CN107244913A - A kind of combined high temperature piezoceramic material - Google Patents

A kind of combined high temperature piezoceramic material Download PDF

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CN107244913A
CN107244913A CN201710357002.XA CN201710357002A CN107244913A CN 107244913 A CN107244913 A CN 107244913A CN 201710357002 A CN201710357002 A CN 201710357002A CN 107244913 A CN107244913 A CN 107244913A
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tatio
bifeo
ceramic
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high temperature
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CN107244913B (en
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张伟飞
袁国亮
穆罕默德·阿德南·凯瑟
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Nanjing University of Science and Technology
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Abstract

The invention discloses a kind of combined high temperature piezoceramic material.The ceramic material composition is with Formula B i3TaTiO9‑xBiFeO3To represent, wherein x is BiFeO3With Bi3TaTiO9Percentage by weight, and x=20wt%~50wt%.The preparation process of the material is:Bi is respectively synthesized first3TaTiO9Powder and BiFeO3Powder, then by Bi3TaTiO9Ceramic powder and BiFeO3Ceramic powder ball milling mixing sinters porcelain into.The piezoelectric constant d of the combined high temperature piezoceramic material of the present invention3324pC/N is reached, is single-phase Bi3TaTiO91.8 times of ceramic material, have larger resistivity, ρ is about 10 under 500 DEG C of hot environments4Ω·m.The composite ceramic material of the present invention is applied to prepare the piezoelectric actuator and piezoelectric transducer used in high temperature environments.

Description

A kind of combined high temperature piezoceramic material
Technical field
The invention belongs to inorganic piezoelectric material technical field, it is related to a kind of combined high temperature piezoceramic material, and in particular to The compound lead-free piezoceramic material that a kind of hot environment field is used.
Background technology
With the fast development of the industry such as Aero-Space, automobile, metallurgical and petrochemical industry, jet engine, nuclear energy power generation Automatic monitoring, and numerous special dimensions such as the automatically controlling of space flight and aviation, satellite, guided missile, the monitoring of automobile engine fuel oil, All need the piezoelectric sensing device that can be worked at high temperature without failure badly.
Bismuth laminated high-temperature piezoelectric ceramics have the characteristics that as a kind of more high-temperature piezoelectric ceramics are studied:Compared with High Curie temperature, relatively low ageing rate, excellent insulaion resistance and voltage endurance, higher mechanical quality factor.Wherein Bi3TaTiO9It is used as typical laminated structure bismuth piezoelectric ceramic, about 850 DEG C of its ferroelectrie Curie temperature (Tc), the resistance at 500 DEG C Rate ρ is about 104Ω m, but the crystal characteristic of its tabular result in the ceramic piezoelectric constant d33It is relatively low, it is about 8pC/ under normal temperature N, seriously limits its application (Y.H.Suna, et al, Mater.Lett.175,79, (2016)) in the industry.
BiFeO3It is a kind of multi-ferroic material being widely studied, its structure is rhombohedron perovskite structure, and its Tc is about It it is 810 DEG C, while its piezoelectric constant d under normal temperature3340pC/N can be reached.But, in 400 DEG C and its temperatures above, BiFeO3Resistivity less than 103Ω m, limit it high-temperature piezoelectric ceramic field application (A.Perej ó n, et al, J.Eur.Ceram.Soc.35,2283(2015))。
The content of the invention
For existing Bi3TaTiO9The problem of piezoelectric constant is relatively low present in piezoelectric ceramics, the invention provides one kind Combined high temperature piezoceramic material.The combined high temperature piezoceramic material is by by Bi3TaTiO9Ceramic powder and BiFeO3Ceramics Powder is mixed in proportion, sinters be made at high temperature.
Technical scheme is as follows:
A kind of combined high temperature piezoceramic material, the ceramic component is Bi3TaTiO9-xBiFeO3, wherein x is BiFeO3With Bi3TaTiO9Percentage by weight, x=20wt%~50wt%.
Preferably, x=30wt%~40wt%.
Further, the present invention also provides the preparation method of above-mentioned combined high temperature piezoceramic material, first by initial former Expect Ta2O5、Bi2O3、TiO2Single-phase Bi is made3TaTiO9Nano particle, by Bi2O3、Fe2O3Single-phase BiFeO is made3Micron particles, Then by Bi3TaTiO9Nano particle and BiFeO3Combined high temperature piezoelectricity is made by ball milling, drying, Fast Sintering in micron particles Ceramic material, is comprised the following steps that:
Step 1, by Bi3TaTiO9Ceramic powder and BiFeO3Ceramic powder wet ball grinding, is well mixed it, dries To Bi3TaTiO9-xBiFeO3Powder, wherein x represent BiFeO3With Bi3TaTiO9Mass percent, x=20wt%~ 50wt%;
Step 2, in Bi3TaTiO9-xBiFeO3The poly-vinyl alcohol solution as binding agent is added in powder, is suppressed after grinding Into ceramic disks;
Step 3, by ceramic disks after 550 DEG C~650 DEG C insulations carry out dumping in 2~3 hours, with 50-100 DEG C/min's Heating rate rises to 750 DEG C~900 DEG C, sinters 1~2 hour, after terminating, room is down to 50-100 DEG C/min speed Temperature, is made combined high temperature piezoceramic material.
Preferably, in step 1, described Bi3TaTiO9Ceramic powder is prepared by following steps:By single-phase Bi3TaTiO9 Ceramic block ball milling 6~12 hours in rotating speed 300r/min ball mill, it is nanometer diameter that drying, which is obtained more than 80% particle, Bi3TaTiO9Ceramic powder.
Preferably, described Ball-milling Time is 8~10 hours.
Preferably, in step 1, described BiFeO3Ceramic powder is prepared by following steps:By single-phase BiFeO3Ceramic block Body ball milling 2~5 hours in rotating speed 300r/min ball mill, drying is obtained more than the BiFeO that 80% particle is micron diameter3 Ceramic powder.
Preferably, described Ball-milling Time is 3~4 hours.
Preferably, in step 3, described sintering temperature is 850 DEG C~900 DEG C.
The combined high temperature lead-free piezoceramic material of the present invention has 0-3 type composite constructions, with Bi3TaTiO9Ceramic material As the continuous matrix of three-dimensional in composite, while by BiFeO3Ceramic material is distributed in inside three dimensional matrix, makes BiFeO3 Ceramic particle isolates each other in intrinsic silicon.
The piezoelectric constant d of the compound piezoceramic material of the present invention3324pC/N is reached, relative to single-phase Bi3TaTiO9Pressure Electroceramics material (d33=13pC/N) it is obviously improved, and the composite ceramic material is by controlling BiFeO3With Bi3TaTiO9Ratio Example, even in the BiFeO for being compounded with low-resistivity3Afterwards, composite remains to keep larger piezoelectric constant under 500 DEG C of high temperature (d33=24pC/N) and larger resistivity (ρ ≈ 104Ω·m)。
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrum of the ceramics sample of embodiment 1 to 11.
Fig. 2 is piezoelectric constant of the ceramics sample of embodiment 2 to 11 under different annealing temperature.
Fig. 3 is the resistivity of the ceramics sample of embodiment 3 to 11 at different temperatures.
Embodiment
With reference to embodiment and accompanying drawing, the invention will be further described.
Embodiment 1
BiFeO3The preparation of ceramic powder is referred to【G.L.Yuan,S.W.Or,Y.P.Wang,Z.G.Liu,and J.M.Liu,Solid State Commun.138,76(2006).】
The present embodiment is with Bi2O3、Fe2O3Powder prepares BiFeO3Ceramics.Ball milling 8 is small in rotating speed 300r/min ball mill When and dry, obtain more than 80% particle be micron diameter BiFeO3Ceramic powder.
With X-ray diffractometer to BiFeO made from the present embodiment3Ceramics sample is analyzed.As a result as shown in figure 1, table Bright BiFeO3Ceramic well-crystallized.
Embodiment 2
Bi3TaTiO9The preparation of ceramic powder is referred to【Y.Noguchi,R.Satoh,M.Miyayama, K.Tetsuichi,J.Ceram.Soc.Jpn.109,29(2001)】
The present embodiment is with Ta2O5、Bi2O3、TiO2Powder prepares Bi3TaTiO9Ceramics.In rotating speed 300r/min ball mill Middle ball milling 4 hours is simultaneously dried, and is obtained more than the Bi that 80% particle is nanometer diameter3TaTiO9Ceramic powder.And by burned ceramics The upper and lower surface of piece sample paints silver electrode, is placed in methyl-silicone oil, increases piezoelectric field and is polarized, and polarized electric field is 150kV/ Cm, the polarization time is 30 minutes.
With X-ray diffractometer to Bi made from the present embodiment3TaTiO9Ceramics sample is analyzed.As a result as shown in figure 1, Show the ceramic well-crystallized.
Use quasistatic d33Tester is to the Bi after the present embodiment polarization3TaTiO9Ceramics sample is tested, while not Tested after synthermal annealing.As a result as shown in Fig. 2 d when measuring 20 DEG C of the ceramics sample of 0.6 millimeter of thickness33=13pC/N, After 500 DEG C are annealed, piezoelectric constant when remaining in that its 20 DEG C.
With high temperature four-point probe measurment system to the present embodiment Bi3TaTiO9Ceramics sample is tested.Measure the ceramics sample Resistivity at 20 DEG C is about 109Ω m, the resistivity at 500 DEG C is about 104Ω·m。
Embodiment 3
The present embodiment is with the BiFeO of embodiment 13The Bi of powder and embodiment 23TaTiO9Powder prepares Bi3TaTiO9- 20wt%BiFeO3Ceramics, sintering temperature is 750 DEG C.
Preparation process is:
1. by the BiFeO in embodiment 13Bi in ceramic powder and embodiment 23TaTiO9Ceramic powder, according to Bi3TaTiO9- 20wt%BiFeO3Weighed, be put into low speed ball milling 1 hour in planetary ball mill.
2. slurry is taken out, dried by ball milling after terminating, in Bi3TaTiO9- 20wt%BiFeO3Polyvinyl alcohol is added in powder Solution is pressed into ceramic disks as binding agent after regrinding.
3. the ceramic disks suppressed are raised into temperature after 550 DEG C of insulations carry out dumping in 3 hours with 80 DEG C/min speed Degree is to 750 DEG C of sintering, and soaking time is 1 hour, and with 80 DEG C/min rate reduction temperature to room temperature, ceramics sample is made. The sample number into spectrum is No. 1.
4. the upper and lower surface of potsherd burned in step 3 is painted into silver electrode, it is placed in methyl-silicone oil, increases piezoelectric field Polarized, polarized electric field is 150kV/cm, the polarization time is 30 minutes.
Bi after being sintered with X-ray diffractometer to the present embodiment3TaTiO9- 20wt%BiFeO3Ceramics sample is analyzed. As a result as shown in Fig. 11, the ceramic well-crystallized is shown.
Use quasistatic d33Tester is to the Bi after the present embodiment polarization3TaTiO9- 20wt%BiFeO3Ceramics sample is surveyed Examination, while being tested after different temperatures annealing.As a result as shown in Fig. 2 when measuring 20 DEG C of the ceramics sample of 0.6 millimeter of thickness d33=15pC/N, after 500 DEG C are annealed, piezoelectric constant when remaining in that its 20 DEG C.
With high temperature four-point probe measurment system to the present embodiment Bi3TaTiO9- 20wt%BiFeO3Ceramics sample is tested. As a result as shown in Fig. 31, resistivity when measuring 20 DEG C of the ceramics sample is about 109Ω m, the resistivity at 500 DEG C is about For 104Ω·m。
Embodiment 4
The present embodiment is with the BiFeO of embodiment 13The Bi of powder and embodiment 23TaTiO9Powder prepares Bi3TaTiO9- 40wt%BiFeO3Ceramics, sintering temperature is 750 DEG C.
Preparation process is:
1. by the BiFeO in embodiment 13Bi in ceramic powder and embodiment 23TaTiO9Ceramic powder, according to Bi3TaTiO9- 40wt%BiFeO3Weighed, be put into low speed ball milling 1 hour in planetary ball mill.
2. slurry is taken out, dried by ball milling after terminating, in Bi3TaTiO9- 40wt%BiFeO3Polyvinyl alcohol is added in powder Solution is as binding agent, press ceramic disk after regrinding.
3. the ceramic disks suppressed are raised into temperature after 600 DEG C of insulations carry out dumping in 2 hours with 80 DEG C/min speed Degree is to 750 DEG C of sintering, and soaking time is 1 hour, and with 80 DEG C/min rate reduction temperature to room temperature, ceramics sample is made. The sample number into spectrum is No. 2.
4. the upper and lower surface of potsherd burned in step 3 is painted into silver electrode, it is placed in methyl-silicone oil, increases piezoelectric field Polarized, polarized electric field is 150kV/cm, the polarization time is 30 minutes.
Bi after being sintered with X-ray diffractometer to the present embodiment3TaTiO9- 40wt%BiFeO3Ceramics sample is analyzed. As a result as shown in Fig. 12, the ceramic well-crystallized is shown.
Use quasistatic d33Tester is to the Bi after the present embodiment polarization3TaTiO9- 40wt%BiFeO3Ceramics sample is surveyed Examination, while being tested after different temperatures annealing.As a result as shown in Fig. 2 when measuring 20 DEG C of the ceramics sample of 0.6 millimeter of thickness d33=23pC/N, after 500 DEG C are annealed, piezoelectric constant when remaining in that its 20 DEG C.
With high temperature four-point probe measurment system to the present embodiment Bi3TaTiO9- 40wt%BiFeO3Ceramics sample is tested. As a result as shown in Fig. 32, resistivity when measuring 20 DEG C of the ceramics sample is about 109Ω m, the resistivity at 500 DEG C is about For 104Ω·m。
Embodiment 5
The present embodiment is with the BiFeO of embodiment 13The Bi of powder and embodiment 23TaTiO9Powder prepares Bi3TaTiO9- 50wt%BiFeO3Ceramics, sintering temperature is 750 DEG C.
Preparation process is:
1. by the BiFeO in embodiment 13Bi in ceramic powder and embodiment 23TaTiO9Ceramic powder, according to Bi3TaTiO9- 50wt%BiFeO3Weighed, be put into low speed ball milling 1 hour in planetary ball mill.
2. slurry is taken out, dried by ball milling after terminating, in Bi3TaTiO9- 50wt%BiFeO3Polyvinyl alcohol is added in powder Solution is pressed into ceramic disks as binding agent after regrinding.
3. the ceramic disks suppressed are raised after 600 DEG C of insulations carry out dumping in 2 hours with 100 DEG C/min speed Temperature is to 750 DEG C of sintering, and soaking time is 1 hour, and with 100 DEG C/min rate reduction temperature to room temperature, Ceramic Like is made Product.The sample number into spectrum is No. 3.
4. the upper and lower surface of potsherd burned in step 3 is painted into silver electrode, it is placed in methyl-silicone oil, increases piezoelectric field Polarized, polarized electric field is 150kV/cm, the polarization time is 30 minutes.
Bi after being sintered with X-ray diffractometer to the present embodiment3TaTiO9- 50wt%BiFeO3Ceramics sample is analyzed. As a result as shown in Fig. 13, the ceramic well-crystallized is shown.
Use quasistatic d33Tester is to the Bi after the present embodiment polarization3TaTiO9- 50wt%BiFeO3Ceramics sample is surveyed Examination, while being tested after different temperatures annealing.As a result as shown in Fig. 2 when measuring 20 DEG C of the ceramics sample of 0.6 millimeter of thickness d33=19pC/N, after 500 DEG C are annealed, piezoelectric constant when remaining in that its 20 DEG C.
With high temperature four-point probe measurment system to the present embodiment Bi3TaTiO9- 50wt%BiFeO3Ceramics sample is tested. As a result as shown in Fig. 33, resistivity when measuring 20 DEG C of the ceramics sample is about 109Ω m, the resistivity at 500 DEG C is about For 104Ω·m。
Embodiment 6
The present embodiment is with the BiFeO of embodiment 13The Bi of powder and embodiment 23TaTiO9Powder prepares Bi3TaTiO9- 20wt%BiFeO3Ceramics, sintering temperature is 820 DEG C.
Preparation process is:
1. by the BiFeO in embodiment 13Bi in ceramic powder and embodiment 23TaTiO9Ceramic powder, according to Bi3TaTiO9- 20wt%BiFeO3Weighed, be put into low speed ball milling 1 hour in planetary ball mill.
2. slurry is taken out, dried by ball milling after terminating, in Bi3TaTiO9- 20wt%BiFeO3Polyvinyl alcohol is added in powder Solution is pressed into ceramic disks as binding agent after regrinding.
3. the ceramic disks suppressed are raised into temperature after 650 DEG C of insulations carry out dumping in 2 hours with 80 DEG C/min speed Degree is to 820 DEG C of sintering, and soaking time is 2 hours, and with 80 DEG C/min rate reduction temperature to room temperature, ceramics sample is made. The sample number into spectrum is No. 4.
4. the upper and lower surface of potsherd burned in step 3 is painted into silver electrode, it is placed in methyl-silicone oil, increases piezoelectric field Polarized, polarized electric field is 150kV/cm, the polarization time is 30 minutes.
Bi after being sintered with X-ray diffractometer to the present embodiment3TaTiO9- 20wt%BiFeO3Ceramics sample is analyzed. As a result as shown in Fig. 14, the ceramic well-crystallized is shown.
Use quasistatic d33Tester is to the Bi after the present embodiment polarization3TaTiO9- 20wt%BiFeO3Ceramics sample is surveyed Examination, while being tested after different temperatures annealing.As a result as shown in Fig. 2 when measuring 20 DEG C of the ceramics sample of 0.6 millimeter of thickness d33=15pC/N, after 500 DEG C are annealed, piezoelectric constant when remaining in that its 20 DEG C.
With high temperature four-point probe measurment system to the present embodiment Bi3TaTiO9- 20wt%BiFeO3Ceramics sample is tested. As a result as shown in Fig. 34, resistivity when measuring 20 DEG C of the ceramics sample is about 109Ω m, the resistivity at 500 DEG C is about For 104Ω·m。
Embodiment 7
The present embodiment is with the BiFeO of embodiment 13The Bi of powder and embodiment 23TaTiO9Powder prepares Bi3TaTiO9- 40wt%BiFeO3Ceramics, sintering temperature is 820 DEG C.
Preparation process is:
1. by the BiFeO in embodiment 13Bi in ceramic powder and embodiment 23TaTiO9Ceramic powder, according to Bi3TaTiO9- 40wt%BiFeO3Weighed, be put into low speed ball milling 1 hour in planetary ball mill.
2. slurry is taken out, dried by ball milling after terminating, in Bi3TaTiO9- 40wt%BiFeO3Polyvinyl alcohol is added in powder Solution is pressed into ceramic disks as binding agent after regrinding.
3. the ceramic disks suppressed are raised into temperature after 600 DEG C of insulations carry out dumping in 2 hours with 80 DEG C/min speed Degree is to 820 DEG C of sintering, and soaking time is 1 hour, and with 80 DEG C/min rate reduction temperature to room temperature, ceramics sample is made. The sample number into spectrum is No. 5.
4. the upper and lower surface of potsherd burned in step 3 is painted into silver electrode, it is placed in methyl-silicone oil, increases piezoelectric field Polarized, polarized electric field is 150kV/cm, the polarization time is 30 minutes.
Bi after being sintered with X-ray diffractometer to the present embodiment3TaTiO9- 40wt%BiFeO3Ceramics sample is analyzed. As a result as shown in Fig. 15, the ceramic well-crystallized is shown.
Use quasistatic d33Tester is to the Bi after the present embodiment polarization3TaTiO9- 40wt%BiFeO3Ceramics sample is surveyed Examination, while being tested after different temperatures annealing.As a result as shown in Fig. 2 when measuring 20 DEG C of the ceramics sample of 0.6 millimeter of thickness d33=24pC/N, after 500 DEG C are annealed, piezoelectric constant when remaining in that its 20 DEG C.
With high temperature four-point probe measurment system to the present embodiment Bi3TaTiO9- 40wt%BiFeO3Ceramics sample is tested. As a result as shown in Fig. 35, resistivity when measuring 20 DEG C of the ceramics sample is about 109Ω m, the resistivity at 500 DEG C is about For 104Ω·m。
Embodiment 8
The present embodiment is with the BiFeO of embodiment 13The Bi of powder and embodiment 23TaTiO9Powder prepares Bi3TaTiO9- 50wt%BiFeO3Ceramics, sintering temperature is 820 DEG C.
Preparation process is:
1. by the BiFeO in embodiment 13Bi in ceramic powder and embodiment 23TaTiO9Ceramic powder, according to Bi3TaTiO9- 50wt%BiFeO3Weighed, be put into low speed ball milling 1 hour in planetary ball mill.
2. slurry is taken out, dried by ball milling after terminating, in Bi3TaTiO9- 50wt%BiFeO3Polyvinyl alcohol is added in powder Solution is pressed into ceramic disks as binding agent after regrinding.
3. the ceramic disks suppressed are raised into temperature after 600 DEG C of insulations carry out dumping in 2 hours with 80 DEG C/min speed Degree is to 820 DEG C of sintering, and soaking time is 1 hour, and with 80 DEG C/min rate reduction temperature to room temperature, ceramics sample is made. The sample number into spectrum is No. 6.
4. the upper and lower surface of potsherd burned in step 3 is painted into silver electrode, it is placed in methyl-silicone oil, increases piezoelectric field Polarized, polarized electric field is 150kV/cm, the polarization time is 30 minutes.
Bi after being sintered with X-ray diffractometer to the present embodiment3TaTiO9- 50wt%BiFeO3Ceramics sample is analyzed. As a result as shown in Fig. 16, the ceramic well-crystallized is shown.
Use quasistatic d33Tester is to the Bi after the present embodiment polarization3TaTiO9- 50wt%BiFeO3Ceramics sample is surveyed Examination, while being tested after different temperatures annealing.As a result as shown in Fig. 2 when measuring 20 DEG C of the ceramics sample of 0.6 millimeter of thickness d33=21pC/N, after 500 DEG C are annealed, piezoelectric constant when remaining in that its 20 DEG C.
With high temperature four-point probe measurment system to the present embodiment Bi3TaTiO9- 50wt%BiFeO3Ceramics sample is tested. As a result as shown in Fig. 36, resistivity when measuring 20 DEG C of the ceramics sample is about 109Ω m, the resistivity at 500 DEG C is about For 104Ω·m。
Embodiment 9
The present embodiment is with the BiFeO of embodiment 13The Bi of powder and embodiment 23TaTiO9Powder prepares Bi3TaTiO9- 20wt%BiFeO3Ceramics, sintering temperature is 900 DEG C.
Preparation process is:
1. by the BiFeO in embodiment 13Bi in ceramic powder and embodiment 23TaTiO9Ceramic powder, according to Bi3TaTiO9- 20wt%BiFeO3Weighed, be put into low speed ball milling 1 hour in planetary ball mill.
2. slurry is taken out, dried by ball milling after terminating, in Bi3TaTiO9- 20wt%BiFeO3Polyvinyl alcohol is added in powder Solution is pressed into ceramic disks as binding agent after regrinding.
3. the ceramic disks suppressed are raised into temperature after 600 DEG C of insulations carry out dumping in 2 hours with 50 DEG C/min speed Degree is to 900 DEG C of sintering, and soaking time is 1 hour, and with 50 DEG C/min rate reduction temperature to room temperature, ceramics sample is made. The sample number into spectrum is No. 7.
4. the upper and lower surface of potsherd burned in step 3 is painted into silver electrode, it is placed in methyl-silicone oil, increases piezoelectric field Polarized, polarized electric field is 150kV/cm, the polarization time is 30 minutes.
Bi after being sintered with X-ray diffractometer to the present embodiment3TaTiO9- 20wt%BiFeO3Ceramics sample is analyzed. As a result as shown in Fig. 17, the ceramic well-crystallized is shown.
Use quasistatic d33Tester is to the Bi after the present embodiment polarization3TaTiO9- 20wt%BiFeO3Ceramics sample is surveyed Examination, while being tested after different temperatures annealing.As a result as shown in Fig. 2 when measuring 20 DEG C of the ceramics sample of 0.6 millimeter of thickness d33=16pC/N, after 500 DEG C are annealed, piezoelectric constant when remaining in that its 20 DEG C.
With high temperature four-point probe measurment system to the present embodiment Bi3TaTiO9- 20wt%BiFeO3Ceramics sample is tested. As a result as shown in Fig. 37, resistivity when measuring 20 DEG C of the ceramics sample is about 109Ω m, the resistivity at 500 DEG C is about For 104Ω·m。
Embodiment 10
The present embodiment is with the BiFeO of embodiment 13The Bi of powder and embodiment 23TaTiO9Powder prepares Bi3TaTiO9- 40wt%BiFeO3Ceramics, sintering temperature is 900 DEG C.
Preparation process is:
1. by the BiFeO in embodiment 13Bi in ceramic powder and embodiment 23TaTiO9Ceramic powder, according to Bi3TaTiO9- 40wt%BiFeO3Weighed, be put into low speed ball milling 1 hour in planetary ball mill.
2. slurry is taken out, dried by ball milling after terminating, in Bi3TaTiO9- 40wt%BiFeO3Polyvinyl alcohol is added in powder Solution is pressed into ceramic disks as binding agent after regrinding.
3. the ceramic disks suppressed are raised into temperature after 600 DEG C of insulations carry out dumping in 2 hours with 80 DEG C/min speed Degree is to 900 DEG C of sintering, and soaking time is 1 hour, and with 80 DEG C/min rate reduction temperature to room temperature, ceramics sample is made. The sample number into spectrum is No. 8.
4. the upper and lower surface of potsherd burned in step 3 is painted into silver electrode, it is placed in methyl-silicone oil, increases piezoelectric field Polarized, polarized electric field is 150kV/cm, the polarization time is 30 minutes.
Bi after being sintered with X-ray diffractometer to the present embodiment3TaTiO9- 40wt%BiFeO3Ceramics sample is analyzed. As a result as shown in Fig. 18, the ceramic well-crystallized is shown.
Use quasistatic d33Tester is to the Bi after the present embodiment polarization3TaTiO9- 40wt%BiFeO3Ceramics sample is surveyed Examination, while being tested after different temperatures annealing.As a result as shown in Fig. 2 when measuring 20 DEG C of the ceramics sample of 0.6 millimeter of thickness d33=22pC/N, after 500 DEG C are annealed, piezoelectric constant when remaining in that its 20 DEG C.
With high temperature four-point probe measurment system to the present embodiment Bi3TaTiO9- 40wt%BiFeO3Ceramics sample is tested. As a result as shown in Fig. 38, resistivity when measuring 20 DEG C of the ceramics sample is about 109Ω m, the resistivity at 500 DEG C is about For 104Ω·m。
Embodiment 11
The present embodiment is with the BiFeO of embodiment 13The Bi of powder and embodiment 23TaTiO9Powder prepares Bi3TaTiO9- 50wt%BiFeO3Ceramics, sintering temperature is 900 DEG C.
Preparation process is:1. by the BiFeO in embodiment 13Bi in ceramic powder and embodiment 23TaTiO9Ceramic powder Body, according to Bi3TaTiO9- 50wt%BiFeO3Weighed, be put into low speed ball milling 1 hour in planetary ball mill.
2. slurry is taken out, dried by ball milling after terminating, in Bi3TaTiO9- 50wt%BiFeO3Powder gross weight is added in powder 1wt% poly-vinyl alcohol solution is measured as binding agent, ceramic disks are pressed into after regrinding.
3. the ceramic disks suppressed are raised into temperature after 600 DEG C of insulations carry out dumping in 2 hours with 80 DEG C/min speed Degree is to 900 DEG C of sintering, and soaking time is 1 hour, and with 80 DEG C/min rate reduction temperature to room temperature, ceramics sample is made. The sample number into spectrum is No. 9.
4. the upper and lower surface of potsherd burned in step 3 is painted into silver electrode, it is placed in methyl-silicone oil, increases piezoelectric field Polarized, polarized electric field is 150kV/cm, the polarization time is 30 minutes.
Bi after being sintered with X-ray diffractometer to the present embodiment3TaTiO9- 50wt%BiFeO3Ceramics sample is analyzed. As a result as shown in Fig. 19, the ceramic well-crystallized is shown.
Use quasistatic d33Tester is to the Bi after the present embodiment polarization3TaTiO9- 50wt%BiFeO3Ceramics sample is surveyed Examination, while being tested after different temperatures annealing.As a result as shown in Fig. 2 when measuring 20 DEG C of the ceramics sample of 0.6 millimeter of thickness d33=18pC/N, after 500 DEG C are annealed, piezoelectric constant when remaining in that its 20 DEG C.
With high temperature four-point probe measurment system to the present embodiment Bi3TaTiO9- 50wt%BiFeO3Ceramics sample is tested. As a result as shown in Fig. 39, resistivity when measuring 20 DEG C of the ceramics sample is about 109Ω m, the resistivity at 500 DEG C is about For 104Ω·m。

Claims (8)

1. a kind of combined high temperature piezoceramic material, it is characterised in that described ceramic component is Bi3TaTiO9-xBiFeO3, Wherein x is BiFeO3With Bi3TaTiO9Percentage by weight, x=20wt%~50wt%.
2. combined high temperature piezoceramic material according to claim 1, it is characterised in that x=30wt%~40wt%.
3. the preparation method of combined high temperature piezoceramic material according to claim 1 or 2, it is characterised in that specific step It is rapid as follows:
Step 1, by Bi3TaTiO9Ceramic powder and BiFeO3Ceramic powder wet ball grinding, is well mixed it, drying is obtained Bi3TaTiO9-xBiFeO3Powder, wherein x represent BiFeO3With Bi3TaTiO9Mass percent, x=20wt%~50wt%;
Step 2, in Bi3TaTiO9-xBiFeO3Added in powder and pottery is pressed into after the poly-vinyl alcohol solution as binding agent, grinding Porcelain disk;
Step 3, by ceramic disks after 550 DEG C~650 DEG C insulations carry out dumping in 2~3 hours, with 50-100 DEG C/min heating Speed rises to 750 DEG C~900 DEG C, sinters 1~2 hour, after terminating, room temperature is down to 50-100 DEG C/min speed, makes Obtain combined high temperature piezoceramic material.
4. preparation method according to claim 3, it is characterised in that in step 1, described Bi3TaTiO9Ceramic powder leads to Cross following steps preparation:By single-phase Bi3TaTiO9Ceramic block ball milling 6~12 hours in rotating speed 300r/min ball mill, dry It is dry to obtain more than the Bi that 80% particle is nanometer diameter3TaTiO9Ceramic powder.
5. preparation method according to claim 4, it is characterised in that described Ball-milling Time is 8~10 hours.
6. preparation method according to claim 3, it is characterised in that in step 1, described BiFeO3Ceramic powder passes through It is prepared by following steps:By single-phase BiFeO3Ceramic block ball milling 2~5 hours in rotating speed 300r/min ball mill, are dried To more than the BiFeO that 80% particle is micron diameter3Ceramic powder.
7. preparation method according to claim 6, it is characterised in that described Ball-milling Time is 3~4 hours.
8. preparation method according to claim 3, it is characterised in that in step 3, described sintering temperature for 850 DEG C~ 900℃。
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