CN109678495A - A kind of BaTiO3-Sr2CoMoO6Magnetoelectric ceramic and preparation method thereof - Google Patents
A kind of BaTiO3-Sr2CoMoO6Magnetoelectric ceramic and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000000919 ceramic Substances 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 26
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 19
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims abstract description 11
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract 2
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims abstract 2
- 239000000126 substance Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 3
- 238000000748 compression moulding Methods 0.000 claims 3
- 239000003960 organic solvent Substances 0.000 claims 2
- 238000002791 soaking Methods 0.000 claims 1
- 230000005291 magnetic effect Effects 0.000 abstract description 13
- 239000011812 mixed powder Substances 0.000 abstract description 10
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract 1
- 238000009702 powder compression Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 230000005621 ferroelectricity Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007775 ferroic material Substances 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 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
- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
- C04B35/465—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
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Abstract
The invention discloses a kind of BaTiO3‑Sr2CoMoO6Magnetoelectric ceramic.The ceramics the preparation method comprises the following steps: taking analytically pure BaCO3And TiO2Ball milling after preparation is dried, sieving, briquetting, and pre-burning obtains BaTiO after crushing3Powder；Take analytically pure SrCO3,Co2O3,MoO3Ball milling after preparation is dried, sieving, briquetting, and pre-burning obtains Sr after crushing2CoMoO6Powder.By BaTiO3With Sr2CoMoO6It is uniformly mixed to obtain mixed powder.By mixed-powder compression moulding as needed, magnetoelectric composite ceramic material, and the dielectric constant and preferable magnetic dielectric coefficient that composite ceramic material obtained is with higher is made in sintering under conditions of 1250-1290 DEG C.
Description
Technical field
The invention belongs to materials science fields, and in particular to a kind of preparation of BaTiO3-Sr2CoMoO6 magnetoelectric ceramic
Method.
Background technique
Multi-ferroic material has important scientific research meaning and broad application prospect, it includes ferromagnetics, ferroelectricity
Many problem in science such as, iron bullet, are related to transition group metallic oxide, ABO3The strong related system of perovskite structure, tool
Have a materials such as ferromagnetic ferromagnetism functive, the spin order of material internal, charge order, track orderly, quantum regulation and control and
The Issues On Multi-scales such as farmland engineering science are also particularly important.Multi-ferroic material not only has various single iron, and each iron
Property between some new functions can be generated by collaboration coupling, realize the effect that one-plus-one is greater than two, widened multiferroic significantly
The application range of material makes ferroelectric-ferromagnetic composite material in phase shifter, Spin Valve, polymorphic memory cell, ultra-high-tension power transmission line
The fields such as circuit measuring, energy conversion system, broadband magnetic detection, alternating current-direct current magnetic field sensor, information storage have extensive
Application value, thus the research of ferroelectric-ferromagnetic composite material increasingly causes the attention of domestic and international researchers.In numerous nothings
In lead piezoelectric material, BaTiO3It is important ferroelectricity, piezoceramic material, there is excellent ferroelectricity, piezoelectric property.Compared to it
His material there are sintering temperatures in terms of sample preparation it is high, sintering warm area is narrow the problems such as, BaTiO3The preparation process of material is opposite
Simply.The Sr of structure of double perovskite2CoMoO6Always without being mutually investigated as the magnetism in magnetic electric compound material, there is scholar
It is found by first-principles calculations, in BaTiO3/Sr2CoMoO6Hetero-junctions in, BaTiO3Presence can change Sr2CoMoO6
The orbit occupancy rate of middle Co atom 3d track, to make Sr2CoMoO6It is changed into semimetal state from antiferromagnetic state.At present about
BaTiO3/Sr2CoMoO6It is not recorded in the document of the preparation of composite ceramics at home and abroad.
Summary of the invention
Technical problem to be solved by the present invention lies in provide a kind of process stabilizing and product has good magnetic electricity performance
BaTiO3/Sr2CoMoO6The preparation method of compound magnetoelectric ceramics, the BaTiO that this preparation method obtains3/Sr2CoMoO6Composite ceramics
Dielectric constant with higher and preferable magnetic dielectric coefficient.
The present invention provides a kind of BaTiO3-Sr2CoMoO6Magnetoelectric composite ceramic material and preparation method thereof, it is characterised in that
The following steps are included:
Step 1: firstly, according to chemical general formula BaTiO3Take analytically pure BaCO3And TiO2Ball milling 6 hours, then dry after preparation
It is dry, sieving, briquetting, through 1150 DEG C pre-burning 3 hours, gained bulk sample is smashed it through into 120 meshes and obtains BaTiO3Powder；
Step 2: secondly, pressing chemical general formula Sr2CoMoO6, take the pure SrCO of analysis3,Co2O3,MoO3Ball milling 6 hours after preparation, so
After dry, grind, briquetting, through 750 DEG C pre-burning 3 hours, will gained bulk sample crush after carry out secondary ball milling, then dry,
Grinding, briquetting, through 850 DEG C of pre-burning 3 hours again, will gained bulk sample crush after grind, briquetting, finally in 1250 DEG C of condition
Lower heat preservation 10 hours, finally smashes it through 120 meshes for gained bulk sample and obtains Sr2CoMoO6Powder.
Step 3: according to (1-x) BaTiO3-xSr2CoMoO6Molar ratio by BaTiO3Powder and Sr2CoMoO6Powder is mixed
Uniform mixed powder is closed,x≤0.20；
Step 4: crossing 120 meshes for gained mixed powder, is then pressed into small sheet block, and sintering obtains BaTiO3-
Sr2CoMoO6Magnetoelectric ceramic.
BaTiO in the present invention3-Sr2CoMoO6The sintering temperature of magnetoelectric composite ceramic material is 1250-1290 DEG C.When heat preservation
Between be 2-5 hours.
BaTiO in the present invention3-Sr2CoMoO6Magnetoelectric composite ceramic material dielectric constant with higher and preferable magnetic are situated between
Electrical property.
Detailed description of the invention
Fig. 1 BaTiO3The X-ray diffractogram of powder.
Fig. 2 Sr2CoMoO6The X-ray diffractogram of powder.
Fig. 3 (1-x) BaTiO3-xSr2CoMoO6Magnetoelectric composite ceramic material dielectric constant and dielectric loss change with frequency
Figure.
Fig. 4 0.90BaTiO3-0.10Sr2CoMoO6The magnetic dielectric figure of magnetoelectric composite ceramic material.
Fig. 5 0.85BaTiO3-0.15Sr2CoMoO6The magnetic dielectric figure of magnetoelectric composite ceramic material.
Fig. 6 0.80BaTiO3-0.20Sr2CoMoO6The magnetic dielectric figure of magnetoelectric composite ceramic material.
Specific embodiment
Now in conjunction with example, attached drawing, the present invention will be further described:
Implementation column 1
1) firstly, according to chemical general formula BaTiO3Take analytically pure BaCO3And TiO2Ball milling 6 hours, are then dried after preparation, mistake
Sieve, briquetting, through 1150 DEG C pre-burning 3 hours, gained bulk sample is smashed it through into 120 meshes and obtains BaTiO3Powder；
2) secondly, pressing chemical general formula Sr2CoMoO6, take the pure SrCO of analysis3,Co2O3,MoO3Ball milling 6 hours, then dry after preparation
It is dry, grinding, briquetting, through 750 DEG C pre-burning 3 hours, will gained bulk sample crush after carry out secondary ball milling, then dry, grind,
Briquetting, through 850 DEG C of pre-burning 3 hours again, will gained bulk sample crush after grind, briquetting is finally protected under conditions of 1250 DEG C
Temperature 10 hours, finally smashes it through 120 meshes for gained bulk sample and obtains Sr2CoMoO6Powder.
3) according to 0.90BaTiO3-0.10Sr2CoMoO6Molar ratio by BaTiO3Powder and Sr2CoMoO6Powder mixing ball
Mill obtains uniform mixed powder for 6 hours.
4) gained mixed powder is crossed into 120 meshes, is then pressed into small sheet block, is arrived with the heating rate of 5 DEG C/min
1270 DEG C keep the temperature three hours, then drop to 500 DEG C with the rate of temperature fall of 5 DEG C/min and obtain 0.90BaTiO3-0.10Sr2CoMoO6Magnetic
Electric composite ceramics.
Implementation column 2
1) firstly, according to chemical general formula BaTiO3Take analytically pure BaCO3And TiO2Ball milling 6 hours, are then dried after preparation, mistake
Sieve, briquetting, through 1150 DEG C pre-burning 3 hours, gained bulk sample is smashed it through into 120 meshes and obtains BaTiO3Powder；
2) secondly, pressing chemical general formula Sr2CoMoO6, take the pure SrCO of analysis3,Co2O3,MoO3Ball milling 6 hours, then dry after preparation
It is dry, grinding, briquetting, through 750 DEG C pre-burning 3 hours, will gained bulk sample crush after carry out secondary ball milling, then dry, grind,
Briquetting, through 850 DEG C of pre-burning 3 hours again, will gained bulk sample crush after grind, briquetting is finally protected under conditions of 1250 DEG C
Temperature 10 hours, finally smashes it through 120 meshes for gained bulk sample and obtains Sr2CoMoO6Powder.
3) according to 0.85BaTiO3-0.15Sr2CoMoO6Molar ratio by BaTiO3Powder and Sr2CoMoO6Powder mixing ball
Mill obtains uniform mixed powder for 6 hours.
4) gained mixed powder is crossed into 120 meshes, is then pressed into small sheet block, is arrived with the heating rate of 5 DEG C/min
1280 DEG C keep the temperature three hours, then drop to 500 DEG C with the rate of temperature fall of 5 DEG C/min and obtain 0.85BaTiO3-0.15Sr2CoMoO6Magnetic
Electric composite ceramics.
Implementation column 3
1) firstly, according to chemical general formula BaTiO3Take analytically pure BaCO3And TiO2Ball milling 6 hours, are then dried after preparation, mistake
Sieve, briquetting, through 1150 DEG C pre-burning 3 hours, gained bulk sample is smashed it through into 120 meshes and obtains BaTiO3Powder；
2) secondly, pressing chemical general formula Sr2CoMoO6, take the pure SrCO of analysis3,Co2O3,MoO3Ball milling 6 hours, then dry after preparation
It is dry, grinding, briquetting, through 750 DEG C pre-burning 3 hours, will gained bulk sample crush after carry out secondary ball milling, then dry, grind,
Briquetting, through 850 DEG C of pre-burning 3 hours again, will gained bulk sample crush after grind, briquetting is finally protected under conditions of 1250 DEG C
Temperature 10 hours, finally smashes it through 120 meshes for gained bulk sample and obtains Sr2CoMoO6Powder.
3) according to 0.80BaTiO3-0.20Sr2CoMoO6Molar ratio by BaTiO3Powder and Sr2CoMoO6Powder mixing ball
Mill obtains uniform mixed powder for 6 hours.
4) gained mixed powder is crossed into 120 meshes, is then pressed into small sheet block, is arrived with the heating rate of 5 DEG C/min
1290 DEG C keep the temperature three hours, then drop to 500 DEG C with the rate of temperature fall of 5 DEG C/min and obtain 0.95BaTiO3-0.05Sr2CoMoO6Magnetic
Electric composite ceramics.
From Fig. 1 Fig. 2 it will be seen that the BaTiO of synthesis3And Sr2CoMoO6Powder is all relatively pure.From Fig. 3 frequency sweep figure
In spectrum it may be seen that with Sr2CoMoO6The raising of content is added, the dielectric constant of sample is gradually increased, dielectric loss
With Sr2CoMoO6It adds the raising of content and increases.Fig. 4 Fig. 5 Fig. 6 is Sr respectively2CoMoO6Addition content is 0.10,0.15,
The magnetic dielectric map of 0.20 sample, all samples are all as the increase magnetic dielectric coefficient of magnetic field strength is gradually increased.
Claims (10)
1. a kind of BaTiO3-Sr2CoMoO6Magnetoelectric composite ceramic material, which is characterized in that chemical formula is (1-x) BaTiO3-xSr2CoMoO6,x≤0.20。
2. a kind of BaTiO3-Sr2CoMoO6The preparation method of magnetoelectric composite ceramic material, which comprises the following steps:
According to (1-x) BaTiO3-xSr2CoMoO6Molar ratio by BaTiO3Powder and Sr2CoMoO6Powder is uniformly mixed to obtain mixing
Powder, sieving, compression moulding, sintering obtain BaTiO3-Sr2CoMoO6Magnetoelectric ceramic.
3. a kind of BaTiO according to claim 23-Sr2CoMoO6The preparation method of magnetoelectric composite ceramic material, feature
It is, by BaTiO3Powder and Sr2CoMoO6Powder carries out ball milling in enough organic solvents, and Ball-milling Time 12-24 hours.
4. a kind of BaTiO according to claim 33-Sr2CoMoO6The preparation method of magnetoelectric composite ceramic material, feature
It is, the organic solvent is absolute alcohol or industrial alcohol.
5. a kind of BaTiO according to claim 23-Sr2CoMoO6The preparation method of magnetoelectric composite ceramic material, feature
It is, the sieve mesh number of the sieving is 120 mesh.
6. a kind of BaTiO according to claim 23-Sr2CoMoO6The preparation method of magnetoelectric composite ceramic material, feature
It is, the compression moulding uses isostatic cool pressing technique, and the pressure applied is 120Mpa-200Mpa.
7. a kind of BaTiO according to claim 23-Sr2CoMoO6The preparation method of magnetoelectric composite ceramic material, feature
It is, the sintering temperature is 1250-1290 DEG C；Soaking time is 2-5 hours.
8. a kind of BaTiO according to claim 23-Sr2CoMoO6The preparation method of magnetoelectric composite ceramic material, feature
It is, the compression moulding uses isostatic cool pressing technique, and the pressure applied is 120Mpa-200Mpa.
9. a kind of BaTiO according to claim 23-Sr2CoMoO6The preparation method of magnetoelectric composite ceramic material, feature
It is, the powder is obtained by method comprising the following steps: takes analytically pure BaCO according to chemical general formula3、TiO2, after preparation
Abundant ball milling, then dry, be sieved, briquetting, through 1150 DEG C pre-burning 3 hours, gained bulk sample grinding and sieving is obtained into powder
Body.
10. a kind of BaTiO according to claim 23-Sr2CoMoO6The preparation method of magnetoelectric composite ceramic material, it is special
Sign is, the Sr2CoMoO6Powder is obtained by method comprising the following steps: by chemical general formula Sr2CoMoO6Take analysis pure
SrCO3、Co2O3And MoO3, abundant ball milling after preparation, then dry, grind, briquetting, through 750 DEG C pre-burning 3 hours；By gained block
Secondary ball milling is carried out after shape sample comminution, is then dried, is ground, briquetting, through 850 DEG C of pre-burning 3 hours again；By gained bulk sample
It is ground after crushing, briquetting, finally keeps the temperature 10 hours under conditions of 1250 DEG C；Finally gained bulk sample grinding and sieving is obtained
To Sr2CoMoO6Powder.
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