CN102757232A - Preparation method of lead magnesio-niobate-lead titanate ceramic - Google Patents

Preparation method of lead magnesio-niobate-lead titanate ceramic Download PDF

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CN102757232A
CN102757232A CN2012102472421A CN201210247242A CN102757232A CN 102757232 A CN102757232 A CN 102757232A CN 2012102472421 A CN2012102472421 A CN 2012102472421A CN 201210247242 A CN201210247242 A CN 201210247242A CN 102757232 A CN102757232 A CN 102757232A
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powder
lead
pmn
niobate
ball
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樊慧庆
彭彪林
李强
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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Abstract

The invention discloses a preparation method of lead magnesio-niobate-lead titanate ceramic for solving the technical problem that dielectric loss of the lead magnesio-niobate-lead titanate ceramic prepared by the conventional method is large. The technical scheme is that: weighing and dosing analytically pure MgO (magnesium oxide), Nb2O5 (niobium oxide), PbO (lead oxide) and TiO2 (titanium dioxide) according to the chemical metering ratio (1-x)Pb(Mgl/3Nb2/3)O3-xPbTiO3 (x is smaller than or equal to 0.07 and greater than or equal to 0.01); drying and pressing the materials into blocks after ball-milling, crushing the materials to obtain MgNb2O6 (magnesium niobium oxide) powder; adding TiO2 and PbO to MgNb2O6 powder and then ball-milling, and obtaining PMN-PT (lead magnesium niobate) powder by pressing and burning the material into large blocks; sieving and pre-pressing the PMN-PT powder into wafer, and carrying out isostatic pressing pressure molding; and carrying out heat preservation for 1-4 hours on the molded wafer at 1175-1250 DEG C, and then sintering the molded wafer into ceramic. Two systems are composited together, so that the prepared lead magnesio-niobate-lead titanate ceramic has combination properties of two different systems of lead magnesio and niobate-lead titanate, and has high dielectric constant under the condition that the temperature is 300K same as that of a background technology, meanwhile, lower dielectric loss and higher dielectric tenability are respectively kept at 0.007-0.011 and 63-87% at the same time.

Description

The preparation method of PMN-PT pottery
Technical field
The present invention relates to a kind of preparation method of lead titanate ceramics, particularly relate to a kind of preparation method of PMN-PT pottery.
Background technology
Most of researchist concentrates on and studies Ba xSr 1-xTiO 3, (Sr, Pb) TiO 3, Ba (Zr, Ti) O 3Or (Ba, Sn) TiO 3Etc. system, but because the problem of technology and proportioning aspect, the dielectric loss of these materials and dielectric tuning rate can not satisfy the user demand of instrument simultaneously.
Document " R.Wongmaneerung.R.Yimnirun.S.Ananta.Fabrication and characterization of perovskite ferroelectrric PMN/PT ceramic nanocomposites.J Mater Sci (2009) 44:5428-5440 " discloses a kind of preparation method of PMN-PT pottery; Document has prepared the PMN-PT pottery with traditional ceramic preparation; With the preparatory synthetic method of secondary at 300K; The PMN-PT pottery for preparing under the condition of 1KHz; Though obtained higher dielectric constant (～2000), the dielectric loss of gained (～0.03) is bigger.
Summary of the invention
In order to overcome the big deficiency of PMN-PT ceramic dielectric loss of existing method preparation, the present invention provides a kind of preparation method of PMN-PT pottery.This method is through optimizing the proportioning of lead titanate ceramics, rationally the control pottery synthetic in advance with the agglomerating temperature, can obtain that specific inductivity is higher, dielectric loss is low and the higher stupalith of tuning rate.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of PMN-PT pottery is characterized in may further comprise the steps:
(a) with analytical pure MgO, Nb 2O 5, PbO and TiO 2, according to stoichiometric ratio (1-x) Pb (Mg 1/3Nb 2/3) O 3-xPbTiO 3(0.01≤x≤0.07) weighing and batching;
(b) batching is put into ball grinder, in zirconia ball: batching: alcohol is the ratio batch mixing ball milling of 3:1:1, and the ball milling time is 2-5 hour;
(c) with batch mixing oven dry back briquetting, carry out synthesizing in advance, obtain MgNb 1000-1300 ℃ of temperature 2O 6Powder;
(d) again according to stoichiometric ratio (1-x) Pb (Mg 1/3Nb 2/3) O 3-xPbTiO 3(0.01≤x≤0.07) is weighing TiO respectively 2Add MgNb with PbO through pre-burning 2O 6In the powder;
(e) will be that the powder that step (d) prepares is put into ball grinder, ball milling 4-10 hour again, sieve after the oven dry;
(f) will pass through step (e) and press bulk in the material oven dry back of ball milling again, obtain the PMN-PT powder at 900-1200 ℃ of temperature lower calcination 2-8 hour;
(g) the PMN-PT powder that step (f) is obtained sieves, and to become diameter be 10-12mm in the back precompressed, and thickness is the disk of 1-1.2mm, then at the hydrostatic pressure compacted under of 200-300MPa;
(h) disk after the moulding is incubated 1-4 hour down at 1175-1250 ℃, sinters porcelain into, the silver coated slurry under 500-550 ℃, is incubated 20-30 minute and burns till silver electrode behind the economy-combat grinding and polishing light.
The invention has the beneficial effects as follows: because single lead magnesio-niobate ceramics specific inductivity is not high; The characteristics of the comprehensive two kinds of different systems of the present invention; Two kinds of systems are combined with each other, and the PMN-PT pottery of preparation has the over-all properties of these two kinds of different systems of lead magnoniobate and lead titanate.Under the temperature identical (300K), higher dielectric constant is arranged, dielectric loss (0.007～0.011) that maintenance simultaneously is lower and higher tuning rate (63%～87%) with the background technology temperature.
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the prepared PMN-PT pottery of four embodiment of the inventive method.
Fig. 2 is the inventive method embodiment 3 prepared PMN-PT potteries, the temperature variant relation curve of specific inductivity and dielectric loss under different frequency.
Fig. 3 is the inventive method embodiment 3 prepared PMN-PT potteries, and tuning rate is with the variation relation of extra electric field under different frequency.
Embodiment
Following examples are with reference to Fig. 1～3.
Embodiment 1, during x=0.01, and by stoichiometric ratio weighing 0.8125g MgO, 5.3994g Nb 2O 5, the material that weighs up is put into ball grinder, in zirconia ball: material: alcohol is the ratio batch mixing ball milling of 3:1:1, and the ball milling time is 2 hours; Material oven dry back briquetting with mixing carries out synthesizing in advance under 1000 ℃ of temperature, takes out the good material of calcining and grinds, and obtains niobic acid magnesium pre-burning powder, again with niobic acid magnesium powder and 13.7389g PbO and 0.0492g TiO 2, put into ball grinder, ball milling 4 hours sieves after the oven dry; Powder precompressed after sieving is become bulk, 900 ℃ of following pre-burnings 8 hours, bulk is pulverized again, sieve, it is 10mm that precompressed becomes diameter, and thickness is the disk of 1mm, then final molding under the hydrostatic pressure of 200MPa; Disk after the moulding is incubated 4 hours down at 1175 ℃; Sinter into after the porcelain, sanding and polishing, the silver coated slurry under 500 ℃, is incubated 20 minutes and burns till silver electrode then.Full-automatic X-ray diffractometer (D/Max2550VB+/PC) with Japanese company of science is tested ceramic structure, tests carried out the temperature spectrum by the pottery behind the silver with Agilent impedance instrument (4294A).(a) X ray diffracting spectrum of PMN-PT pottery when being x=0.01 among Fig. 1, as can be seen from the figure, prepared PMN-PT pottery is the pure perovskite phase.Fig. 2 is the specific inductivity of pottery under the different frequency and the value of dielectric loss.The specific inductivity and the dielectric loss of PMN-PT pottery are respectively 1503 and 0.009 under the 1KHz, and Fig. 3 is the value of tuning rate under the different frequency, can find out, the tuning rate of this component pottery is 80% under 1KHz and the 30Kv/CM.
Through test, the dielectric loss of the PMN-PT pottery of embodiment 1 preparation is 0.007, and tuning rate is 87%.
Embodiment 2, during x=0.03, and by stoichiometric ratio weighing 0.7972g MgO, 5.2975g Nb 2O 5, the material that weighs up is put into ball grinder, in zirconia ball: material: alcohol is the ratio batch mixing ball milling of 3:1:1, and the ball milling time is 3 hours; Material oven dry back briquetting with mixing carries out synthesizing in advance under 1100 ℃ of temperature, takes out the good material of calcining and grinds, and obtains niobic acid magnesium pre-burning powder, again with niobic acid magnesium powder and 13.7576g PbO and 0.1478g TiO 2, put into ball grinder, ball milling 6 hours sieves after the oven dry; Powder precompressed after sieving is become bulk, 1000 ℃ of following pre-burnings 6 hours, bulk is pulverized again, sieve, it is 10mm that precompressed becomes diameter, and thickness is the disk of 1mm, then at the hydrostatic pressure compacted under of 250MPa; Disk after the moulding is incubated 3 hours down at 1200 ℃; Sinter into after the porcelain, sanding and polishing, the silver coated slurry under 500 ℃, is incubated 25 minutes and burns till silver electrode then.Full-automatic X-ray diffractometer (D/Max2550VB+/PC) with Japanese company of science is tested ceramic structure, tests carried out the temperature spectrum by the pottery behind the silver with Agilent impedance instrument (4294A).The X ray diffracting spectrum of (b) PMN-PT pottery when being x=0.03 among Fig. 1, as can be seen from the figure, prepared PMN-PT pottery is the pure perovskite phase.Fig. 2 is the specific inductivity of pottery under the different frequency and the value of dielectric loss.The specific inductivity and the dielectric loss of PMN-PT pottery are respectively 1253 and 0.011 under the 1KHz, and Fig. 3 is the value of tuning rate under the different frequency, can find out, the tuning rate of this component pottery is 63% under 1KHz and the 30Kv/CM.
Embodiment 3, during x=0.05, and by stoichiometric ratio weighing 0.7445g MgO, 4.9472g Nb 2O 5, the material that weighs up is put into ball grinder, in zirconia ball: material: alcohol is the ratio batch mixing ball milling of 3:1:1, and the ball milling time is 4 hours; Material oven dry back briquetting with mixing carries out synthesizing in advance under 1200 ℃ of temperature, takes out the good material of calcining and grinds, and obtains niobic acid magnesium pre-burning powder, again with niobic acid magnesium powder and 13.1181g PbO and 0.2466g TiO 2, put into ball grinder, ball milling is 8 hours again, sieves after the oven dry; Powder precompressed after sieving is become bulk, 1100 ℃ of following pre-burnings 4 hours, bulk is pulverized again, sieve, it is 12mm that precompressed becomes diameter, and thickness is the disk of 1.2mm, then at the hydrostatic pressure compacted under of 250MPa; Disk after the moulding is incubated 2 hours down at 1225 ℃; Sinter into after the porcelain, sanding and polishing, the silver coated slurry under 550 ℃, is incubated 25 minutes and burns till silver electrode then.Full-automatic X-ray diffractometer (D/Max2550VB+/PC) with Japanese company of science is tested ceramic structure, tests carried out the temperature spectrum by the pottery behind the silver with Agilent impedance instrument (4294A).(c) is the X ray diffracting spectrum of the PMN-PT pottery of x=0.05 among Fig. 1, and as can be seen from the figure, prepared PMN-PT pottery is the pure perovskite phase.Under the different frequency; The specific inductivity of PMN-PT pottery and dielectric loss are as shown in Figure 2 with the variation of temperature relation; As can be seen from the figure, under the 1kHz, its specific inductivity and dielectric loss are respectively 1300 and 0.007 during 300k; In the time of can finding out x=0.05 by Fig. 3, PMN-PT pottery its tuning rate when extra electric field is 30kV/cm under 1kHz is 87%.
Embodiment 4, during x=0.07, and by stoichiometric ratio weighing 0.7664g MgO, 5.0924g Nb 2O 5, the material that weighs up is put into ball grinder, in zirconia ball: material: alcohol is the ratio batch mixing ball milling of 3:1:1, and the ball milling time is 5 hours; Material oven dry back briquetting with mixing carries out synthesizing in advance under 1300 ℃ of temperature, takes out the good material of calcining and grinds, and obtains niobic acid magnesium pre-burning powder, again with niobic acid magnesium powder and 13.7938g PbO and 0.3457g TiO 2, put into ball grinder, ball milling 10 hours sieves after the oven dry; Powder precompressed after sieving is become bulk, 1200 ℃ of following pre-burnings 2 hours, bulk is pulverized again, sieve, it is 12mm that precompressed becomes diameter, and thickness is the disk of 1.2mm, then at the hydrostatic pressure compacted under of 300MPa; Disk after the moulding is incubated 1 hour down at 1250 ℃; Sinter into after the porcelain, sanding and polishing, the silver coated slurry under 550 ℃, is incubated 30 minutes and burns till silver electrode then.Full-automatic X-ray diffractometer (D/Max2550VB+/PC) with Japanese company of science is tested ceramic structure, tests carried out the temperature spectrum by the pottery behind the silver with Agilent impedance instrument (4294A).The X ray diffracting spectrum of (d) PMN-PT pottery when being x=0.07 among Fig. 1, as can be seen from the figure, prepared PMN-PT pottery is the pure perovskite phase.Fig. 2 is the specific inductivity of pottery under the different frequency and the value of dielectric loss.The specific inductivity and the dielectric loss of PMN-PT pottery are respectively 1380 and 0.006 under the 1KHz, and Fig. 3 is the value of tuning rate under the different frequency, can find out, the tuning rate of this component pottery is 75% under 1KHz and the 30Kv/CM.
In a word, the present invention has prepared the PMN-PT pottery through traditional ceramic preparation technology, and through constituent optimization and suitable temperature control, the PMN-PT pottery has obtained preferable performance.Therefore PMN-PT pottery of the present invention can well satisfy the request for utilization of shifter and wave filter, and its prescription and preparation method are fit to industrialization promotion and production in enormous quantities.

Claims (1)

1. the preparation method of PMN-PT pottery is characterized in that may further comprise the steps:
(a) with analytical pure MgO, Nb 2O 5, PbO and TiO 2, according to stoichiometric ratio (1-x) Pb (Mg 1/3Nb 2/3) O 3-xPbTiO 3(0.01≤x≤0.07) weighing and batching;
(b) batching is put into ball grinder, in zirconia ball: batching: alcohol is 3: 1: 1 ratio batch mixing ball milling, and the ball milling time is 2-5 hour;
(c) with batch mixing oven dry back briquetting, carry out synthesizing in advance, obtain MgNb 1000-1300 ℃ of temperature 2O 6Powder;
(d) again according to stoichiometric ratio (1-x) Pb (Mg 1/3Nb 2/3) O 3-xPbTiO 3(0.01≤x≤0.07) is weighing TiO respectively 2Add MgNb with PbO through pre-burning 2O 6In the powder;
(e) will be that the powder that step (d) prepares is put into ball grinder, ball milling 4-10 hour again, sieve after the oven dry;
(f) will pass through step (e) and press bulk in the material oven dry back of ball milling again, obtain the PMN-PT powder at 900-1200 ℃ of temperature lower calcination 2-8 hour;
(g) the PMN-PT powder that step (f) is obtained sieves, and to become diameter be 10-12mm in the back precompressed, and thickness is the disk of 1-1.2mm, then at the hydrostatic pressure compacted under of 200-300MPa;
(h) disk after the moulding is incubated 1-4 hour down at 1175-1250 ℃, sinters porcelain into, the silver coated slurry under 500-550 ℃, is incubated 20-30 minute and burns till silver electrode behind the economy-combat grinding and polishing light.
CN2012102472421A 2012-07-17 2012-07-17 Preparation method of lead magnesio-niobate-lead titanate ceramic Pending CN102757232A (en)

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CN107473743A (en) * 2017-09-15 2017-12-15 西安交通大学 A kind of lead base high-K capacitor dielectric material and preparation method thereof
CN107915486A (en) * 2017-11-17 2018-04-17 南京大学 A kind of method of raising PMN PT Curie temperature, piezoelectricity and heat endurance
WO2019174719A1 (en) * 2018-03-13 2019-09-19 Tdk Electronics Ag Polycrystalline ceramic solid body and method for producing a polycrystalline ceramic solid body
CN112062564A (en) * 2020-09-17 2020-12-11 广西大学 Preparation method of PMN-PSN ultrahigh breakdown electric field thin film material
CN113636840A (en) * 2021-10-15 2021-11-12 北京国械堂科技发展有限责任公司 Ceramic thick film of ceramic electrode for electric field treatment of tumor and preparation method thereof
CN114163234A (en) * 2021-12-27 2022-03-11 佛山(华南)新材料研究院 Lead magnesium niobate-lead titanate relaxation ferroelectric ceramic and preparation method and application thereof
CN114349506A (en) * 2022-01-07 2022-04-15 森霸传感科技股份有限公司 Preparation method and application of low-loss high-dielectric-constant lead magnesium niobate-lead titanate dielectric ceramic material
CN114621009A (en) * 2022-03-16 2022-06-14 南京理工大学 Lead magnesium niobate-lead titanate-based piezoelectric ceramic material and preparation method thereof

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CN107473743A (en) * 2017-09-15 2017-12-15 西安交通大学 A kind of lead base high-K capacitor dielectric material and preparation method thereof
CN107915486A (en) * 2017-11-17 2018-04-17 南京大学 A kind of method of raising PMN PT Curie temperature, piezoelectricity and heat endurance
WO2019174719A1 (en) * 2018-03-13 2019-09-19 Tdk Electronics Ag Polycrystalline ceramic solid body and method for producing a polycrystalline ceramic solid body
EP4234515A3 (en) * 2018-03-13 2023-09-06 TDK Electronics AG Polycrystalline ceramic solid body and method for producing a polycrystalline ceramic solid body
CN112566882A (en) * 2018-03-13 2021-03-26 Tdk电子股份有限公司 Polycrystalline ceramic solid body and method for producing a polycrystalline ceramic solid body
JP2021516204A (en) * 2018-03-13 2021-07-01 ティーディーケイ・エレクトロニクス・アクチェンゲゼルシャフトＴｄｋ Ｅｌｅｃｔｒｏｎｉｃｓ Ａｇ Polycrystalline ceramic solid and method for producing polycrystalline ceramic solid
US11680021B2 (en) 2018-03-13 2023-06-20 Tdk Electronics Ag Polycrystalline ceramic solid and method for producing a polycrystalline ceramic solid
JP7113904B2 (en) 2018-03-13 2022-08-05 ティーディーケイ・エレクトロニクス・アクチェンゲゼルシャフト Polycrystalline ceramic solid and method for producing polycrystalline ceramic solid
CN112062564B (en) * 2020-09-17 2022-05-17 广西大学 Preparation method of PMN-PSN ultrahigh breakdown electric field thin film material
CN112062564A (en) * 2020-09-17 2020-12-11 广西大学 Preparation method of PMN-PSN ultrahigh breakdown electric field thin film material
CN113636840A (en) * 2021-10-15 2021-11-12 北京国械堂科技发展有限责任公司 Ceramic thick film of ceramic electrode for electric field treatment of tumor and preparation method thereof
CN114163234A (en) * 2021-12-27 2022-03-11 佛山(华南)新材料研究院 Lead magnesium niobate-lead titanate relaxation ferroelectric ceramic and preparation method and application thereof
CN114349506A (en) * 2022-01-07 2022-04-15 森霸传感科技股份有限公司 Preparation method and application of low-loss high-dielectric-constant lead magnesium niobate-lead titanate dielectric ceramic material
CN114621009A (en) * 2022-03-16 2022-06-14 南京理工大学 Lead magnesium niobate-lead titanate-based piezoelectric ceramic material and preparation method thereof
CN114621009B (en) * 2022-03-16 2023-02-28 南京理工大学 Lead magnesium niobate-lead titanate-based piezoelectric ceramic material and preparation method thereof

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Application publication date: 20121031