CN107573067A - The low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece - Google Patents

The low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece Download PDF

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Publication number
CN107573067A
CN107573067A CN201710758267.0A CN201710758267A CN107573067A CN 107573067 A CN107573067 A CN 107573067A CN 201710758267 A CN201710758267 A CN 201710758267A CN 107573067 A CN107573067 A CN 107573067A
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temperature
piezoelectric ceramic
ceramic piece
sintering
zirconate titanate
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李元勋
郑阳
陈大明
郁国良
李亚菲
苏桦
刘悦
张怀武
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University of Electronic Science and Technology of China
Guangdong Electronic Information Engineering Research Institute of UESTC
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University of Electronic Science and Technology of China
Guangdong Electronic Information Engineering Research Institute of UESTC
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Abstract

The present invention provides a kind of low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece, comprises the steps:By PbO material powders, ZrO2Material powder, TiO2Material powder and Sm2O3Material powder presses Pb1‑xSmx(Zr0.52Ti0.48)1‑x/4O3Chemical general formula carries out dispensing, obtains mixed powder;Ball milling, drying, and pre-burning obtains pre-sintered powder;Prepare glass sintering aid LBBS with quenching method, pre-sintered powder is mixed with glass sintering aid, ball milling, drying, granulation, and tabletting obtains piezoelectric ceramics green compact;Piezoelectric ceramics green compact is subjected to dumping and sintering, obtain piezoelectric ceramic piece, the sintering temperature of piezoelectric ceramic piece is reduced to 850 DEG C by the present invention from more than 1000 DEG C, largely reduce the volatilization of lead (fusing point is 980 DEG C), alleviate the infringement to human body and the pollution of environment, the densification of ceramic post sintering is improved, relative density reaches 95%.

Description

The low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece
Technical field
The present invention relates to inorganic non-metallic technical field of electronic materials, more particularly, to a kind of lead zirconate titanate (PZT) base The low-temperature sintering method of piezoelectric ceramic piece.
Background technology
An important branch of the piezoelectric ceramics as electronic information material, is widely used in piezoelectric vibrator and PZT (piezoelectric transducer) Deng field.Because PZT base piezoelectric ceramics have the characteristics that Curie temperature is high, piezoelectric constant is high, easy doping vario-property, stability are good, Occupied an leading position at present in piezoceramic material field.
For PZT base piezoelectric ceramics sintering temperature typically more than 1200 DEG C, the lead in its component is readily volatilized at high temperature, leads Cause component nonstoichiometry ratio and make its piezoelectric property reduction, therefore by way of supplementing lead with maintain formula in piezoelectricity Energy highest stoichiometric proportion, conventional atmosphere sintering method and excess PbO method can not be inherently eliminated the volatilization of lead, while its Volatilization not only can cause damage to human body but also environment can be polluted.
On the other hand, LTCC (LTCC) technology is that low sintering ceramic powder is made into green band, in ceramics Required circuitous pattern is produced using processes such as punching, filling perforation, accurate conductor (silver) printings on green band, is then laminated on Together, sintered after cleaved, dumping at 900 DEG C, the non-interfering high-density circuit of three dimensions is made.As a kind of multilayer Connect up ceramic substrate process technology, reduce small product size, mitigate product weight, reduce cost etc. have obviously Advantage, realize batch micro operations and the large-scale production of product.If PZT based piezoelectric ceramic materials can be applied to LTCC manufacture skills In art, the process advantage with regard to LTCC can be given full play to, piezoelectric device is developed to planarization and integrated direction.In order to reach this One target, it is necessary to solve following two technical problems.First, PZT based piezoelectric ceramic materials low-temperature sintering at 900 DEG C is realized, two It is to realize PZT base piezoelectric ceramics and conductor silver matching co-firing, otherwise causes piezoelectric ceramics to give birth to mutual diffusive migration with conductor silver hair, Device performance is caused to decline, or even failure.
The content of the invention
The present invention provides a kind of low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece, it is intended to solves existing piezoelectricity pottery Porcelain sintering temperature height causes the highly volatile of lead in sintering process and realizes the problem of burning altogether with the silver electrode of low melting point.
For achieving the above object, it is as follows to provide technical scheme by the present invention:
A kind of low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece, comprises the steps:
Step A:By PbO material powders, ZrO2Material powder, TiO2Material powder and Sm2O3Material powder presses Pb1-xSmx (Zr0.52Ti0.48)1-x/4O3Chemical general formula carries out dispensing, 0.03≤x≤0.06, obtains mixed powder;Ball milling, drying, and pre-burning Obtain pre-sintered powder;
Step B:Glass sintering aid LBBS is prepared with quenching method, glass sintering aid LBBS composition includes Li2O、B2O3、 Bi2O3、SiO2
Specifically, quenching method prepares glass sintering aid LBBS and comprised the following steps:
(1) by Li2O material powders, B2O3Material powder, Bi2O3Material powder, SiO2Material powder is according to certain mol proportion Dispensing is carried out, obtains mixed powder.
(2) by mixed powder ball milling obtained by step (1), dry, sintering, taking-up obtains sintered body.Wherein drying temperature is 70~90 DEG C, preferably 80 DEG C.Sintering temperature is 1100~1300 DEG C, and sintering time is 2~4 hours, after sintering time terminates Sintered body is taken out at once.
(3) step 2 gained sintered body is placed in cold water and quenched, obtain vitreum.
(4) step 3 gained vitreum is dried, it is levigate, sieving, obtain LBBS sintering aids, wherein drying temperature be 70~ 90 DEG C, preferably 80 DEG C.
Step C:Pre-sintered powder obtained by step A is mixed with step B gained glass sintering aids, ball milling, drying, granulation, And tabletting obtains piezoelectric ceramics green compact;
Step D:Piezoelectric ceramics green compact obtained by step C is subjected to dumping and sintering, obtains piezoelectric ceramic piece.
It is preferred that the mechanical milling process in step A and/or step C is specially:Using deionized water as dispersant, Using the zirconia ball of two kinds of sizes as ball-milling medium, mixed powder, big zirconia ball, the matter of small zirconia ball and deionized water Amount is than being 1:(1.5~2.5):(1.5~2.5):(1.5~2.5), milling time are 8~16 hours, are obtained well mixed Ball milling material.
It is preferred that drying temperature is 70~90 DEG C in step A.
It is preferred that in step A, calcined temperature is 850~900 DEG C, and burn-in time is 2~4 hours.
It is preferred that in stepb, the mol ratio of each compositions of glass sintering aid LBBS is Li2O:B2O3:Bi2O3: SiO2=(1.5~2.5):(1.5~2.5):(0.5~1.5):(0.5~1.5).
It is preferred that after adding glass sintering aid in step C, glass sintering aid accounts for pre-sintered powder and helps burning with glass The percentage of agent composition gross weight is 1-5wt%.
It is preferred that in step C:Drying temperature is 70~90 DEG C;The binding agent added during granulation is PVA, is added Amount be 5~10wt%;Pressure during tabletting is 10~20MPa.
It is preferred that in step D, dump temperature is 400~550 DEG C, the dumping time is 2~3 hours;Sintering temperature Spend for 850 DEG C, sintering time is 10~12 hours.
It is preferred that the heating rate of the pre-burning, dumping, sintering in step is 2~5 DEG C/min.
Beneficial effects of the present invention are:The present invention provides a kind of low-temperature sintering method of piezoelectric ceramic piece, in pre-burning process Principal crystalline phase is synthesized, glass sintering aid is added after pre-burning, the sintering temperature of piezoelectric ceramic piece is reduced to 850 from more than 1000 DEG C DEG C, largely reduce the volatilization of lead (fusing point is 980 DEG C), alleviate the infringement to human body and the pollution of environment, improve The densification of ceramic post sintering, relative density reach 95%.Face from the silver electrode to sample obtained by the present invention with piezoelectric ceramics Microscopic appearance and elementary composition (SEM+EDS) analysis result (Fig. 5) at boundary is as can be seen that silver electrode layer has with piezoceramics layer Obvious boundary.In figure, the left side is piezoelectric ceramics region, and the right is silver electrode region, and white line scans for elementary analysis line Region, red curve are the elementary analysis result in the region, and the detection peak intensity of piezoelectric ceramics region silver element is very low to be almost Zero, illustrate that silver ion is not diffused to inside piezoceramic material, realize the common burning of piezoceramic material and silver electrode, be advantageous to Piezoelectric device is produced in enormous quantities using LTCC technology.Preparation method provided by the invention is advantageous to PZT base piezoelectric ceramics In LTCC application, the business demand of piezoelectric ceramics is met.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum of ceramic material after the embodiment of the present invention 1~3 sinters under 850 DEG C of environment;
The microscopic appearance figure for the ceramic section that Fig. 2 sinters to obtain for the embodiment of the present invention 1 under 850 DEG C of environment;
The microscopic appearance figure for the ceramic section that Fig. 3 sinters to obtain for the embodiment of the present invention 2 under 850 DEG C of environment;
The microscopic appearance figure for the ceramic section that Fig. 4 sinters to obtain for the embodiment of the present invention 3 under 850 DEG C of environment;
Fig. 5 is the sample silver electrode and piezoelectric ceramics critical part that the embodiment of the present invention 2 sinters to obtain under 850 DEG C of environment SEM+EDS schemes.
Embodiment
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through specific realities different in addition The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from Various modifications or alterations are carried out under the spirit of the present invention.
Embodiment 1
The low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece, comprises the steps:
Step A:By PbO material powders, ZrO2Material powder, TiO2Material powder and Sm2O3Material powder presses Pb1-xSmx (Zr0.52Ti0.48)1-x/4O3Chemical general formula carries out dispensing, x=0.03, obtains mixed powder;
Mixed powder obtained by step A is put into polytetrafluoroethylene (PTFE) ball grinder, using deionized water as dispersant, with two kinds As ball-milling medium, mixed powder, big zirconia ball, the mass ratio of small zirconia ball and deionized water are the zirconia ball of size 1:1.5:1.5:1.5, milling time is 8 hours, obtains well mixed ball milling material.Well mixed ball milling material is put into baking Drying obtains drying powder in case, and drying temperature is 70 DEG C.Powder will be dried to be placed in alumina crucible, in atmospheric atmosphere condition Lower pre-burning obtains pre-sintered powder, and calcined temperature is 850 DEG C, and pre-burning heating rate is 2 DEG C/min, and burn-in time is 2 hours.
Step B:Glass sintering aid LBBS is prepared with quenching method, glass sintering aid LBBS composition includes Li2O、B2O3、 Bi2O3、SiO2;The mol ratio of each compositions of glass sintering aid LBBS is Li2O:B2O3:Bi2O3:SiO2=1.5:1.5:0.5:0.5.
Step C:Pre-sintered powder obtained by step A is mixed with glass sintering aid LBBS obtained by step B, with pre-sintered powder Calculated with glass sintering aid total weight of the mixture, the amount that glass sintering aid adds is 1wt%;
Mixed powder is put into polytetrafluoroethylene (PTFE) ball grinder, using deionized water as dispersant, with two kinds of sizes Zirconia ball as ball-milling medium, mixed powder, big zirconia ball, the mass ratio of small zirconia ball and deionized water are 1: 1.5:1.5:1.5, milling time is 8 hours, obtains well mixed ball milling material.Well mixed ball milling material is put into baking oven Interior drying obtains drying powder, and drying temperature is 70 DEG C.
The PVA for adding 5wt% is granulated as bonding agent, and pressurize obtains a diameter of 11mm for 30 seconds under 10MPa, thick Spend the piezoelectric ceramics green compact for 1.8mm.
Step D:Piezoelectric ceramics green compact obtained by step C is placed in Muffle furnace, risen according to 2 DEG C/min of temperature curves Temperature, dump temperature are 400 DEG C, and 2 hours progress dumpings of insulation, then continue according to 2 DEG C/min of temperature when temperature reaches 400 DEG C Curve is heated up, and when being warming up to 850 DEG C, maintains be sintered within 10 hours at this temperature, finally obtained lead zirconate titanate base pressure Electroceramics piece.
Embodiment 2
The low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece, comprises the steps:
Step A:By PbO material powders, ZrO2Material powder, TiO2Material powder and Sm2O3Material powder presses Pb1-xSmx (Zr0.52Ti0.48)1-x/4O3Chemical general formula carries out dispensing, x=0.03, obtains mixed powder;
Mixed powder obtained by step A is put into polytetrafluoroethylene (PTFE) ball grinder, using deionized water as dispersant, with two kinds As ball-milling medium, mixed powder, big zirconia ball, the mass ratio of small zirconia ball and deionized water are the zirconia ball of size 1:2.5:2.5:2.5, milling time is 16 hours, obtains well mixed ball milling material.Well mixed ball milling material is put into Drying in oven obtains drying powder, and drying temperature is 90 DEG C.Powder will be dried to be placed in alumina crucible, in atmosphere foxing Pre-burning obtains pre-sintered powder under part, and calcined temperature is 900 DEG C, and pre-burning heating rate is 5 DEG C/min, and burn-in time is 4 small When.
Step B:Glass sintering aid LBBS is prepared with quenching method, glass sintering aid LBBS composition includes Li2O、B2O3、 Bi2O3、SiO2;The mol ratio of each compositions of glass sintering aid LBBS is Li2O:B2O3:Bi2O3:SiO2=2.5:2.5:1.5:1.5.
Step C:Pre-sintered powder obtained by step A is mixed with glass sintering aid LBBS obtained by step B, with pre-sintered powder Calculated with glass sintering aid total weight of the mixture, the amount that glass sintering aid adds is 5wt%;
Mixed powder is put into polytetrafluoroethylene (PTFE) ball grinder, using deionized water as dispersant, with two kinds of sizes Zirconia ball as ball-milling medium, mixed powder, big zirconia ball, the mass ratio of small zirconia ball and deionized water are 1: 2.5:2.5:2.5, milling time is 16 hours, obtains well mixed ball milling material.Well mixed ball milling material is put into baking Drying obtains drying powder in case, and drying temperature is 90 DEG C.
The PVA for adding 10wt% is granulated as bonding agent, and pressurize obtains a diameter of 11mm in 30 seconds under 20MPa, Thickness is 1.8mm piezoelectric ceramics green compact.
Step D:Piezoelectric ceramics green compact obtained by step C is placed in Muffle furnace, risen according to 5 DEG C/min of temperature curves Temperature, dump temperature are 550 DEG C, and 3 hours progress dumpings of insulation, then continue according to 5 DEG C/min of temperature when temperature reaches 550 DEG C Curve is heated up, and when being warming up to 850 DEG C, maintains be sintered within 12 hours at this temperature, finally obtained lead zirconate titanate base pressure Electroceramics piece.
Embodiment 3
The low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece, comprises the steps:
Step A:By PbO material powders, ZrO2Material powder, TiO2Material powder and Sm2O3Material powder presses Pb1-xSmx (Zr0.52Ti0.48)1-x/4O3Chemical general formula carries out dispensing, x=0.06, obtains mixed powder;
Mixed powder obtained by step A is put into polytetrafluoroethylene (PTFE) ball grinder, using deionized water as dispersant, with two kinds As ball-milling medium, mixed powder, big zirconia ball, the mass ratio of small zirconia ball and deionized water are the zirconia ball of size 1:2:2:2, milling time is 12 hours, obtains well mixed ball milling material.Well mixed ball milling material is put into baking oven Drying obtains drying powder, and drying temperature is 80 DEG C.Powder will be dried to be placed in alumina crucible, it is pre- under the conditions of atmospheric atmosphere Burning obtains pre-sintered powder, and calcined temperature is 870 DEG C, and pre-burning heating rate is 3 DEG C/min, and burn-in time is 3 hours.
Step B:Glass sintering aid LBBS is prepared with quenching method, glass sintering aid LBBS composition includes Li2O、B2O3、 Bi2O3、SiO2;The mol ratio of each compositions of glass sintering aid LBBS is Li2O:B2O3:Bi2O3:SiO2=2:2:1:1.
Step C:Pre-sintered powder obtained by step A is mixed with glass sintering aid LBBS obtained by step B, with pre-sintered powder Calculated with glass sintering aid total weight of the mixture, the amount that glass sintering aid adds is 3wt%;
Mixed powder is put into polytetrafluoroethylene (PTFE) ball grinder, using deionized water as dispersant, with two kinds of sizes Zirconia ball as ball-milling medium, mixed powder, big zirconia ball, the mass ratio of small zirconia ball and deionized water are 1:2: 2:2, milling time is 12 hours, obtains well mixed ball milling material.Well mixed ball milling material is put into drying in oven Obtain drying powder, drying temperature is 80 DEG C.
The PVA for adding 7wt% is granulated as bonding agent, and pressurize obtains a diameter of 11mm for 30 seconds under 15MPa, thick Spend the piezoelectric ceramics green compact for 1.8mm.
Step D:Piezoelectric ceramics green compact obtained by step C is placed in Muffle furnace, risen according to 3 DEG C/min of temperature curves Temperature, dump temperature are 450 DEG C, and 2.5 hours progress dumpings of insulation, then continue according to 3 DEG C/min of temperature when temperature reaches 550 DEG C Line of writing music is heated up, and when being warming up to 850 DEG C, maintains be sintered within 11 hours at this temperature, finally obtained lead zirconate titanate base Piezoelectric ceramic piece.
Obtained sample is subjected to following performance test:
(1) Phase Structure Analysis of piezoelectric ceramics and Micro-Structure Analysis
The present invention carries out Phase Structure Analysis using XRD to piezoelectric ceramics, and the micro- of piezoelectric ceramic piece section is observed using SEM See tissue topography.
(2) test of piezoelectric ceramics dielectric properties
By piezoelectric ceramic piece with capacitance measuring tester test frequency be 1KHz under capacitance and dielectric loss, then basis The relation formula of capacitance and dielectric constant calculates its relative dielectric constant.
(3) test of piezoelectric ceramics piezoelectric property
The piezoelectric ceramic piece of the embodiment of the present invention is diameter 11mm, thickness 1.8mm disk.Put it into silicone oil, it is right Its added electric field is polarized, and poling temperature is 120 DEG C, polarizing voltage 4kV/mm, and the polarization time is 30 minutes.Test pressure afterwards Electric constant d33With electromechanical coupling factor Kp.
The performance parameter of lead zirconate titanate base piezoelectric ceramic piece made from the present embodiment 1 to 3 is given below:
Embodiment is numbered Relative density Relative dielectric constant Dielectric loss d33 kp
1 95.325% 1076.751 0.040 247 0.672
2 95.4% 1055.072 0.031 225 0.685
3 95.65% 1027.427 0.039 236 0.679
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause This, all those of ordinary skill in the art without departing from disclosed spirit with being completed under technological thought All equivalent modifications or change, should by the present invention claim be covered.

Claims (9)

1. a kind of low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece, it is characterised in that comprise the steps:
Step A:By PbO material powders, ZrO2Material powder, TiO2Material powder and Sm2O3Material powder presses Pb1-xSmx (Zr0.52Ti0.48)1-x/4O3Chemical general formula carries out dispensing, 0.03≤x≤0.06, obtains mixed powder;Ball milling, drying, and pre-burning Obtain pre-sintered powder;
Step B:Glass sintering aid LBBS is prepared with quenching method, glass sintering aid LBBS composition includes Li2O、B2O3、Bi2O3、 SiO2
Step C:Pre-sintered powder obtained by step A is mixed with step B gained glass sintering aids, ball milling, drying, granulation, and press Piece obtains piezoelectric ceramics green compact;
Step D:Piezoelectric ceramics green compact obtained by step C is subjected to dumping and sintering, obtains piezoelectric ceramic piece.
2. the low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece according to claim 1, it is characterised in that step A And/or the mechanical milling process in step C is specially:Using deionized water as dispersant, ball is used as using the zirconia ball of two kinds of sizes Grinding media, mixed powder, big zirconia ball, the mass ratio of small zirconia ball and deionized water are 1:(1.5~2.5):(1.5~ 2.5):(1.5~2.5), milling time are 8~16 hours, obtain well mixed ball milling material.
3. the low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece according to claim 1, it is characterised in that:Step A Middle drying temperature is 70~90 DEG C.
4. the low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece according to claim 1, it is characterised in that:Step A In, calcined temperature is 850~900 DEG C, and burn-in time is 2~4 hours.
5. the low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece according to claim 1, it is characterised in that:In step In B, the mol ratio of each compositions of glass sintering aid LBBS is Li2O:B2O3:Bi2O3:SiO2=(1.5~2.5):(1.5~2.5): (0.5~1.5):(0.5~1.5).
6. the low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece according to claim 1, it is characterised in that:Step C After middle addition glass sintering aid, it is 1- that glass sintering aid, which accounts for pre-sintered powder and the percentage of glass sintering aid total weight of the mixture, 5wt%.
7. the low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece according to claim 1, it is characterised in that:Step C In:Drying temperature is 70~90 DEG C;The binding agent added during granulation is PVA, and the amount of addition is 5~10wt%;Pressure during tabletting Power is 10~20MPa.
8. the low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece according to claim 1, it is characterised in that:In step In D, dump temperature is 400~550 DEG C, and the dumping time is 2~3 hours;Sintering temperature is 850 DEG C, and sintering time is 10~12 Hour.
9. the low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece according to claim 1, it is characterised in that:In step Pre-burning, dumping, sintering heating rate be 2~5 DEG C/min.
CN201710758267.0A 2017-08-29 2017-08-29 The low-temperature sintering method of lead zirconate titanate base piezoelectric ceramic piece Pending CN107573067A (en)

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CN109166960A (en) * 2018-08-23 2019-01-08 浙江理工大学 A kind of preparation method of fiber base flexible piezoelectric sensors
CN110498603A (en) * 2019-09-25 2019-11-26 山东国瓷功能材料股份有限公司 Glass powder and preparation method thereof, piezoelectric ceramics and preparation method thereof, piezoelectric ceramic devices
CN111747740A (en) * 2020-06-28 2020-10-09 安徽容知日新科技股份有限公司 Samarium ion doped lead zirconate titanate based high-performance piezoelectric ceramic and preparation method thereof
CN112794640A (en) * 2021-01-05 2021-05-14 长飞光纤光缆股份有限公司 Pretreatment method of multi-component powder raw material
CN112960981A (en) * 2021-05-07 2021-06-15 重庆文理学院 Preparation method of lanthanum-tin doped lead zirconate titanate ceramic material
CN113402285A (en) * 2021-05-26 2021-09-17 济南大学 Low-temperature co-fired sintering agent for piezoelectric ceramics and preparation method thereof
CN115124340A (en) * 2022-06-29 2022-09-30 安徽大学 Medium low-loss low-temperature co-fired ceramic material and preparation method and application thereof

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RAJIV RANJAN等: "Impedance and electric modulus analysis of Sm-modified Pb(Zr0.55Ti0.45)1−x/4O3 ceramics", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
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Cited By (12)

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Publication number Priority date Publication date Assignee Title
CN109166960A (en) * 2018-08-23 2019-01-08 浙江理工大学 A kind of preparation method of fiber base flexible piezoelectric sensors
CN110498603A (en) * 2019-09-25 2019-11-26 山东国瓷功能材料股份有限公司 Glass powder and preparation method thereof, piezoelectric ceramics and preparation method thereof, piezoelectric ceramic devices
CN110498603B (en) * 2019-09-25 2021-11-23 山东国瓷功能材料股份有限公司 Glass powder and preparation method thereof, piezoelectric ceramic and preparation method thereof, and piezoelectric ceramic device
CN111747740A (en) * 2020-06-28 2020-10-09 安徽容知日新科技股份有限公司 Samarium ion doped lead zirconate titanate based high-performance piezoelectric ceramic and preparation method thereof
CN111747740B (en) * 2020-06-28 2022-06-10 安徽容知日新科技股份有限公司 Samarium ion doped lead zirconate titanate based high-performance piezoelectric ceramic and preparation method thereof
CN112794640A (en) * 2021-01-05 2021-05-14 长飞光纤光缆股份有限公司 Pretreatment method of multi-component powder raw material
CN112794640B (en) * 2021-01-05 2022-06-21 长飞光纤光缆股份有限公司 Pretreatment method of multi-component powder raw material
CN112960981A (en) * 2021-05-07 2021-06-15 重庆文理学院 Preparation method of lanthanum-tin doped lead zirconate titanate ceramic material
CN112960981B (en) * 2021-05-07 2022-07-01 重庆文理学院 Preparation method of lanthanum-tin doped lead zirconate titanate ceramic material
CN113402285A (en) * 2021-05-26 2021-09-17 济南大学 Low-temperature co-fired sintering agent for piezoelectric ceramics and preparation method thereof
CN115124340A (en) * 2022-06-29 2022-09-30 安徽大学 Medium low-loss low-temperature co-fired ceramic material and preparation method and application thereof
CN115124340B (en) * 2022-06-29 2023-02-28 安徽大学 Medium low-loss low-temperature co-fired ceramic material and preparation method and application thereof

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