0.006 in formula.
By such scheme, described Ti position high price replaces SrTiO
3giant dielectric stupalith is by SrCO
3, Nb
2o
5, TiO
2by general formula SrNb
xti
1-xo
3stoichiometric ratio 1:x/2:(1-x) ceramic body that is mixed 1500 ~ 1600 DEG C of heat preservation sinterings and obtaining under nitrogen atmosphere.
Above-mentioned Ti position high price replaces SrTiO
3giant dielectric stupalith SrNb
xti
1-xo
3preparation method, by SrCO
3, Nb
2o
5, TiO
2by general formula SrNb
xti
1-xo
3stoichiometric ratio 1:x/2:(1-x) mixing after ball milling, dry, 1140 ~ 1180 DEG C are carried out pre-burning, then secondary ball milling obtains pre-burning powder, pre-burning powder is added binding agent granulation and sieves, shaping, then binder removal obtains ceramic body, again by ceramic body 1500 ~ 1600 DEG C of heat preservation sinterings under nitrogen atmosphere, obtain with stove naturally cooling.
In such scheme, described ball milling is for adding ball-milling medium and dispersion agent, and ball milling, after 20 ~ 30 hours, is separated ball-milling medium, then the raw mixture after ball milling is put into loft drier and dry.
In such scheme, described dispersion agent is dehydrated alcohol, and ball-milling medium is zirconium ball, according to compound: dehydrated alcohol: zirconium ball mass ratio is 1:(4 ~ 5): (10 ~ 14) carry out ball milling.
In such scheme, described bake out temperature 100 ~ 150 DEG C, drying time 10 ~ 15 hours.
In such scheme, described burn-in time is 2 ~ 3 hours.
In such scheme, it is polyvinyl alcohol solution that described granulation sticks with glue agent.
In such scheme, described compression molding is: composite granule is pressed into the disk that diameter is 12mm, thickness 1 ~ 1.5mm under the pressure of 10 ~ 12MPa.
In such scheme, the heat preservation sintering time of described ceramic body is 2.5 ~ 3.5 hours.
In such scheme, before heat preservation sintering, gas washing process is carried out to tube furnace, concrete steps are: vacuumize whole breather line, pass into nitrogen steadily flow out to nitrogen as vacuum tightness≤10Pa, then after repeating to vacuumize logical nitrogen 3 ~ 5 times maintaining nitrogen purge in whole pipeline.
In such scheme, under nitrogen atmosphere, during heat preservation sintering, the circulating rate of nitrogen is 40 ~ 200mL/min.
The invention has the beneficial effects as follows:
The present invention passes through SrTiO
3carry out Ti position trace high valence ion to replace, considerable at the inner quantity of formation of pottery
polarization submanifold group thus fixed electron obtains the SrTiO of huge dielectric constant and low-dielectric loss
3base ceramic material (test specification the temperature range of 25 ~ 250 DEG C, the range of frequency of 0.1 ~ 100kHz).
Ti position provided by the invention high price replaces SrTiO
3giant dielectric ceramic dielectric constant is high, and dielectric loss is low, and electric constant temperature/frequency stability is good, and preparation method is simple, and reproducible, yield rate is high, is easy to produce.When value as x is 0.006, the specific inductivity of stupalith when room temperature under 1kHz is 59191, dielectric loss is 0.03, and specific inductivity changes very little in very wide frequency and temperature range, simultaneously dielectric loss in very wide frequency and temperature range≤0.08.By changing the different doping contents of Nb, the dielectric properties of this material system can be regulated and controled.
For material powder of the present invention, granularity and particle diameter are had no special requirements, therefore can reduce production cost.
Accompanying drawing explanation
Fig. 1 is nitrogen assisted sintering SrNb in the embodiment of the present invention 1
0.003ti
0.997o
3(SNT
0.003) huge dielectric constant stupalith XRD figure spectrum.
Fig. 2 is nitrogen assisted sintering SrNb in the embodiment of the present invention 1
0.003ti
0.997o
3(SNT
0.003) the XPS collection of illustrative plates of Nb element in huge dielectric constant stupalith.
Fig. 3 is nitrogen assisted sintering SrNb in the embodiment of the present invention 1
0.003ti
0.997o
3(SNT
0.003) impedance spectrum of huge dielectric constant stupalith.
Fig. 4 is nitrogen assisted sintering SrNb in the embodiment of the present invention 1
0.003ti
0.997o
3(SNT
0.003) the dielectric thermogram of huge dielectric constant stupalith.In figure (a), four curves are from top to bottom respectively 0.1kHz, dielectric constant with temperature change curve when 1kHz, 10kHz, 100kHz; In figure (b), four curves are from top to bottom respectively 0.1kHz, and when 1kHz, 10kHz, 100kHz, dielectric loss varies with temperature curve.
Fig. 5 is nitrogen assisted sintering SrNb in inventive embodiments 1
0.003ti
0.997o
3(SNT
0.003) the dielectric and magnetic figure of huge dielectric constant stupalith.In figure (a), four curves are from top to bottom respectively 25 DEG C, 100 DEG C, 150 DEG C, and when 200 DEG C, specific inductivity is with frequency variation curve; In figure (b), four curves are from top to bottom respectively 25 DEG C, 100 DEG C, 150 DEG C, and when 200 DEG C, dielectric loss is with frequency variation curve.
Fig. 6 is nitrogen assisted sintering SrTiO in comparative example 1 of the present invention
3the dielectric thermogram of stupalith.In figure (a), four curves are from top to bottom respectively 1kHz, dielectric constant with temperature change curve when 10kHz, 100kHz, 1MHz; In figure (b), four curves are from top to bottom respectively 1kHz, and when 10kHz, 100kHz, 1MHz, dielectric loss varies with temperature curve.
Fig. 7 is nitrogen assisted sintering SrAl in comparative example 2 of the present invention
0.003al
0.997o
3the dielectric thermogram of stupalith.In figure (a), four curves are from top to bottom respectively 1kHz, dielectric constant with temperature change curve when 10kHz, 100kHz, 1MHz; In figure (b), four curves are from top to bottom respectively 1kHz, and when 10kHz, 100kHz, 1MHz, dielectric loss varies with temperature curve.
Fig. 8 is oxygen assisted sintering SrNb in comparative example 4 of the present invention
0.006ti
0.994o
3the dielectric thermogram of stupalith.In figure (a), four curves are from top to bottom respectively 0.1kHz, dielectric constant with temperature change curve when 1kHz, 10kHz, 100kHz; In figure (b), four curves are from top to bottom respectively 0.1kHz, and when 1kHz, 10kHz, 100kHz, dielectric loss varies with temperature curve.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment and accompanying drawing, but content of the present invention is not only confined to the following examples.
Embodiment 1
The present embodiment provides SrNb
0.003ti
0.997o
3(SNT
0.003) represented by the preparation method of stupalith, concrete steps are as follows:
1) oxide composite powder is prepared
By SrNb
0.003ti
0.997o
3(SNT
0.003) stoichiometric ratio to be equipped with raw material compound gross weight be 30g, loaded by raw mixture in ball grinder, add zirconium ball and dehydrated alcohol, the mass ratio of compound, dehydrated alcohol, zirconium ball is 1:4:12.Ball milling is after 24 hours, and separating zirconium ball, puts into loft drier by mixture slurry and dry, and loft drier temperature is set to 100 DEG C and dry 12 hours, and the compound after oven dry manually grinds and to be placed in retort furnace in 1150 DEG C of pre-burnings 2 hours, naturally cools to room temperature.Powder after calcining need carry out secondary ball milling, and mechanical milling process is consistent with primary mechanical milling process.
2) ceramic body is prepared
Pre-burning powder after secondary ball milling need add binding agent to carry out granulation and sieves, and obtains the spherical powder with certain particle size grating.The concrete steps of this process are as follows: use the concentration prepared to be that the polyvinyl alcohol solution of 5% is as binding agent, the ratio adding 2 binding agents according to 1g powder is divided and is ground for three times, and the powder after grinding obtains the spherical powder with certain particle size grating after crossing 80 object sieves.
Take 0.4g granulation powder at every turn, put into mould, obtain through dry-pressing formed the disk that diameter is 12mm, thickness 1 ~ 1.5mm.Ceramic body after shaping need get rid of polyvinyl alcohol colloid before sintering, and the actual temp system of binder removal is as follows: in retort furnace, rise to 600 DEG C according to the temperature rise rate of 1 DEG C/min and be incubated 120min, naturally cooling to room temperature.
3) nitrogen atmosphere assisted sintering
The ceramic body being drained through glue is placed in tube furnace and carries out sintering process, before sintering gas washing is carried out to tube furnace, the detailed process of gas washing is as follows: vacuumize whole breather line, pass into nitrogen as vacuum tightness≤10Pa steadily to flow out to nitrogen with the speed of 100mL/min, then after repeating to vacuumize logical nitrogen 3 times maintaining nitrogen purge in whole pipeline.The actual temp system of sintering is: be first warming up to 1000 DEG C with the temperature rise rate of 5 DEG C/min, be then warming up to 1530 DEG C with the temperature rise rate of 2 DEG C/min and be incubated 3 hours, naturally cooling to room temperature with stove.In the process of whole intensification, insulation and cooling, nitrogen circulates in whole system all the time.
SNT
0.003the XRD figure of ceramics sample as shown in Figure 1.As seen from Figure 1, the SNT of nitrogen atmosphere assisted sintering
0.003ceramics sample is complete cubic perovskite structure, does not occur dephasign, illustrate Nb completely solid solution enter a cube SrTiO
3in crystal.
SNT
0.003in ceramics sample, the XPS spectrum figure of Nb as shown in Figure 2.As seen from Figure 2, the 3d of Nb
5/2with 3d
3/2energy level be 2.8eV, Nb valence state in the material in conjunction with energy difference be+5 valencys.
SNT
0.003the impedance spectrogram of ceramics sample as shown in Figure 3.SNT
0.003shown in the dielectric thermogram 4 of stupalith.SNT
0.003the dielectric and magnetic figure of pottery as shown in Figure 5.As seen from the figure, the SNT of nitrogen atmosphere assisted sintering
0.003ceramics sample within the scope of 25 ~ 200 DEG C, in the range of frequency of 0.1 ~ 100kHz, specific inductivity >10
4dielectric loss≤0.08 simultaneously, the specific inductivity wherein when room temperature (25 DEG C) under 1kHz is 39920, and dielectric loss is 0.04.
Embodiment 2
The present embodiment provides SrNb
0.006ti
0.994o
3(SNT
0.006) represented by the preparation method of stupalith, except following difference, all the other steps are identical with embodiment 1:
Step 1 in embodiment 1) in, by SrNb
0.006ti
0.994o
3(SNT
0.006) stoichiometric ratio to be equipped with raw material compound gross weight be 30g.During wet ball-milling, the mass ratio of compound, dehydrated alcohol, zirconium ball is 1:4.5:10, ball milling is after 30 hours, separating zirconium ball, mixture slurry is put into loft drier dry, loft drier temperature is set to 100 DEG C and dry 15 hours, compound after oven dry manually grinds and to be placed in retort furnace in 1180 DEG C of pre-burnings 2.5 hours, naturally cools to room temperature.
Step 3 in embodiment 1) in, in the gas scrubbing before carrying out nitrogen assisted sintering, repeat to vacuumize logical nitrogen continuously and continue afterwards for 5 times to lead to nitrogen in whole pipeline with the speed of 200mL/min.In the process of whole intensification, insulation and cooling, nitrogen circulates in whole system all the time.Sintering temperature is set to 1550 DEG C and is incubated 2.5 hours.
The SNT of preparation
0.006ceramics sample, has huge dielectric constant and low-dielectric loss, and the specific inductivity 25 DEG C time under 1kHz and dielectric loss are respectively 59191 and 0.03.
Embodiment 3
The present embodiment provides SrNb
0.003ti
0.997o
3(SNT
0.003) represented by the preparation method of stupalith, except following difference, all the other steps are identical with embodiment 1:
Step 1 in embodiment 1) in, during wet ball-milling, the mass ratio of mixture, dehydrated alcohol, zirconium ball is 1:5:14, and ball milling is after 20 hours, separating zirconium ball, then mixture slurry is put into loft drier to dry, loft drier temperature is set to 150 DEG C and dry 10 hours.Compound after oven dry manually grinds to be placed in retort furnace and calcines 2 hours in 1150 DEG C, naturally cools to room temperature.
Step 3 in embodiment 1) in, in gas scrubbing before carrying out nitrogen assisted sintering, repeat to vacuumize logical nitrogen continuously to continue afterwards for 5 times to lead to nitrogen in whole pipeline with the speed of 60mL/min, in the process of whole intensification, insulation and cooling, nitrogen circulates in whole system all the time, 1600 DEG C of insulations 3 hours during sintering.
The SNT of preparation
0.003pottery has huge dielectric constant (>10
4) and low-dielectric loss (≤0.08).
Comparative example 1
By SrCO
3and TiO
2according to SrTiO
3stoichiometric ratio proportioning mixing, take dehydrated alcohol as dispersion agent, by wet ball-milling method mixing and ball milling 24 hours post-dryings, then in 1150 DEG C of air atmospheres calcine 2 hours.Powder after calcining, through the secondary ball milling process post-drying of 24 hours, adds 5% polyvinyl alcohol solution granulation and sieves.Through dry-pressing formed obtained diameter be 12mm, thickness is the ceramic body of 1 ~ 1.5mm.By its in nitrogen atmosphere 1530 DEG C insulation 3 hours, obtain sinter SrTiO
3stupalith, in whole preparation process, NM part is all identical with the condition of embodiment 1.To the SrTiO of preparation
3pottery carries out dielectric properties test, and its dielectric temperature spectrum as shown in Figure 6, is obtained by figure: 25 DEG C, under 1kHz condition, its specific inductivity and dielectric loss are respectively 305 and 0.003, dielectric properties are starkly lower than Nb of the present invention and adulterate SrTiO
3giant dielectric stupalith.
Comparative example 2
By SrCO
3, Al
2o
3, TiO
2according to SrAl
0.003ti
0.997o
3stoichiometric ratio proportioning mixing, take dehydrated alcohol as dispersion agent, by wet ball-milling method mixing and ball milling 24 hours post-dryings, then in 1150 DEG C of air atmospheres calcine 2 hours.Powder after calcining, through the secondary ball milling process post-drying of 24 hours, adds 5% polyvinyl alcohol solution granulation and sieves.Through dry-pressing formed obtained diameter be 12mm, thickness is the ceramic body of 1 ~ 1.5mm.By its in nitrogen atmosphere 1530 DEG C sintering 3 hours, obtain sinter SrAl
0.003ti
0.997o
3stupalith, in whole preparation process, NM part is all identical with the condition of embodiment 1.To the SrAl of preparation
0.003ti
0.997o
3pottery carries out dielectric properties test, and its dielectric temperature spectrum as shown in Figure 7, is obtained by figure: 25 DEG C, under 1kHz condition, its specific inductivity and dielectric loss are respectively 298 and 0.001, specific inductivity is starkly lower than Nb of the present invention and adulterates SrTiO
3giant dielectric stupalith.
Comparative example 3
By SrCO
3, Nb
2o
3, TiO
2according to SrNb
0.003ti
0.997o
3stoichiometric ratio proportioning mixing, take dehydrated alcohol as dispersion agent, by wet ball-milling method mixing and ball milling 24 hours post-dryings, then in 1150 DEG C of air atmospheres calcine 2 hours.Powder after calcining, through the secondary ball milling process post-drying of 24 hours, adds 5% polyvinyl alcohol solution granulation and sieves.Through dry-pressing formed obtained diameter be 12mm, thickness is the ceramic body of 1 ~ 1.5mm.By its in oxygen atmosphere 1530 DEG C insulation 3 hours, the SrNb sintered under obtaining oxygen atmosphere
0.003ti
0.997o
3stupalith, in whole preparation process, NM part is all identical with the condition of embodiment 1.To the SrNb of preparation
0.003ti
0.997o
3pottery carries out dielectric properties test, obtains: 25 DEG C, under 1kHz condition, its specific inductivity and dielectric loss are respectively 11397 and 0.03, specific inductivity is starkly lower than Nb of the present invention and adulterates SrTiO
3giant dielectric stupalith.
Comparative example 4
By SrCO
3, Nb
2o
3, TiO
2according to SrNb
0.006ti
0.994o
3stoichiometric ratio proportioning mixing, take dehydrated alcohol as dispersion agent, by wet ball-milling method mixing and ball milling 24 hours post-dryings, then in 1150 DEG C of air atmospheres calcine 2 hours.Powder after calcining, through the secondary ball milling process post-drying of 24 hours, adds 5% polyvinyl alcohol solution granulation and sieves.Through dry-pressing formed obtained diameter be 12mm, thickness is the ceramic body of 1 ~ 1.5mm.By its in oxygen atmosphere 1530 DEG C sintering 3 hours, obtain SrNb
0.006ti
0.994o
3stupalith.And dielectric properties test is carried out to it, its dielectric temperature spectrum as shown in Figure 8, is obtained by figure: 25 DEG C, under 1kHz condition, its specific inductivity and dielectric loss are respectively 9069 and 0.12, specific inductivity is starkly lower than Nb of the present invention and adulterates SrTiO
3giant dielectric stupalith, dielectric loss is apparently higher than Nb doping SrTiO of the present invention
3giant dielectric stupalith.
Whether the present invention is by adulterating, and adopt different components doping, adopt which kind of calcination atmosphere, the stupalith of preparation has carried out the investigation of electrical property, experimental result contrast shows: under Nb nitrogen doped atmosphere of the present invention, sintering can obtain the ceramics sample of dielectric properties excellence, the stupalith that its specific inductivity sinters in air or oxygen, dielectric loss is lower than the stupalith sintered in air or oxygen.
Claims (10)
1. a Ti position high price replaces SrTiO
3giant dielectric stupalith, is characterized in that: replace Ti by Nb high price and obtain, using general formula SrNb
xti
1-xo
3represent, 0.003≤x≤0.006 in formula.
2. Ti position according to claim 1 high price replaces SrTiO
3giant dielectric stupalith, is characterized in that: described Ti position high price replaces SrTiO
3giant dielectric stupalith is by SrCO
3, Nb
2o
5, TiO
2by general formula SrNb
xti
1-xo
3stoichiometric ratio 1:x/2:(1-x) ceramic body that is mixed 1500 ~ 1600 DEG C of heat preservation sinterings and obtaining under nitrogen atmosphere.
3. Ti position according to claim 1 high price replaces SrTiO
3the preparation method of giant dielectric stupalith, is characterized in that: by SrCO
3, Nb
2o
5, TiO
2by general formula SrNb
xti
1-xo
3stoichiometric ratio 1:x/2:(1-x) mixing after ball milling, dry, 1140 ~ 1180 DEG C are carried out pre-burning, then secondary ball milling obtains pre-burning powder, pre-burning powder is added tackiness agent granulation and sieves, shaping, then binder removal obtains ceramic body, again by ceramic body 1500 ~ 1600 DEG C of heat preservation sinterings under nitrogen atmosphere, obtain with stove naturally cooling.
4. Ti position according to claim 3 high price replaces SrTiO
3the preparation method of giant dielectric stupalith, is characterized in that: described ball milling is for adding ball-milling medium and dispersion agent, and ball milling is after 20 ~ 30 hours, and separating zirconium ball, then puts into loft drier by the raw mixture after ball milling and dry.
5. Ti position according to claim 4 high price replaces SrTiO
3the preparation method of giant dielectric stupalith, is characterized in that: described dispersion agent is dehydrated alcohol, and ball-milling medium is zirconium ball, according to compound: dehydrated alcohol: zirconium ball mass ratio is 1:(4 ~ 5): (10 ~ 14) carry out ball milling.
6. Ti position according to claim 3 high price replaces SrTiO
3the preparation method of giant dielectric stupalith, is characterized in that: described bake out temperature 100 ~ 150 DEG C, drying time 10 ~ 15 hours; It is polyvinyl alcohol solution that described granulation sticks with glue agent; Described compression molding is: composite granule is pressed into the disk that diameter is 12mm, thickness 1 ~ 1.5mm under the pressure of 10 ~ 12MPa.
7. Ti position according to claim 3 high price replaces SrTiO
3the preparation method of giant dielectric stupalith, is characterized in that: described burn-in time is 2 ~ 3 hours.
8. Ti position according to claim 3 high price replaces SrTiO
3the preparation method of giant dielectric stupalith, is characterized in that: the heat preservation sintering time of described ceramic body is 2.5 ~ 3.5 hours.
9. Ti position according to claim 3 high price replaces SrTiO
3the preparation method of giant dielectric stupalith, it is characterized in that: before heat preservation sintering, gas washing process is carried out to tube furnace, concrete steps are: vacuumize whole breather line, pass into nitrogen as vacuum tightness≤10Pa steadily to flow out to nitrogen, then after repeating to vacuumize logical nitrogen 3 ~ 5 times maintaining nitrogen purge in whole pipeline.
10. Ti position according to claim 3 high price replaces SrTiO
3the preparation method of giant dielectric stupalith, is characterized in that: when being incubated under nitrogen atmosphere, the circulating rate of nitrogen is 40 ~ 200mL/min.
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| CN107500756A (en) * | 2017-09-13 | 2017-12-22 | 武汉理工大学 | A kind of high-k low-loss SrTiO3Based dielectric material and preparation method thereof |
| CN108191428A (en) * | 2018-02-02 | 2018-06-22 | 天津大学 | It is a kind of to prepare SrTiO3The method of base huge dielectric constant medium ceramic material |
| CN108275995A (en) * | 2018-01-24 | 2018-07-13 | 天津大学 | A kind of promotion SrTiO3The method of base huge dielectric constant dielectric substance dielectric constant |
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| CN108275995A (en) * | 2018-01-24 | 2018-07-13 | 天津大学 | A kind of promotion SrTiO3The method of base huge dielectric constant dielectric substance dielectric constant |
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