CN104529447B - Bismuth layered composite structure piezoceramic material and preparation method thereof - Google Patents
Bismuth layered composite structure piezoceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of bismuth layered composite structure piezoceramic material and preparation method thereof, the chemical general formula of the material is：[Ca1‑xMexBi2Nb2‑2yMe’2yO9]1‑z‑[Bi3‑aMea(TiNb)1‑ bMe’2bO9]z；Wherein, Me and Me ' are respectively the doped chemical of suitable different crystalline lattice position, and Me is the one or more in Li, Mn, Ce, and Me ' is the one or more in Ta, W；X, y, z, a, b are respectively molar fraction, 0≤x≤0.05,0≤y≤0.05,0≤a≤0.05,0≤b≤0.05,0.2≤z≤0.8.The piezoceramic material has very high Curie temperature, excellent piezoelectric property and adjustable comprehensive electrochemical properties, available for various high temperature piezoelectric devices.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of bismuth layered composite structure piezoceramic material and its preparation
Method.
Background technology
Piezoelectric ceramics is a kind of functional ceramic material that can mutually convert electric energy and mechanical energy.The material is in dispatch from foreign news agency
Strain can be produced under field action, and relative displacement occurs for the positive and negative charge center of material internal under mechanical force, so that
The two poles of the earth of material produce opposite charges.Piezoelectric ceramics is widely used in the fields such as wave filter, transducer, sensor.Piezoelectricity is made pottery
Porcelain is usually ferroelectric, can be disappeared near Curie temperature piezoelectricity.Aero-Space auto industry etc. is used in recent years
Service behaviour demand is improved constantly various piezoelectric devices in high temperature environments, and the piezoelectric ceramics demand with high-curie temperature is increasingly
Urgently.However, the Curie temperature of traditional lead zirconate titanate (PZT) is about 300 DEG C to 370 DEG C or so.Because temperature rise causes
Piezoelectricity instability problem caused by depolarization, its operating temperature upper limit is usually that at the 1/2 of its Tc, thus PZT makes
180 DEG C are generally significantly less than with temperature.
Laminated structure bismuth piezoelectric ceramic is the important pottery of the piezoelectricity with superelevation Curie temperature (550 DEG C -950 DEG C) of a class
Porcelain, but its piezoelectric property is poor, and coercive electric field is high, resistivity is low, it is difficult to also cause it the problems such as preparation structure uniform porcelain body
It is not easy to be polarized.In addition, similar with conventional ceramic, such ceramics is generally prepared with solid reaction process, and related process is cumbersome,
The stable homogeneous of sample is difficult to control, and comprehensive electrochemical properties are difficult to.Therefore how to prepare with superelevation Curie temperature and
The bismuth-containing of preferable piezoelectric property is laminated electroceramics and improves its technique, is the important content of the area research, to related device
Exploitation is also significant.
The content of the invention
The embodiments of the invention provide a kind of bismuth layered composite structure piezoceramic material and preparation method thereof.The piezoelectricity is made pottery
Ceramic material has very high Curie temperature, excellent piezoelectric property and adjustable comprehensive electrochemical properties, available for various high-temperature piezoelectrics
Device.
In a first aspect, the embodiments of the invention provide a kind of bismuth layered composite structure piezoceramic material, chemical general formula is：
[Ca1-xMexBi2Nb2-2yMe’2yO9]1-z-[Bi3-aMea(TiNb)1-bMe’2bO9]z；
Wherein, Me and Me ' are respectively the doped chemical of suitable different crystalline lattice position, and Me is one kind or many in Li, Mn, Ce
Kind, Me ' is the one or more in Ta, W；X, y, z, a, b are respectively molar fraction, 0≤x≤0.05,0≤y≤0.05,0≤a
≤ 0.05,0≤b≤0.05,0.2≤z≤0.8.
Second aspect, the embodiments of the invention provide a kind of preparation of the piezoceramic material as described in above-mentioned first aspect
Method, the preparation method includes：
By calcium carbonate, titanium oxide, bismuth oxide, niobium pentaoxide, lithium carbonate, manganese carbonate, and doped chemical Me and/or Me '
Oxide or salt, according to stoichiometric proportion Ca1-xMexBi2Nb2-2yMe’2yO9(referred to as CBN) and Bi3-aMea(TiNb)1- bMe’2bO9(referred to as BTN), carries out weighing dispensing respectively, obtains the first original powder for preparing CBN and for preparing
BTN second of original powder；Wherein, Me and Me ' are respectively the doped chemical of suitable different crystalline lattice position, and Me is Li, Mn, Ce
In one or more, Me ' be Ta, W in one or more；X, y, z, a, b are respectively molar fraction, and 0≤x≤0.05,0≤
Y≤0.05,0≤a≤0.05,0≤b≤0.05,0.2≤z≤0.8；
The first described original powder and second of original powder are subjected to ball milling using water or ethanol as medium respectively,
The first slurry and the second slurry are obtained, and first slurry and the second slurry are respectively dried, ground and sieved, first is obtained
Original powder and the second original powder；
First original powder is placed in crucible and calcined, is obtained with bismuth laminated CBN powders；By the second original powder
Material is placed in crucible and calcined, and obtains with bismuth laminated BTN powders；
By the CBN powders and the BTN powders, the ratio needed for is weighed after dispensing mixes, additions concentration for 1wt%~
6wt% PVAC polyvinylalcohol solution, ground in mortar it is uniform after, granulate and sieve and obtain mixed powder (abbreviation CBTN)；
The CBTN is pressed into ceramic body；
The ceramic body is placed in into heating in crucible to carry out after dumping, piezoelectric ceramic body is made in sintering；
After piezoelectric ceramic body polishing, polishing, coating metal electrode, heat and apply polarizing voltage to enter in silicone oil
Row polarization, the piezoceramic material is obtained after cooling.
It is preferred that, the temperature of the calcining is 600 DEG C~900 DEG C, and the time is 1.5~5 hours.
It is preferred that, the sieving is specially：Sieved using the sieve of 150~200 mesh.
It is preferred that, the pressure for suppressing CBTN formation ceramic bodies is 50MPa~150MPa.
It is preferred that, the temperature of the sintering is 950 DEG C~1150 DEG C, and the time is 2~6 hours.
It is preferred that, the temperature of the polarization is 150 DEG C~200 DEG C, and the electric-field intensity of polarization is 5kV/mm~15kV/mm,
The time of polarization is 10~30 minutes.
The principle of the present invention can obtain the single-phase thing of high-purity when being and calcining synthesis respectively based on two kinds of powders CBN and BTN,
In being re-sintered after mixing afterwards, because the crystal structure of two kinds of systems is close, grain growth is not by mixed influence, so as to can be caused
The ceramic body of densification.Compared with current material system and technology of preparing, the present invention has many merits.Answering prepared by the present invention
Closing bismuth-containing lamination electroceramics has the microstructure of dense uniform, high phase purity and crystallinity, very high Curie temperature (TcReach
More than 900 DEG C), higher piezoelectric constant (d33Up to 18pC/N), adjustable dielectric properties (εr=100~500) etc., available for each
Planting needs the dependent piezoelectric devices such as sensor of the operating temperature more than 600 DEG C；In addition, the preparation of the compound bismuth-containing layer ceramic systems
Technique has preparation process easy, it is easy to controls compound system component, is easy to large-scale industrialized production, with low cost, product
The advantages of purity is high.The method and prepared high temperature piezoceramics that the present invention is provided have preferable application prospect.
Brief description of the drawings
Below by drawings and Examples, the technical scheme to the embodiment of the present invention is described in further detail.
Fig. 1 is the preparation method flow chart for the bismuth layered composite structure piezoceramic material that the embodiment of the present invention 2 is provided；
Fig. 2 is the piezoceramic material [Ca that the embodiment of the present invention 3 is provided0.95Li0.025Mn0.025Bi2Nb2O9]0.7-
[Bi2.95Li0.02Mn0.03TiNbO9]0.3Piezoelectric constant different temperatures anneal rear chamber temperature and pressure electric constant change curve；
Fig. 3 is the piezoceramic material [Ca that the embodiment of the present invention 3 is provided0.95Li0.025Mn0.025Bi2Nb2O9]0.7-
[Bi2.95Li0.02Mn0.03TiNbO9]0.3Stereoscan photograph.
Embodiment
With reference to embodiment, the present invention is described in further detail, but is not intended to the guarantor of the limitation present invention
Protect scope.
Embodiment 1
The embodiment of the present invention 1 provides a kind of bismuth layered composite structure piezoceramic material, and its chemical general formula is：[Ca1- xMexBi2Nb2-2yMe’2yO9]1-z-[Bi3-aMea(TiNb)1-bMe’2bO9]z；
Wherein, Me and Me ' are respectively the doped chemical of suitable different crystalline lattice position, and Me is one kind or many in Li, Mn, Ce
Kind, Me ' is the one or more in Ta, W；X, y, z, a, b are respectively molar fraction, 0≤x≤0.05,0≤y≤0.05,0≤a
≤ 0.05,0≤b≤0.05,0.2≤z≤0.8.
Bismuth layered composite structure piezoceramic material provided in an embodiment of the present invention, with very high Curie temperature, excellent
Piezoelectric property and adjustable comprehensive electrochemical properties, available for various high temperature piezoelectric devices.
Embodiment 2
The preparation method of laminated structure bismuth piezoelectric ceramic material in above-described embodiment 1 is present embodiments provided, such as Fig. 1 institutes
Show, including：
Step 201, by calcium carbonate, titanium oxide, bismuth oxide, niobium pentaoxide, lithium carbonate, manganese carbonate, and doped chemical Me
And/or Me ' oxide or salt, according to stoichiometric proportion Ca1-xMexBi2Nb2-2yMe’2yO9(referred to as CBN) and Bi3-aMea
(TiNb)1-bMe’2bO9(referred to as BTN), carries out weighing dispensing respectively, obtain the first original powder for preparing CBN and
Second of original powder for preparing BTN；
Wherein, Me and Me ' are respectively the doped chemical of suitable different crystalline lattice position, and Me is one kind or many in Li, Mn, Ce
Kind, Me ' is the one or more in Ta, W；X, y, z, a, b are respectively molar fraction, 0≤x≤0.05,0≤y≤0.05,0≤a
≤ 0.05,0≤b≤0.05,0.2≤z≤0.8.
Step 202, by the first described original powder and second of original powder respectively using water or ethanol as medium
Ball milling is carried out, the first slurry and the second slurry is obtained, and first slurry and the second slurry are respectively dried, ground and mistake
Sieve, obtains the first original powder and the second original powder；
Specifically, the sieving is specially：Sieved using the sieve of 150~200 mesh.
Step 203, the first original powder is placed in crucible and calcined, obtained with bismuth laminated CBN powders；By
Two original powders are placed in crucible and calcined, and obtain with bismuth laminated BTN powders；
Specifically, the temperature of calcining is 600 DEG C~900 DEG C, the time is 1.5~5 hours.
Step 204, by the CBN powders and the BTN powders, the ratio needed for is weighed after dispensing mixing, is added concentration and is
1wt%~6wt% PVAC polyvinylalcohol solution, ground in mortar it is uniform after, granulate and sieve and obtain mixed powder (referred to as
CBTN)；
Step 205, the CBTN is pressed into ceramic body；
Specifically, being 50MPa~150MPa for the pressure for suppressing CBTN formation ceramic bodies.
Step 206, the ceramic body is placed in into heating in crucible to carry out after dumping, piezoelectric ceramic body is made in sintering；
Specifically, the temperature of the sintering is 950 DEG C~1150 DEG C, the time is 2~6 hours.
Step 207, by after piezoelectric ceramic body polishing, polishing, coating metal electrode, heated in silicone oil and apply pole
Change voltage to be polarized, the piezoceramic material is obtained after cooling.
Specifically, the temperature of the polarization is 150 DEG C~200 DEG C, the electric-field intensity of polarization is 5kV/mm~15kV/mm,
The time of polarization is 10~30 minutes.
The preparation method for the piezoceramic material that the present embodiment is provided, its principle is based on two kinds of powder CBN and BTN difference
The single-phase thing of high-purity is can obtain during calcining synthesis, it is brilliant because the crystal structure of two kinds of systems is close in being re-sintered after mixing afterwards
Grain growth is not by mixed influence, so that the ceramic body that can be densified.Compared with current material system and technology of preparing, this hair
It is bright that there are many merits.Compound bismuth-containing lamination electroceramics prepared by the present invention has the microstructure of dense uniform, high phase
Purity and crystallinity, very high Curie temperature (TcUp to more than 900 DEG C), higher piezoelectric constant (d33Up to 18pC/N), it is adjustable
Dielectric properties (εr=100~500) etc., available for dependent piezoelectric devices such as the various sensors for needing operating temperature to be more than 600 DEG C
Part；In addition, the preparation technology of the compound bismuth-containing layer ceramic systems has preparation process easy, it is easy to control compound system component,
It is easy to large-scale industrialized production, it is with low cost, the advantages of product purity is high.Method and prepared high-temperature high-pressure that the present invention is provided
Electroceramics material has preferable application prospect.
The technical scheme provided for a better understanding of the present invention, it is following to be illustrated respectively using the present invention with multiple instantiations
The preparation method that above-described embodiment is provided prepares the detailed process of piezoceramic material, and its performance.
Embodiment 3
Using calcium carbonate, bismuth oxide, titanium oxide, niobium pentaoxide, lithium carbonate and manganese carbonate as raw material, according to chemical formula
Ca0.95Li0.025Mn0.025Bi2Nb2O9And Bi2.95Li0.02Mn0.03TiNbO9Dispensing is carried out respectively, by doping Li, Mn for preparing
CBN and doping Li, Mn BTN powders are respectively put into different ball grinders, using absolute ethyl alcohol as medium ball milling 10 hours, are then dried
Powder is respectively put into crucible by dry doubling, is calcined at 800 DEG C 3 hours, CBN and BTN powder is made respectively；Two kinds of powders are pressed
CBN0.7BTN0.3Ratio be mixed into agate mortar, add poly-vinyl alcohol solution and grind 20 minutes, cross ageing after 200 mesh sieves 10 small
When, a diameter of 1.2cm, the disk biscuit that thickness is about 1.2mm are pressed under 150MPa pressure.By after biscuit dumping
3 hours obtained CBTN compound systems ceramic bodies are sintered at 1020 DEG C.By following table on the CBTN compound system ceramic bodies of sanding and polishing
Face coats metal electrode, cools in 180 DEG C of silicone oil after being polarized 20 minutes under 8KV/mm electric fields, obtained piezoelectric ceramics sample
[Ca0.95Li0.025Mn0.025Bi2Nb2O9]0.7-[Bi2.95Li0.02Mn0.03TiNbO9]0.3, its piezoelectric modulus is 14pC/N, Ju Liwen
Spend Tc=911 DEG C, permittivity εrFor 445, dielectric loss is 0.0203.
[the Ca that the present embodiment is prepared0.95Li0.025Mn0.025Bi2Nb2O9]0.7-[Bi2.95Li0.02Mn0.03TiNbO9]0.3
Piezoelectric constant different temperatures anneal rear chamber temperature and pressure electric constant change curve as shown in Fig. 2 its stereoscan photograph such as Fig. 3
It is shown.
Embodiment 4
Using calcium carbonate, bismuth oxide, titanium oxide, niobium pentaoxide, lithium carbonate, manganese carbonate and tungsten oxide as raw material, by chemistry
Formula Ca0.96Li0.02Mn0.02Bi2Nb2O9And Bi2.98Li0.02(TiNb)0.998W0.004O9Dispensing is carried out respectively, by the doping prepared
LiMn CBN and doping LiW BTN raw material are respectively put into different ball grinders, using absolute ethyl alcohol as medium ball milling 10 hours,
Then dry and powder is respectively put into crucible, calcined at 850 DEG C 3 hours, CBN and BTN powder is made respectively；By two kinds of powder
Material presses CBN0.4BTN0.6Ratio be mixed into agate mortar, add poly-vinyl alcohol solution after grind 20 minutes.Sample crosses 200 mesh sieves
It is aged 10 hours afterwards, a diameter of 1.2cm, the disk biscuit that thickness is about 1.2mm is pressed under 100MPa pressure.Biscuit is arranged
3 hours obtained CBTN compound systems ceramic bodies are sintered after glue at 1050 DEG C.By the CBTN compound system ceramic bodies of sanding and polishing
Upper and lower surface applies and is covered with metal electrode, in being polarized 20 minutes under 8.5KV/mm electric fields in 180 DEG C of silicone oil, cools afterwards, makes
Piezoelectric ceramics sample [the Ca obtained0.96Li0.02Mn0.02Bi2Nb2O9]0.4-[Bi2.98Li0.02(TiNb)0.998W0.004O9]0.6Piezoelectricity
Coefficient is 9pC/N, Curie temperature Tc=913 DEG C, permittivity εrFor 351, dielectric loss is 0.0215.
Embodiment 5
Using calcium carbonate, bismuth oxide, titanium oxide, niobium pentaoxide, lithium carbonate, manganese carbonate and cerium oxide as raw material, according to change
Formula Ca0.96Li0.02Ce0.02Bi2Nb2O9And Bi2.98Li0.01Mn0.01TiNbO9Dispensing is carried out respectively, by the doping LiCe prepared
CBN and doping LiMn BTN raw materials be respectively put into different ball grinders, using absolute ethyl alcohol as medium ball milling 10 hours, then
Dry and powder is respectively put into crucible, calcined at 850 DEG C 3 hours, CBN and BTN powder is made respectively；Two kinds of powders are pressed
CBN0.5BTN0.5Ratio be mixed into agate mortar, add poly-vinyl alcohol solution after grind 20 minutes.Sample is crossed old after 200 mesh sieves
Change 10 hours, a diameter of 1.2cm, the disk biscuit that thickness is about 1.0mm are pressed under 100MPa pressure.Biscuit dumping
Afterwards, 3 hours obtained CBTN compound systems ceramic bodies are sintered at 1080 DEG C.By on the CBTN compound system ceramic bodies of sanding and polishing
Lower surface applies and is covered with metal electrode, cools in 180 DEG C of silicone oil after being polarized 20 minutes under 12KV/mm electric fields, obtained pressure
Electroceramics sample [Ca0.96Li0.02Ce0.02Bi2Nb2O9]0.5-[Bi2.98Li0.01Mn0.01TiNbO9]0.5Piezoelectric modulus be 18pC/
N, Curie temperature Tc=906 DEG C, permittivity εrFor 258, dielectric loss is 0.0313.
Embodiment 6
Using calcium carbonate, bismuth oxide, titanium oxide, niobium pentaoxide, lithium carbonate and tantalum oxide as raw material, according to chemical formula
Ca0.98Li0.02Bi2Nb1.995W0.005O9And Bi2.98Li0.02(TiNb)0.997Ta0.006O9Dispensing is carried out respectively, by the doping prepared
Li, W CBN and adulterate Li, Ta BTN raw material are respectively put into different ball grinders, and it is small to make medium ball milling 10 with absolute ethyl alcohol
When, then dry and powder is respectively put into crucible, calcined at 800 DEG C 3 hours, CBN and BTN powder is made respectively；By two
Plant powder and press CBN0.45BTN0.55Ratio be mixed into agate mortar, add poly-vinyl alcohol solution grind 20 minutes.Sample crosses 200
It is aged 10 hours after mesh sieve, a diameter of 1.2cm, the disk biscuit that thickness is about 1.2mm is pressed under 120MPa pressure.Element
3 hours obtained CBTN compound systems ceramic bodies are sintered after base dumping at 1080 DEG C.The CBTN compound systems of sanding and polishing are made pottery
Porcelain body upper and lower surface applies and is covered with metal electrode, cools in 180 DEG C of silicone oil after being polarized 20 minutes under 8KV/mm electric fields, is made
Piezoelectric ceramics sample [Ca0.98Li0.02Bi2Nb1.995W0.005O9]0.45-[Bi2.98Li0.02(TiNb)0.997Ta0.006O9]0.55Pressure
Electrostrictive coefficient is 11pC/N, Curie temperature Tc=899 DEG C, permittivity εrFor 121, dielectric loss is 0.019.
Embodiment 7
Using calcium carbonate, bismuth oxide, titanium oxide, niobium pentaoxide, lithium carbonate, cerium oxide and tantalum oxide as raw material, according to change
Formula Ca0.99Li0.01Bi2Nb1.997Ta0.003O9And Bi2.97Li0.01Ce0.02TiNbO9Dispensing is carried out respectively, by the doping prepared
Li, Ta CBN and adulterate Li, Ce BTN raw material are respectively put into different ball grinders, and it is small to make medium ball milling 10 with absolute ethyl alcohol
When, then dry and powder is respectively put into crucible, calcined at 850 DEG C 3 hours, CBN and BTN powder is made respectively；By two
Plant powder and press CBN0.3BTN0.7Ratio be mixed into agate mortar, add poly-vinyl alcohol solution grind 15 minutes.Sample crosses 200 mesh
It is aged 10 hours after sieve, a diameter of 1.2cm, the disk biscuit that thickness is about 1.2mm is pressed under 150MPa pressure.Biscuit
After dumping, 3 hours obtained CBTN compound systems ceramic bodies are sintered at 1100 DEG C.By the CBTN compound systems ceramics of sanding and polishing
Body upper and lower surface applies and is covered with metal electrode, cools in 180 DEG C of silicone oil after being polarized 20 minutes under 8.5KV/mm electric fields, is made
Piezoelectric ceramics sample [Ca0.99Li0.01Bi2Nb1.997Ta0.003O9]0.3-[Bi2.97Li0.01Ce0.02TiNbO9]0.7Piezoelectric modulus
For 12pC/N, Curie temperature Tc=901 DEG C, permittivity εrFor 261, dielectric loss is 0.0107.
Above example be premised on technical solution of the present invention under, the detailed implementation material component that provides and specific preparation
Technical process, but protection scope of the present invention is not limited to above-described embodiment.
The preparation method for the piezoceramic material that the present embodiment is provided, its principle is based on two kinds of powder CBN and BTN difference
The single-phase thing of high-purity is can obtain during calcining synthesis, it is brilliant because the crystal structure of two kinds of systems is close in being re-sintered after mixing afterwards
Grain growth is not by mixed influence, so that the ceramic body that can be densified.Compared with current material system and technology of preparing, this hair
It is bright that there are many merits.Compound bismuth-containing lamination electroceramics prepared by the present invention has the microstructure of dense uniform, high phase
Purity and crystallinity, very high Curie temperature (TcUp to more than 900 DEG C), higher piezoelectric constant (d33Up to 18pC/N), it is adjustable
Dielectric properties (εr=100~500) etc., available for dependent piezoelectrics such as the various sensors for needing operating temperature to be more than 600 DEG C
Device；In addition, the preparation technology of the compound bismuth-containing layer ceramic systems has preparation process easy, it is easy to control compound system group
Part, it is easy to large-scale industrialized production, it is with low cost, the advantages of product purity is high.Method and prepared height that the present invention is provided
Temperature and pressure electroceramics material has preferable application prospect.
Above-described embodiment, has been carried out further to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail, should be understood that the embodiment that the foregoing is only the present invention, be not intended to limit the present invention
Protection domain, within the spirit and principles of the invention, any modifications, equivalent substitutions and improvements done etc. all should be included
Within protection scope of the present invention.
Claims (7)
1. a kind of bismuth layered composite structure piezoceramic material, it is characterised in that the chemical general formula of the piezoceramic material is：
[Ca1-xMexBi2Nb2-2yMe’2yO9]1-z-[Bi3-aMea(TiNb)1-bMe’2bO9]z；
Wherein, Me and Me ' are respectively the doped chemical of suitable different crystalline lattice position, and Me is the one or more in Li, Mn, Ce,
Me ' is the one or more in Ta, W；X, y, z, a, b are respectively molar fraction, and 0 ＜ x≤0.05,0 ＜ y≤0.05,0 ＜ a≤
0.05,0 ＜ b≤0.05,0.2≤z≤0.8.
2. a kind of preparation method of piezoceramic material as described in above-mentioned claim 1, it is characterised in that the preparation method
Including：
By the oxide and Me ' of calcium carbonate, titanium oxide, bismuth oxide, niobium pentaoxide, lithium carbonate, manganese carbonate, and doped chemical Me
Oxide or salt, according to stoichiometric proportion Ca1-xMexBi2Nb2-2yMe’2yO9(referred to as CBN) and Bi3-aMea(TiNb)1- bMe’2bO9(referred to as BTN), carries out weighing dispensing respectively, obtains the first original powder for preparing CBN and for preparing
BTN second of original powder；Wherein, Me and Me ' are respectively the doped chemical of suitable different crystalline lattice position, and Me is Li, Mn, Ce
In one or more, Me ' be Ta, W in one or more；X, y, z, a, b are respectively molar fraction, 0 ＜ x≤0.05,0 ＜
Y≤0.05,0 ＜ a≤0.05,0 ＜ b≤0.05,0.2≤z≤0.8；
The first described original powder and second of original powder are subjected to ball milling using water or ethanol as medium respectively, obtained
First slurry and the second slurry, and first slurry and the second slurry are respectively dried, ground and sieved, obtain first original
Powder and the second original powder；
First original powder is placed in crucible and calcined, is obtained with bismuth laminated CBN powders；Second original powder is put
Calcine, obtained with bismuth laminated BTN powders in crucible；
By the CBN powders and the BTN powders, the ratio needed for is weighed after dispensing mixing, and addition concentration is 1wt%~6wt%
PVAC polyvinylalcohol solution, ground in mortar it is uniform after, granulate and sieve and obtain mixed powder (abbreviation CBTN)；
The CBTN is pressed into ceramic body；
The ceramic body is placed in into heating in crucible to carry out after dumping, piezoelectric ceramic body is made in sintering；
After piezoelectric ceramic body polishing, polishing, coating metal electrode, heated in silicone oil and apply polarizing voltage progress pole
Change, the piezoceramic material is obtained after cooling.
3. preparation method according to claim 2, it is characterised in that first original powder and the second original powder
The temperature of the calcining of material is 600 DEG C~900 DEG C, and the time is 1.5~5 hours.
4. preparation method according to claim 2, it is characterised in that sieving when obtaining the CBTN mixed powders is specific
For：
Sieved using the sieve of 150~200 mesh.
5. preparation method according to claim 2, it is characterised in that the pressure for suppressing CBTN formation ceramic bodies is
50MPa~150MPa.
6. preparation method according to claim 2, it is characterised in that the temperature of the sintering is 950 DEG C~1150 DEG C, when
Between be 2~6 hours.
7. preparation method according to claim 2, it is characterised in that the temperature of the polarization is 150 DEG C~200 DEG C, pole
The electric-field intensity of change is 5kV/mm~15kV/mm, and the time of polarization is 10~30 minutes.
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| CN105732022A (en) * | 2015-12-31 | 2016-07-06 | 中国科学院声学研究所 | Preparation method of piezoelectric ceramic with high Curie temperature and film thereof |
| CN106986629B (en) * | 2017-05-02 | 2020-04-14 | 北京理工大学 | Preparation method of bismuth titanate-based bismuth laminated structure ferroelectric ceramic target material |
| CN111933786A (en) * | 2020-08-17 | 2020-11-13 | 东莞传晟光电有限公司 | Pyroelectric sensor and manufacturing method thereof |
| CN114455944B (en) * | 2022-01-28 | 2022-11-11 | 厦门乃尔电子有限公司 | Bismuth layer-structured piezoelectric ceramic material and preparation method thereof |
| CN116462506A (en) * | 2023-04-14 | 2023-07-21 | 厦门乃尔电子有限公司 | Bismuth layered ceramic with excellent high-temperature insulation and piezoelectricity and preparation method thereof |
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