CN104961451A - Bismuth lanthanum ferrite ceramic and preparation method thereof - Google Patents
Bismuth lanthanum ferrite ceramic and preparation method thereof Download PDFInfo
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- CN104961451A CN104961451A CN201510377306.3A CN201510377306A CN104961451A CN 104961451 A CN104961451 A CN 104961451A CN 201510377306 A CN201510377306 A CN 201510377306A CN 104961451 A CN104961451 A CN 104961451A
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Abstract
The invention discloses bismuth lanthanum ferrite ceramic and a preparation method thereof, which is used for solving the technical problem that the existing lanthanum-doped ceramic is low in nonlinearity coefficient. According to the technical scheme, the bismuth lanthanum ferrite ceramic is prepared according to the formula Bi<1-x>LaxFeO3. The preparation method comprises the steps: adjusting the proportion of lanthanum substituting the bismuth ferrite ceramic according to the formula Bi<1-x>Lax FeO3, taking a solid-phase sintering technology to be combined with an atmospheric treatment method, taking bismuth oxide, lanthanum oxide and iron oxide as raw materials, and obtaining the bismuth lanthanum ferrite ceramic with nonlinear volt-ampere characteristic in steps of mixing, ball milling, low-temperature pre-burning, high-temperature sintering and atmosphere treatment. The nonlinearity coefficient of the bismuth lanthanum ferrite ceramic prepared by adopting the method can reach 2.84 and is apparently higher than the nonlinearity coefficient 1.67 of the lanthanum-doping ceramic of the background art.
Description
Technical field
The present invention relates to one and mix lanthanum pottery, particularly relate to a kind of cadmium ferrite bismuth pottery.Also relate to the preparation method of this cadmium ferrite bismuth pottery.
Background technology
Piezoresistive material; it is a kind of resistance device with nonlinear wind vibration; be mainly used in carrying out voltage control when circuit bears overvoltage, the existing aspect such as facility overvoltage protection, voltage stabilizing being widely used in the fields such as electric power, communication, railway, post and telecommunications, chemical industry, oil.Traditional voltage dependent resistor mainly adopts one " binary II-VI race's oxide semiconductor " zinc oxide material manufacture.And in the recent period in novel tertiary perovskite structure pottery as have also discovered nonlinear wind vibration in CaCu 3 Ti 4 O and ferrous acid bismuth-based ceramics, widened the selectable range of piezoresistive material.
Document " Laijun Liu, et al.Dielectric and nonlinear current – voltage characteristics ofrare-earth doped CaCu
3ti4O
12ceramics.Journal of Applied Physics, 2011,110,094101 " report discloses a kind of formula; by mixing a certain amount of rare earth element in calcium copper titanate ceramics; obtain the electronic ceramics with nonlinear wind vibration, but its nonlinear factor α is lower, wherein adopts the nonlinear factor of lanthanum element doped titanic acid copper calcium pottery to be about 1.67.
Summary of the invention
Existingly mixing the low deficiency of lanthanum pottery nonlinear factor to overcome, the invention provides a kind of cadmium ferrite bismuth pottery and preparation method thereof.Cadmium ferrite bismuth pottery of the present invention is according to formula Bi
1-xla
xfeO
3be prepared from.Preparation method is according to formula Bi
1-xla
xfeO
3adjustment lanthanum replaces the proportioning of bismuth ferrite pottery, adopt solid-phase sintering technology in conjunction with atmosphere treatment process, with bismuth oxide, lanthanum trioxide and ferric oxide for raw material, after mixing and ball milling, low temperature presintering, high temperature sintering and atmosphere process, obtain the cadmium ferrite bismuth pottery with nonlinear wind vibration.The cadmium ferrite bismuth pottery nonlinear factor adopting the inventive method to prepare reaches 2.84, is significantly higher than the nonlinear factor 1.67 that background technology mixes lanthanum pottery.
The technical solution adopted for the present invention to solve the technical problems is: a kind of cadmium ferrite bismuth pottery, is characterized according to formula Bi
1-xla
xfeO
3be prepared from; Wherein, x=0 ~ 0.2.
A preparation method for above-mentioned cadmium ferrite bismuth pottery, is characterized in adopting following steps:
Step one, by analytical pure Bi
2o
3, La
2o
3, Fe
2o
3according to stoichiometric ratio Bi
1-xla
xfeO
3weigh and prepare burden, wherein x=0 ~ 0.2;
Step 2, the raw material prepared is put into ball grinder, in zirconia ball: raw material: alcohol is the ratio batch mixing ball milling of 3:1:1, and Ball-milling Time is 4 ~ 8 hours;
Step 3, by ball milling material dry after briquetting, pre-burning 1 ~ 5 hour at 680 ~ 720 DEG C of temperature, take out grind, secondary ball milling 8 ~ 12 hours, then sieves;
Step 4, the powder after sieving is pressed into diameter is in advance 11 ~ 15mm, and thickness is the disk of 1.1 ~ 1.5mm, then at the hydrostatic pressure compacted under of 210 ~ 250MPa;
Step 5, the disk after shaping is incubated 2 ~ 4 hours at 800 ~ 880 DEG C, sinters porcelain into;
Step 6, the cadmium ferrite bismuth ceramic plate sanding and polishing that will prepare, then silver coating slurry, at 510 ~ 550 DEG C, is incubated and burns till silver electrode in 20 ~ 40 minutes.
The invention has the beneficial effects as follows: cadmium ferrite bismuth pottery of the present invention is according to formula Bi
1-xla
xfeO
3be prepared from.Preparation method is according to formula Bi
1-xla
xfeO
3adjustment lanthanum replaces the proportioning of bismuth ferrite pottery, adopt solid-phase sintering technology in conjunction with atmosphere treatment process, with bismuth oxide, lanthanum trioxide and ferric oxide for raw material, after mixing and ball milling, low temperature presintering, high temperature sintering and atmosphere process, obtain the cadmium ferrite bismuth pottery with nonlinear wind vibration.The cadmium ferrite bismuth pottery nonlinear factor adopting the inventive method to prepare reaches 2.84, is significantly higher than the nonlinear factor 1.67 that background technology mixes lanthanum pottery.
Below in conjunction with the drawings and specific embodiments, the present invention is elaborated.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of cadmium ferrite bismuth pottery prepared by the inventive method embodiment 1 ~ 5.
Fig. 2 be under cadmium ferrite bismuth pottery room temperature prepared by the inventive method embodiment 2 ~ 5 electric current with the change curve of impressed voltage.
Fig. 3 is that the electric current of cadmium ferrite bismuth pottery at 25 ~ 150 DEG C of temperature prepared by the inventive method embodiment 2 is with the change curve of impressed voltage.
Fig. 4 is the change curve of electric current with impressed voltage of cadmium ferrite bismuth prepared by the inventive method embodiment 2 ceramic after different partial atmosphere (nitrogen, air, oxygen).
Embodiment
With reference to Fig. 1-4.
Embodiment 1:
1, by ceramic composition chemical formula BiFeO
3proportioning weighs 18.416g Bi
2o
3, 6.284g Fe
2o
3, the raw material weighed up is put into ball grinder;
2, in zirconia ball: raw material: alcohol is the ratio batch mixing ball milling of 3:1:1, and Ball-milling Time is 4 hours;
3, briquetting after being dried by the material mixed, pre-burning 5 hours at 680 DEG C of temperature, takes out the material calcined and grinds, obtain BiFeO
3pre-burning powder, puts into ball grinder secondary ball milling 8 hours, sieves after oven dry;
4, the powder after sieving being pressed into diameter is in advance 11mm, and thickness is the disk of 1.1mm, then final molding under the hydrostatic pressure of 210MPa;
5, the disk after shaping is incubated 4 hours at 800 DEG C, sinters porcelain into;
6, sanding and polishing, then silver coating slurry, at 510 DEG C, insulation burns till silver electrode in 40 minutes.
The phase structure X-ray diffraction spectrum analysis of the ceramics sample of preparation, its INSTRUMENT MODEL is X ' the Pert PRO MPD of PANalytical company, its test result, as Fig. 1 (a), can find out that unadulterated bismuth ferrite pottery (BFO) thing of preparation is pure phase mutually; The current-voltage curve of ceramics sample is tested with ferroelectric analyser, and INSTRUMENT MODEL is TF2000, and test result, as Fig. 2 (a), can find out that the pure bismuth ferrite pottery of preparation does not have obvious nonlinear wind vibration, and leakage current is higher.
Embodiment 2:
With embodiment 1, difference is that in step 1, ceramic composition chemical formula is Bi
0.95la
0.05feO
3, take Bi
2o
3weight 17.997g, takes La
2o
3weight 0.642g, takes Fe
2o
3weight 6.361g; In step 2, Ball-milling Time is 5 hours; In step 3, calcined temperature is 690 DEG C, and burn-in time is 4 hours, and the secondary ball milling time is 9 hours; Being pressed into diameter in step 4 is in advance 12mm, and thickness is the disk of 1.2mm, and hydrostatic pressure is 220MPa; In step 5, sintering temperature is 820 DEG C, and sintering time is 3.5 hours; In step 6, temperature is 520 DEG C, and the time is 35 minutes.
The phase structure X-ray diffraction spectrum analysis of the ceramics sample of preparation, its INSTRUMENT MODEL is X ' the Pert PRO MPD of PANalytical company, and its test result, as Fig. 1 (b), can find out that the cadmium ferrite bismuth pottery thing of preparation is pure phase mutually; The current-voltage curve of ceramics sample is tested with ferroelectric analyser, and INSTRUMENT MODEL is TF2000, and test result, as Fig. 2 (b), can find out the cadmium ferrite bismuth pottery (Bi of doping 5mol% lanthanum
0.95la
0.05feO
3, BLF05) and there is significantly reversible nonlinear wind vibration relative to unadulterated bismuth ferrite pottery, and leakage current has and significantly reduces; (25 ~ 150 DEG C) are tested the current-voltage curve of ceramics sample at different temperatures, and test result, as Fig. 3, can find out the increase along with temperature, and the nonlinear wind vibration of cadmium ferrite bismuth pottery has significantly to be increased; The current-voltage curve of the ceramics sample after different partial atmosphere (nitrogen, air, oxygen) thermal treatment is tested, test result is as Fig. 4, can find out that the nonlinear wind vibration of the cadmium ferrite bismuth pottery through processing test in a nitrogen atmosphere declines to some extent, and the nonlinear wind vibration processing the cadmium ferrite bismuth pottery of test under oxygen atmosphere has and significantly improves, its nonlinear factor α equals 2.84, is much higher than 1.67 of La doped calcium copper titanate ceramics in background technology.
Embodiment 3:
With embodiment 1, difference is that in step 1, ceramic composition chemical formula is Bi
0.90la
0.10feO
3, take Bi
2o
3weight 17.260g, takes La
2o
3weight 1.301g, takes Fe
2o
3weight 6.439g; In step 2, Ball-milling Time is 6 hours; In step 3, calcined temperature is 700 DEG C, and burn-in time is 3 hours, and the secondary ball milling time is 10 hours; Being pressed into diameter in step 4 is in advance 13mm, and thickness is the disk of 1.3mm, and hydrostatic pressure is 230MPa; In step 5, sintering temperature is 840 DEG C, and sintering time is 3 hours; In step 6, temperature is 530 DEG C, and the time is 30 minutes.
The phase structure X-ray diffraction spectrum analysis of the ceramics sample of preparation, its INSTRUMENT MODEL is X ' the Pert PRO MPD of PANalytical company, and its test result, as Fig. 1 (c), can find out that the cadmium ferrite bismuth pottery thing of preparation is pure phase mutually; The current-voltage curve of ceramics sample is tested with ferroelectric analyser, and INSTRUMENT MODEL is TF2000, and test result, as Fig. 2 (c), can find out the cadmium ferrite bismuth pottery (Bi of doping 10mol% lanthanum
0.90la
0.10feO
3, BLF10) relatively unadulterated bismuth ferrite pottery has significantly reversible nonlinear wind vibration, and leakage current has and significantly reduces.
Embodiment 4:
With embodiment 1, difference is that in step 1, ceramic composition chemical formula is Bi
0.85la
0.15feO
3, take Bi
2o
3weight 16.505g, takes La
2o
3weight 1.975g, takes Fe
2o
3weight 6.520g; In step 2, Ball-milling Time is 7 hours; In step 3, calcined temperature is 710 DEG C, and burn-in time is 2 hours, and the secondary ball milling time is 11 hours; Being pressed into diameter in step 4 is in advance 14mm, and thickness is the disk of 1.4mm, and hydrostatic pressure is 240MPa; In step 5, sintering temperature is 860 DEG C, and sintering time is 2.5 hours; In step 6, temperature is 540 DEG C, and the time is 25 minutes.
The phase structure X-ray diffraction spectrum analysis of the ceramics sample of preparation, its INSTRUMENT MODEL is X ' the Pert PRO MPD of PANalytical company, and its test result, as Fig. 1 (d), can find out that the cadmium ferrite bismuth pottery thing of preparation is pure phase mutually; The current-voltage curve of ceramics sample is tested with ferroelectric analyser, and INSTRUMENT MODEL is TF2000, and test result, as Fig. 2 (d), can find out the cadmium ferrite bismuth pottery (Bi of doping 15mol% lanthanum
0.85la
0.15feO
3, BLF15) relatively unadulterated bismuth ferrite pottery has significantly reversible nonlinear wind vibration, and leakage current has and significantly reduces.
Embodiment 5:
With embodiment 1, difference is that in step 1, ceramic composition chemical formula is Bi
0.80la
0.20feO
3, take Bi
2o
3weight 15.731g, takes La
2o
3weight 2.667g, takes Fe
2o
3weight 6.602g; In step 2, Ball-milling Time is 8 hours; In step 3, calcined temperature is 720 DEG C, and burn-in time is 1 hour, and the secondary ball milling time is 12 hours; Being pressed into diameter in step 4 is in advance 15mm, and thickness is the disk of 1.5mm, and hydrostatic pressure is 250MPa; In step 5, sintering temperature is 880 DEG C, and sintering time is 2 hours; In step 6, temperature is 550 DEG C, and the time is 20 minutes.
The phase structure X-ray diffraction spectrum analysis of the ceramics sample of preparation, its INSTRUMENT MODEL is X ' the Pert PRO MPD of PANalytical company, and its test result, as Fig. 1 (e), can find out that the cadmium ferrite bismuth pottery thing of preparation is pure phase mutually; The current-voltage curve of ceramics sample is tested with ferroelectric analyser, and INSTRUMENT MODEL is TF2000, and test result, as Fig. 2 (e), can find out the cadmium ferrite bismuth pottery (Bi of doping 20mol% lanthanum
0.80la
0.20feO
3, BLF20) relatively unadulterated bismuth ferrite pottery has significantly reversible nonlinear wind vibration, and leakage current has and significantly reduces.
The present invention is by the formula of a kind of cadmium ferrite bismuth pottery of design, be specially the bismuth element in lanthanum element part replacement perovskite structure bismuth ferrite pottery, adopt solid-phase sintering technology in conjunction with atmosphere treatment process, with bismuth oxide, lanthanum trioxide and ferric oxide for raw material, after mixing and ball milling, low temperature presintering, high temperature sintering and atmosphere process, prepare a series of cadmium ferrite bismuth pottery with nonlinear wind vibration.The pottery prepared has nonlinear current-voltage reversible preferably, possesses lower leakage current simultaneously, and process stabilizing is ripe.Therefore the cadmium ferrite bismuth series ceramic prepared in the present invention meets the speciality of Non-linear pressure sensitive resistive element, can meet the rheostatic service requirements of voltage dependent resistor.
Claims (2)
1. a cadmium ferrite bismuth pottery, is characterized in that: according to formula Bi
1-xla
xfeO
3be prepared from; Wherein, x=0 ~ 0.2.
2. a preparation method for cadmium ferrite bismuth pottery described in claim 1, is characterized in that comprising the following steps:
Step one, by analytical pure Bi
2o
3, La
2o
3, Fe
2o
3according to stoichiometric ratio Bi
1-xla
xfeO
3weigh and prepare burden, wherein x=0 ~ 0.2;
Step 2, the raw material prepared is put into ball grinder, in zirconia ball: raw material: alcohol is the ratio batch mixing ball milling of 3:1:1, and Ball-milling Time is 4 ~ 8 hours;
Step 3, by ball milling material dry after briquetting, pre-burning 1 ~ 5 hour at 680 ~ 720 DEG C of temperature, take out grind, secondary ball milling 8 ~ 12 hours, then sieves;
Step 4, the powder after sieving is pressed into diameter is in advance 11 ~ 15mm, and thickness is the disk of 1.1 ~ 1.5mm, then at the hydrostatic pressure compacted under of 210 ~ 250MPa;
Step 5, the disk after shaping is incubated 2 ~ 4 hours at 800 ~ 880 DEG C, sinters porcelain into;
Step 6, the cadmium ferrite bismuth ceramic plate sanding and polishing that will prepare, then silver coating slurry, at 510 ~ 550 DEG C, is incubated and burns till silver electrode in 20 ~ 40 minutes.
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CN108947514A (en) * | 2018-09-28 | 2018-12-07 | 东北大学 | A kind of ferroelectric material and the preparation method and application thereof of excellent temperature stability |
CN110498676A (en) * | 2019-09-17 | 2019-11-26 | 江西科技学院 | A kind of nano ceramics and preparation method |
CN110550954A (en) * | 2019-09-18 | 2019-12-10 | 昆明贵研新材料科技有限公司 | Core-shell lanthanum-doped bismuth ferrite/silicon dioxide composite ceramic and preparation method thereof |
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2015
- 2015-07-01 CN CN201510377306.3A patent/CN104961451A/en active Pending
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G. LE BRAS ET AL.: "Effect of La doping in the multiferroic compound BiFeO3", 《PHYSICA B》 * |
G. LE BRAS ET AL.: "Magnetization and magnetoelectric effect in Bi1-xLaxFeO3 (0≤x≤0.15)", 《PHYSICAL REVIEW B》 * |
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CN106745303A (en) * | 2017-02-27 | 2017-05-31 | 陕西科技大学 | A kind of three-dimensional flower ball-shaped cadmium ferrite bismuth meal body and preparation method thereof |
CN107140968A (en) * | 2017-05-11 | 2017-09-08 | 桂林电子科技大学 | A kind of high-temp leadless piezoelectric ceramics and preparation method thereof |
CN107140968B (en) * | 2017-05-11 | 2020-04-17 | 桂林电子科技大学 | High-temperature lead-free piezoelectric ceramic and preparation method thereof |
CN108947514A (en) * | 2018-09-28 | 2018-12-07 | 东北大学 | A kind of ferroelectric material and the preparation method and application thereof of excellent temperature stability |
CN108947514B (en) * | 2018-09-28 | 2020-03-31 | 东北大学 | Ferroelectric material with excellent temperature stability and preparation method and application thereof |
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CN110498676A (en) * | 2019-09-17 | 2019-11-26 | 江西科技学院 | A kind of nano ceramics and preparation method |
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CN113943882A (en) * | 2021-11-15 | 2022-01-18 | 上海海事大学 | Ag/BiFeO3Metal ceramic, preparation method and application thereof |
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Application publication date: 20151007 |