CN109503158A - 一种耐温度冲击的压电陶瓷材料及其制备方法 - Google Patents

一种耐温度冲击的压电陶瓷材料及其制备方法 Download PDF

Info

Publication number
CN109503158A
CN109503158A CN201811539037.6A CN201811539037A CN109503158A CN 109503158 A CN109503158 A CN 109503158A CN 201811539037 A CN201811539037 A CN 201811539037A CN 109503158 A CN109503158 A CN 109503158A
Authority
CN
China
Prior art keywords
temperature
resistance
follows
piezoceramic material
stabilizer
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
CN201811539037.6A
Other languages
English (en)
Other versions
CN109503158B (zh
Inventor
张元松
褚涛
张静
燕周民
赖炜
龙香楷
高智红
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.)
GUIZHOU ZHENHUA HONGYUN ELECTRONICS CO Ltd
Original Assignee
GUIZHOU ZHENHUA HONGYUN ELECTRONICS CO Ltd
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 GUIZHOU ZHENHUA HONGYUN ELECTRONICS CO Ltd filed Critical GUIZHOU ZHENHUA HONGYUN ELECTRONICS CO Ltd
Priority to CN201811539037.6A priority Critical patent/CN109503158B/zh
Publication of CN109503158A publication Critical patent/CN109503158A/zh
Application granted granted Critical
Publication of CN109503158B publication Critical patent/CN109503158B/zh
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
    • C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/49—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
    • C04B35/491—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
    • C04B35/493—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT containing also other lead compounds
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • C04B41/5116—Ag or Au
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/88—Metals
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/09—Forming piezoelectric or electrostrictive materials
    • H10N30/092—Forming composite materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/09—Forming piezoelectric or electrostrictive materials
    • H10N30/093—Forming inorganic materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/80—Constructional details
    • H10N30/85—Piezoelectric or electrostrictive active materials
    • H10N30/853—Ceramic compositions
    • H10N30/8536—Alkaline earth metal based oxides, e.g. barium titanates
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/80—Constructional details
    • H10N30/85—Piezoelectric or electrostrictive active materials
    • H10N30/853—Ceramic compositions
    • H10N30/8542—Alkali metal based oxides, e.g. lithium, sodium or potassium niobates
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/80—Constructional details
    • H10N30/85—Piezoelectric or electrostrictive active materials
    • H10N30/853—Ceramic compositions
    • H10N30/8548—Lead-based oxides
    • 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
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
    • C04B2235/3203—Lithium oxide 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
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • 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
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3229—Cerium oxides 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
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • 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
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, 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
    • C04B2235/3231—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
    • C04B2235/3279—Nickel oxides, nickalates, 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
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates 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
    • C04B2235/3294—Antimony oxides, antimonates, antimonites or oxide forming salts thereof, indium antimonate
    • 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
    • C04B2235/3296—Lead oxides, plumbates or oxide forming salts thereof, e.g. silver plumbate
    • 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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
    • 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
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Landscapes

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

Abstract

本发明公开了一种耐温度冲击的压电陶瓷材料及其制备方法，其组分式为：0.90Pb(Zrm,Tin)O3‑0.05Pb(Zn1/3Nb2/3)O3‑0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.05~0.95；x=1.0~2.0；y=0.5~0.8；耐温度冲击稳定剂为：氧化铈、碳酸锂、氧化钨、三氧化二铝其中的两种或两种以上的混合物。先按化学计量比配料、球磨、压块预烧、二次球磨、成型、排胶烧结、印银、极化、测试。通过该工艺制得的压电陶瓷材料参数为：d33≥500pC/N，ε33 T/ε0≥2700，Kp≥0.70，电容变化率≤±3%。该方法制备的压电陶瓷材料应用于倒车雷达上，有利于倒车雷达灵敏度的提高，同时提高倒车雷达的可靠性和稳定性。

Description

一种耐温度冲击的压电陶瓷材料及其制备方法
技术领域
本发明属于压电陶瓷材料领域，具体涉及一种耐温度冲击的压电陶瓷材料及其制备方法。
背景技术
压电陶瓷是一种能够将机械能和电能互相转换的功能陶瓷材料。长期以来，利用锆钛酸铅二元系(PZT)及三元系压电陶瓷制作压电发声器、超声清洗、超声医疗、声纳系统、汽车倒车传感器、超声换能器和压电致动元件等产品，广泛用于航空、航天、舰船、汽车等领域，对国家整个经济发展有着巨大的影响。随着人民生活水平的提高，人们对汽车的需求量越来越大，汽车传感器也得到巨大的发展，其中倒车雷达作为汽车泊车或者倒车时的安全辅助装置，能够解除驾驶员泊车、倒车和起动车辆时前后左右探视所引起的困扰，提高驾驶安全性等作用，备受人们的青睐，并对倒车雷达的技术要求越来越苛刻。
通常，倒车雷达由超声波传感器（俗称探头）、控制器和显示器（或蜂鸣器）等部分构成。其原理是利用超声波传感器产生的超声波对车后发射， 如在一定范围内碰到物体，就有反射波返回发射源 （超声波传感器的表面）， 主机利用发射波和反射波之间的延时时间和声波速度就能测得距离障碍物的距离，由显示器显示距离并发出其他警示信号，及时示警，从而保证驾驶者的安全。通过原理可以看出，倒车雷达的起着最为重要作用的部件是超声波传感器，超声波传感器的灵敏度、可靠性、探测距离、稳定性等性能则取决于其核心部件压电陶瓷。
当压电陶瓷材料具有高的介电常数、压电常数、耐温度冲击稳定性才能获得高品质的倒车雷达。而现有应用于倒车雷达的压电陶瓷材料介电常数≤2300；压电常数≤450pC/N；温度冲击后电容变化率≤±10%，不利于倒车雷达灵敏度的提高，致使可靠性和稳定性降低。
发明内容
本发明所要解决的就是上述存在的技术问题，提供一种耐温度冲击压电陶瓷材料及其制备方法。
为实现上述目的，本发明技术方案如下：
（1）本发明的组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.05~0.95；x=1.0~2.0；y=0.5~0.8。
（2）本发明的一种耐温度冲击压电陶瓷材料及其制备方法是将Pb3O4、ZrO2、TiO2、ZnO、Nb2O5、Ni2O3、Sb2O3、耐温度冲击稳定剂按0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.05~0.95；x=1.0~2.0；y=0.5~0.8。的化学计量比配料，行星式球磨4h，烘干，过40目筛。
（3）将过筛后的粉料，在20T压机下进行压块，然后在箱式炉中进行合成，合成温度800~900℃，升温速率3.0~3.5℃/min，保温2h随炉冷却。
（4）合成后的坯块机械打碎并进行二次球磨，球磨时间4-8h后烘干过40目筛，随后进行挤模成型，然后放入箱式炉中，在1250~1300℃下烧结，850℃以前升温速率0.8~1.0℃/min，850℃之后升温速率2.5~3.0℃/min，保温2h后随炉冷却。
（5）烧结后瓷片进行印银，印完银后在隧道炉中烧银，烧银温度750~780℃，烧银总时间2h。然后在1.6KV/mm的电压下进行空气极化，极化时间30min，极化温度100℃，极化后静置24h，然后在-55℃~85℃下进行循环温度冲击实验，循环次数20次，循环结束后，在室温（25℃）下静置1h，再测试电容，并计算电容变化率。
上述步骤（2）原料纯度均≥98%；球磨参数为：氧化锆球：原料：去离子水=2.5:1:1.2。
上述步骤（3）压机压力为20MPa，压块尺寸：Φ30*5mm。
上述步骤（4）挤模时添加的PVA为20~25wt%；挤模尺寸：Φ7.2*0.2mm；二次球磨参数为：氧化锆球：原料：去离子水=2.5:1:0.8。
上述步骤（5）提到的电容变化率（△C）计算公式为：
△C=(C温冲后-C25℃)/ C25℃×100%
式中：C温冲后为循环温度冲击后，静置1h，在25℃下测试瓷片的容量；
C25℃为循环温度冲击前25℃下测试瓷片的容量。
本发明相对于现有技术的进步性体现在以下几个方面：采用本发明提供的配方以及制备方法，获得优异的介电以及压电性能:d33≥500pC/N，ε33 T/ε0≥2700，Kp≥0.70，电容变化率≤±3%。本发明采用的工艺简单，成本低，易于批量生产，压电性能好，降低了电容变化率，提高了瓷片的温度冲击稳定性，有利于倒车雷达灵敏度的提高，同时提高了倒车雷达的可靠性和稳定性。
具体实施方式
下面结合实施例对本发明作进一步详细的描述：
实施例1
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.0；x=1.5；y=0.7。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.8wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占28wt%、Li2CO3占57wt%、Al2O3占15wt%。
根据上述配方将Pb3O4、ZrO2、TiO2、ZnO、Nb2O5、Ni2O3、Sb2O3、耐温度冲击稳定剂按化学计量比进行配料，并按氧化锆球：原料：去离子水=2.5:1:1.2加入球磨罐中，然后进行行星式球磨，球磨时间4h；再将球磨好后的物料烘干，然后过40目筛。
过筛后的粉料，在20T压机下进行压块，压机压力为20MPa，压块尺寸：Φ30*5mm，然后在箱式炉中进行合成，合成温度800℃，升温速率3.0℃/min，保温2h随炉冷却。
合成后的坯块机械打碎，按氧化锆球：原料：去离子水=2.5:1:0.8加入球磨罐，再在行星式球磨机中进行二次球磨，球磨时间4h，球磨结束后将物料烘干过40目筛，随后进行挤模成型，挤模时添加的PVA为24wt%；挤模尺寸：Φ7.2*0.2mm；挤模后的瓷片放入箱式炉中，在1250℃下烧结，850℃以前升温速率1.0℃/min，850℃之后升温速率3.0℃/min，保温2h后随炉冷却。
烧结后瓷片进行印银，印完银后在隧道炉中烧银，烧银温度780℃，烧银总时间2h。然后在1.6KV/mm的电压下进行空气极化，极化时间30min，极化温度100℃，极化后静置24h，然后在-55℃~85℃下进行循环温度冲击实验，循环次数20次，循环结束后，在室温（25℃）下静置1h，再测试电容，并计算电容变化率，上述材料的测试结果见表1。
实施例2
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.0；x=1.5；y=0.7。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.8wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占28wt%、Li2CO3占57wt%、WO3占15wt%。
根据上述配方将Pb3O4、ZrO2、TiO2、ZnO、Nb2O5、Ni2O3、Sb2O3、耐温度冲击稳定剂按化学计量比进行配料，并按氧化锆球：原料：去离子水=2.5:1:1.2加入球磨罐中，然后进行行星式球磨，球磨时间4h；再将球磨好后的物料烘干，然后过40目筛。
过筛后的粉料，在20T压机下进行压块，压机压力为20MPa，压块尺寸：Φ30*5mm，然后在箱式炉中进行合成，合成温度850℃，升温速率3.5℃/min，保温2h随炉冷却。
合成后的坯块机械打碎，按氧化锆球：原料：去离子水=2.5:1:0.8加入球磨罐，再在行星式球磨机中进行二次球磨，球磨时间6h，球磨结束后将物料烘干过40目筛，随后进行挤模成型，挤模时添加的PVA为22wt%；挤模尺寸：Φ7.2*0.2mm；挤模后的瓷片放入箱式炉中，在1280℃下烧结，850℃以前升温速率0.8℃/min，850℃之后升温速率2.7℃/min，保温2h后随炉冷却。
烧结后瓷片进行印银，印完银后在隧道炉中烧银，烧银温度760℃，烧银总时间2h。然后在1.6KV/mm的电压下进行空气极化，极化时间30min，极化温度100℃，极化后静置24h，然后在-55℃~85℃下进行循环温度冲击实验，循环次数20次，循环结束后，在室温（25℃）下静置1h，再测试电容，并计算电容变化率，上述材料测试结果见表1。
实施例3
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.0；x=1.5；y=0.7。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.8wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂混合物，其中CeO2占25wt%、Li2CO3占75wt%。
根据上述配方将Pb3O4、ZrO2、TiO2、ZnO、Nb2O5、Ni2O3、Sb2O3、耐温度冲击稳定剂按化学计量比进行配料，并按氧化锆球：原料：去离子水=2.5:1:1.2加入球磨罐中，然后进行行星式球磨，球磨时间4h；再将球磨好后的物料烘干，然后过40目筛。
过筛后的粉料，在20T压机下进行压块，压机压力为20MPa，压块尺寸：Φ30*5mm，然后在箱式炉中进行合成，合成温度900℃，升温速率3.3℃/min，保温2h随炉冷却。
合成后的坯块机械打碎，按氧化锆球：原料：去离子水=2.5:1:0.8加入球磨罐，再在行星式球磨机中进行二次球磨，球磨时间8h，球磨结束后将物料烘干过40目筛，随后进行挤模成型，挤模时添加的PVA为25wt%；挤模尺寸：Φ7.2*0.2mm；挤模后的瓷片放入箱式炉中，在1300℃下烧结，850℃以前升温速率1.0℃/min，850℃之后升温速率2.5℃/min，保温2h后随炉冷却。
烧结后瓷片进行印银，印完银后在隧道炉中烧银，烧银温度780℃，烧银总时间2h。然后在1.6KV/mm的电压下进行空气极化，极化时间30min，极化温度100℃，极化后静置24h，然后在-55℃~85℃下进行循环温度冲击实验，循环次数20次，循环结束后，在室温（25℃）下静置1h，再测试电容，并计算电容变化率，上述材料测试结果见表1。
实施例4
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.0；x=1.0；y=0.5。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为98.5wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占28wt%、Li2CO3占57wt%、Al2O3占15wt%。按照实施例1方法制备压电陶瓷片，测试结果见表1。
实施例5
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.0；x=1.0；y=0.5。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为98.5wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占28wt%、Li2CO3占57wt%、WO3占15wt%。按照实施例2方法制备压电陶瓷片，测试结果见表1。
实施例6
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.0；x=1.0；y=0.5。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为98.5wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占25wt%、Li2CO3占75wt%，按照实施例3方法制备压电陶瓷片，测试结果见表1。
实施例7
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.0；x=2.0；y=0.8。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.2wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占28wt%、Li2CO3占57wt%、Al2O3占15wt%，按照实施例1方法制备压电陶瓷片，测试结果见表1。
实施例8
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.0；x=2.0；y=0.8。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.2wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占28wt%、Li2CO3占57wt%、WO3占15wt%，按照实施例2方法制备压电陶瓷片，测试结果见表1。
实施例9
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.0；x=2.0；y=0.8。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.2wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占25wt%、Li2CO3占75wt%，按照实施例3方法制备压电陶瓷片，测试结果见表1。
实施例10
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.05；x=1.5；y=0.7。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.8wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占28wt%、Li2CO3占57wt%、Al2O3占15wt%，按照实施例1方法制备压电陶瓷片，测试结果见表1。
实施例11
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.05；x=1.5；y=0.7。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.8wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占28wt%、Li2CO3占57wt%、WO3占15wt%，按照实施例2方法制备压电陶瓷片，测试结果见表1。
实施例12
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.05；x=1.5；y=0.7。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.8wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占25wt%、Li2CO3占75wt%，按照实施例3方法制备压电陶瓷片，测试结果见表1。
实施例13
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=0.95；x=1.5；y=0.7。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.8wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占28wt%、Li2CO3占57wt%、Al2O3占15wt%，按照实施例1方法制备压电陶瓷片，测试结果见表1。
实施例14
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=0.95；x=1.5；y=0.7。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.8wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占28wt%、Li2CO3占57wt%、WO3占15wt%，按照实施例2方法制备压电陶瓷片，测试结果见表1。
实施例15
一种耐温度冲击压电陶瓷材料，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=0.95；x=1.5；y=0.7。
所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.8wt%。
所述的耐温度冲击稳定剂为氧化铈、碳酸锂以及三氧化二铝混合物，其中CeO2占25wt%、Li2CO3占75wt%，按照实施例3方法制备压电陶瓷片，测试结果见表1。
对比组1其组分式为：0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/ 3Nb2/3)O3+xwt%Sb2O3，相比于实施例，组分式相同，不同之处是未加入耐温度冲击稳定剂。其中m/n=0.95，x=1.5。所述组分铌锌-铌镍-铌锑-锆钛酸铅五元系所占比例为98.5wt%，按照实施例1方法制备压电陶瓷片，测试结果见表1。
对比组2其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3，相比于实施例，组分式相同，不同之处是未加入耐温度冲击稳定剂。其中m/n=1.0，x=1.5。所述组分铌锌-铌镍-铌锑-锆钛酸铅五元系所占比例为98.5wt%，按照实施例1方法制备压电陶瓷片，测试结果见表1。
对比组3其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3，相比于实施例，组分式相同，不同之处是未加入耐温度冲击稳定剂。其中m/n=1.05，x=1.5。所述组分铌锌-铌镍-铌锑-锆钛酸铅五元系所占比例为98.5wt%，按照实施例1方法制备压电陶瓷片，测试结果见表1。
表1 本发明的陶瓷材料性能指标对比表
综上，本发明实施例提供的耐温度冲击压电陶瓷材料及其制备方法中，通过配方的改进，制得的压电陶瓷的d33≥500pC/N，ε33 T/ε0≥2700，Kp≥0.70，电容变化率≤±3%。本发明采用的工艺简单，成本低，易于批量生产，压电性能好，降低了电容变化率，提高了瓷片的温度冲击稳定性，有利于倒车雷达灵敏度的提高，同时提高了倒车雷达的可靠性和稳定性。
以上所述的实施例是本发明一部分实施例，而不是全部的实施例。本发明的实施例的详细描述并非旨在限制要求保护的本发明范围，而是仅仅表示本发明的选定实施例。基于本发明中的实施例，本领域技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明的保护范围之内。

Claims (10)

1.一种耐温度冲击的压电陶瓷材料，其特征在于，其组分式为：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.05~0.95；x=1.0~2.0；y=0.5~0.8；所述组分铌锌-铌镍-锆钛酸铅四元系所占比例为97.2~98.5wt%。
2.根据权利要求1所述一种耐温度冲击的压电陶瓷材料，其特征在于，所述的m/n为1.0。
3.根据权利要求1所述一种耐温度冲击的压电陶瓷材料，其特征在于：所述的x为1.5。
4.根据权利要求1所述一种耐温度冲击的压电陶瓷材料，其特征在于：所述的y为0.7。
5.根据权利要求1所述一种耐温度冲击的压电陶瓷材料，其特征在于：所述的耐温度冲击稳定剂为：氧化铈、碳酸锂、氧化钨、三氧化二铝其中的两种或两种以上的混合物，其中CeO2占25~30wt%、Li2CO3占50~75wt%、WO3占0~10wt%、Al2O3占0~10wt%。
6.根据权利要求1-5任意一项所述的所述耐温度冲击的压电陶瓷材料的制备方法，其特征在于：具体制备步骤为：
（1）在温度为25℃，相对空气湿度≥60%下将Pb3O4、ZrO2、TiO2、ZnO、Nb2O5、Ni2O3、Sb2O3、耐温度冲击稳定剂按组分式：
0.90Pb(Zrm,Tin)O3-0.05Pb(Zn1/3Nb2/3)O3-0.05Pb(Ni1/3Nb2/3)O3+xwt%Sb2O3+ywt%耐温度冲击稳定剂，其中m/n=1.05~0.95；x=1.0~2.0；y=0.5~0.8
的化学计量比配料，行星式球磨4h，烘干，过40目筛；
（2）将过筛后的粉料，在20T压机下进行压块，然后在箱式炉中进行合成，合成温度800~900℃，按照梯度进行升温，升温速率为：3.0~3.5℃/min，保温2h后随炉冷却；
（3）将步骤（2）中合成后的坯块机械打碎并进行二次球磨，球磨时间4~8h后烘干过40目筛，随后进行挤模成型，然后放入箱式炉中，在1250~1300℃下烧结，850℃以前升温速率0.8~1.0℃/min，850℃之后升温速率2.5~3.0℃/min，保温2h后随炉冷却；
（4）烧结后瓷片进行印银，印完银后在隧道炉中烧银，烧银温度750~780℃，烧银总时间2h；然后在1.6KV/mm的电压下进行空气极化，极化时间30min，极化温度100℃，极化后静置24h，然后在-55℃~85℃下进行循环温度冲击实验，循环次数20次，循环结束后，在室温（25℃）下静置1h，再测试电容，并计算电容变化率。
7.根据权利要求6所述的耐温度冲击的压电陶瓷材料的制备方法，其特征在于，步骤（1）原料纯度均≥98%；球磨参数为：氧化锆球：原料：去离子水=2.5:1:1.2。
8.根据权利要求6所述的耐温度冲击的压电陶瓷材料的制备方法，其特征在于，步骤（2）中压机压力为20MPa，压块尺寸：Φ30*5mm。
9. 根据权利要求6所述的耐温度冲击的压电陶瓷材料的制备方法，其特征在于，步骤（3）挤模时添加的PVA为20~25wt%；挤模尺寸：Φ7.2*0.2mm；二次球磨参数为：氧化锆球：原料：去离子水=2.5:1:0.8。
10. 根据权利要求6所述的耐温度冲击的压电陶瓷材料的制备方法，其特征在于，步骤（4）提到的电容变化率（△C）计算公式为：△C=(C温冲后-C25℃)/ C25℃×100%
其中公式中：C温冲后为循环温度冲击后，静置1h，在25℃下测试瓷片的容量；
C25℃为循环温度冲击前25℃下测试瓷片的容量。
CN201811539037.6A 2018-12-17 2018-12-17 一种耐温度冲击的压电陶瓷材料及其制备方法 Active CN109503158B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811539037.6A CN109503158B (zh) 2018-12-17 2018-12-17 一种耐温度冲击的压电陶瓷材料及其制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811539037.6A CN109503158B (zh) 2018-12-17 2018-12-17 一种耐温度冲击的压电陶瓷材料及其制备方法

Publications (2)

Publication Number Publication Date
CN109503158A true CN109503158A (zh) 2019-03-22
CN109503158B CN109503158B (zh) 2022-02-15

Family

ID=65753500

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811539037.6A Active CN109503158B (zh) 2018-12-17 2018-12-17 一种耐温度冲击的压电陶瓷材料及其制备方法

Country Status (1)

Country Link
CN (1) CN109503158B (zh)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113125869A (zh) * 2021-03-11 2021-07-16 温州大学 一种监测压电陶瓷的发电性能的模型箱
CN116444268A (zh) * 2022-01-07 2023-07-18 中国科学院上海硅酸盐研究所 高温极化获得的高压电性能铌锑-锆钛酸铅压电陶瓷

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060060900A1 (en) * 2004-09-20 2006-03-23 Xubai Zhang Tunable low loss material composition and methods of manufacture and use therefore
CN101098836A (zh) * 2005-01-14 2008-01-02 株式会社村田制作所 压电陶瓷组合物和压电驱动器
JP2012009800A (ja) * 2010-05-24 2012-01-12 Mitsubishi Materials Corp 強誘電体薄膜及び該強誘電体薄膜を用いた薄膜キャパシタ
CN103467089A (zh) * 2013-09-09 2013-12-25 天津大学 一种铌锌铌镍锆钛酸铅压电陶瓷
CN103724013A (zh) * 2013-12-26 2014-04-16 重庆胜普昂凯科技有限公司 一种a位复合取代高压电常数的压电陶瓷材料及制备方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060060900A1 (en) * 2004-09-20 2006-03-23 Xubai Zhang Tunable low loss material composition and methods of manufacture and use therefore
CN101098836A (zh) * 2005-01-14 2008-01-02 株式会社村田制作所 压电陶瓷组合物和压电驱动器
JP2012009800A (ja) * 2010-05-24 2012-01-12 Mitsubishi Materials Corp 強誘電体薄膜及び該強誘電体薄膜を用いた薄膜キャパシタ
CN103467089A (zh) * 2013-09-09 2013-12-25 天津大学 一种铌锌铌镍锆钛酸铅压电陶瓷
CN103724013A (zh) * 2013-12-26 2014-04-16 重庆胜普昂凯科技有限公司 一种a位复合取代高压电常数的压电陶瓷材料及制备方法

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
BALGOVIND TIWARI ET AL.: "Study of Impedance Parameters", 《IEEE TRANSACTIONS ON DIELECTRICS AND ELECTRICAL INSULATION》 *
上海科技大学新型无机材料教研组: "《电子陶瓷工艺基础》", 31 May 1977, 上海人民出版社 *
任桂先: "《引爆压电陶瓷原件制造》", 31 March 1985, 国防工业出版社 *
山东大学压电铁电物理教研室: "《压电陶瓷及其应用》", 30 November 1974, 山东人民出版社 *
文理等: "倒车雷达用锆钛酸铅压电陶瓷材料的研究", 《广州化工》 *
贾伯年，俞朴: "《传感器技术》", 28 February 1992, 东南大学出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113125869A (zh) * 2021-03-11 2021-07-16 温州大学 一种监测压电陶瓷的发电性能的模型箱
CN116444268A (zh) * 2022-01-07 2023-07-18 中国科学院上海硅酸盐研究所 高温极化获得的高压电性能铌锑-锆钛酸铅压电陶瓷

Also Published As

Publication number Publication date
CN109503158B (zh) 2022-02-15

Similar Documents

Publication Publication Date Title
CN104987072B (zh) 高电学性能的铌铟酸铅‑铌镁酸铅‑钛酸铅弛豫铁电织构陶瓷及其制备方法和应用
CN103803974B (zh) 一种注塑成型氧化锆及其制备方法
CN109503158A (zh) 一种耐温度冲击的压电陶瓷材料及其制备方法
CN107459346A (zh) 高电学性能的无铅压电钛酸钡基织构陶瓷及其制备方法和应用
CN109180181B (zh) 一种无铅弛豫反铁电陶瓷储能材料及其制备方法
CN103964846B (zh) 压电双晶片用压电陶瓷材料及其制备方法
CN101139202A (zh) 压电/电致伸缩体、其制造方法及压电/电致伸缩元件
CN109534810A (zh) 钛酸铋钠基无铅驱动器陶瓷及其制备方法和应用
CN104291817A (zh) 高居里温度的pzt压电陶瓷材料及其制备方法
CN109400152A (zh) 一种耐电压压电陶瓷材料及其制备方法
CN103641476A (zh) 陶瓷材料、烧结体及制备方法、压电陶瓷器件、压电双晶片及改善其温度稳定性的胶合方法
CN110845230A (zh) 一种三元系铌钪酸铅-铌镁酸铅-钛酸铅陶瓷及其制备方法
CN103360068A (zh) 锰锑掺杂的锆钛酸铅压电陶瓷
CN101786880B (zh) 一种铌酸钾钠-铌酸钾锂压电陶瓷及其制备方法
CN101302105A (zh) 驱动器用含铌锑酸铅的五元系压电陶瓷材料及制备方法
CN101475373B (zh) 高压电应变常数d31、低压电电压常数g31压电陶瓷材料及其制备方法
CN108752010B (zh) 一种压电陶瓷及其制备方法及3d打印压电陶瓷装置
CN101941840B (zh) 制备铌镍-锆钛酸铅压电陶瓷的b位氧化物前驱体方法
CN102249671B (zh) 添加钴和铝的钛酸钡基无铅压电陶瓷材料及其制备方法
CN107162593A (zh) 一种铌酸钾钠无铅压电陶瓷的制备方法
CN102718482B (zh) 压电陶瓷材料及其制备方法、压电发电振子
CN114988872B (zh) 一种锆酸钙粉体在铌酸钾钠基压电陶瓷的应用
CN105294102B (zh) 一种纳米反应器引入纳米烧结助剂常压低温烧结制备铌酸钾钠基无铅压电陶瓷的方法
CN103319175A (zh) 一种压电陶瓷材料及其制备方法和用途
CN103011774A (zh) 高灵敏度压电陶瓷材料及制备方法与应用

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