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

A kind of combined high temperature piezoceramic material Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
tatio
bifeo
ceramic
powder
high temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710357002.XA
Other languages
Chinese (zh)
Other versions
CN107244913B (en
Inventor
张伟飞
袁国亮
穆罕默德·阿德南·凯瑟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing University of Science and Technology
Original Assignee
Nanjing University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing University of Science and Technology filed Critical Nanjing University of Science and Technology
Priority to CN201710357002.XA priority Critical patent/CN107244913B/en
Publication of CN107244913A publication Critical patent/CN107244913A/en
Application granted granted Critical
Publication of CN107244913B publication Critical patent/CN107244913B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C04B35/475—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on bismuth titanates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Inorganic Chemistry (AREA)

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℃。
CN201710357002.XA 2017-05-19 2017-05-19 Composite high-temperature piezoelectric ceramic material Active CN107244913B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710357002.XA CN107244913B (en) 2017-05-19 2017-05-19 Composite high-temperature piezoelectric ceramic material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710357002.XA CN107244913B (en) 2017-05-19 2017-05-19 Composite high-temperature piezoelectric ceramic material

Publications (2)

Publication Number Publication Date
CN107244913A true CN107244913A (en) 2017-10-13
CN107244913B CN107244913B (en) 2020-06-30

Family

ID=60017609

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710357002.XA Active CN107244913B (en) 2017-05-19 2017-05-19 Composite high-temperature piezoelectric ceramic material

Country Status (1)

Country Link
CN (1) CN107244913B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109796205A (en) * 2019-02-20 2019-05-24 山东大学 A kind of bismuth laminated titanium bismuth tantalate high temperature piezoceramics and preparation method thereof
CN112313808A (en) * 2018-06-21 2021-02-02 爱奥尼克斯先进科技有限公司 Method for annealing polarized ceramics
CN115385684A (en) * 2022-09-20 2022-11-25 南京大学 Method for regulating and controlling microstructure and property of Ti-based perovskite ferroelectric ceramic

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1287988A (en) * 1999-08-16 2001-03-21 株式会社村田制作所 Method for mfg. piezoelectric ceramics
CN101607818A (en) * 2009-07-06 2009-12-23 扬州大学 Has laminate structure ferrotianium cobalt acid bismuth stupalith of multi-ferrum property and preparation method thereof
KR20110123566A (en) * 2010-05-07 2011-11-15 호서대학교 산학협력단 Lead-free piezoelectric ceramic composition
CN106565235A (en) * 2016-10-18 2017-04-19 南京理工大学 Composite high temperature piezoelectric ceramic material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1287988A (en) * 1999-08-16 2001-03-21 株式会社村田制作所 Method for mfg. piezoelectric ceramics
CN101607818A (en) * 2009-07-06 2009-12-23 扬州大学 Has laminate structure ferrotianium cobalt acid bismuth stupalith of multi-ferrum property and preparation method thereof
KR20110123566A (en) * 2010-05-07 2011-11-15 호서대학교 산학협력단 Lead-free piezoelectric ceramic composition
CN106565235A (en) * 2016-10-18 2017-04-19 南京理工大学 Composite high temperature piezoelectric ceramic material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YANHUI SUN ET AL.: "Lead free Bi3TaTiO9 ferroelectric ceramics with high Curie point", 《MATERIALS LETTERS》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112313808A (en) * 2018-06-21 2021-02-02 爱奥尼克斯先进科技有限公司 Method for annealing polarized ceramics
CN109796205A (en) * 2019-02-20 2019-05-24 山东大学 A kind of bismuth laminated titanium bismuth tantalate high temperature piezoceramics and preparation method thereof
CN115385684A (en) * 2022-09-20 2022-11-25 南京大学 Method for regulating and controlling microstructure and property of Ti-based perovskite ferroelectric ceramic
CN115385684B (en) * 2022-09-20 2023-04-07 南京大学 Method for regulating and controlling microstructure and property of Ti-based perovskite ferroelectric ceramic

Also Published As

Publication number Publication date
CN107244913B (en) 2020-06-30

Similar Documents

Publication Publication Date Title
Kim et al. Effect of bismuth of oxide content on the sintering of zinc oxide
CN107244913A (en) A kind of combined high temperature piezoceramic material
CN106631007B (en) A kind of high temperature, high-performance, the laminated structure bismuth piezoelectric ceramic material of high stability and its application
CN108675769B (en) Lithium-containing hexahydric medium-temperature negative temperature coefficient thermistor material
CN113387697A (en) Sodium bismuth titanate-based ceramic material with high ferroelectric stability, ultra-fast charge and discharge and high energy storage efficiency and preparation method thereof
CN110498682A (en) A kind of temperature-stable high-temperature ceramic capacitor dielectric material and preparation method thereof
CN110330332A (en) A kind of no sintering aid low-temperature melt piezoelectric ceramic material and preparation method thereof
CN109970443B (en) Rubidium and cerium co-doped bismuth calcium niobate based high-temperature piezoelectric ceramic and preparation method thereof
CN105060879A (en) Sodium bismuth titanate based lead-free piezoelectric ceramic material having high dielectric property
CN113213918B (en) Strontium bismuth titanate-bismuth scandium acid-lead titanate series high-temperature piezoelectric ceramic material with high piezoelectric performance and low loss and preparation method thereof
CN114478006A (en) KNNS-BNZ + CuO piezoceramic material and preparation method and application thereof
CN107903055B (en) Gradient doped sodium bismuth titanate based multilayer lead-free piezoelectric ceramic
CN109020541B (en) High-performance environment-friendly capacitor dielectric and preparation method thereof
CN106565235B (en) Composite high-temperature piezoelectric ceramic material and preparation method thereof
CN108101537A (en) A kind of nanometer of piezoelectric ceramics energy collection material and preparation method thereof
JP2007119269A (en) Piezoelectric ceramic composition and piezoelectric element
CN115385683B (en) Piezoelectric ceramic material with high Curie temperature and high piezoelectric coefficient and preparation method thereof
JP4247936B2 (en) Piezoelectric ceramic composition
CN113979728A (en) Preparation method of double perovskite type and yttrium oxide compounded negative temperature coefficient thermistor material
CN1759455A (en) A ceramic mixture having negative temperature co-efficient, a thermistor containing the ceramic mixture and a process for prepaing thereof
CN116751052B (en) Bismuth layered structure piezoelectric ceramic material and preparation method and application thereof
CN106986633A (en) A kind of piezoelectric ceramics and preparation method and application
CN116730722B (en) Perovskite type potassium-sodium niobate-based ceramic and preparation method thereof
CN108439970B (en) Rare earth doped perovskite type NTC composite thermosensitive ceramic material and preparation method thereof
CN114716241B (en) High-voltage ceramic dielectric material and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant