CN114368968A - 一种铌酸钾钠基无铅压电陶瓷及其制备方法 - Google Patents
一种铌酸钾钠基无铅压电陶瓷及其制备方法 Download PDFInfo
- Publication number
- CN114368968A CN114368968A CN202111582108.2A CN202111582108A CN114368968A CN 114368968 A CN114368968 A CN 114368968A CN 202111582108 A CN202111582108 A CN 202111582108A CN 114368968 A CN114368968 A CN 114368968A
- Authority
- CN
- China
- Prior art keywords
- sodium niobate
- potassium
- ceramic
- piezoelectric ceramic
- ball milling
- 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.)
- Pending
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 76
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 25
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 13
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 13
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 13
- 239000011734 sodium Substances 0.000 claims abstract description 13
- 229910002976 CaZrO3 Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 24
- 238000009694 cold isostatic pressing Methods 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- 230000005684 electric field Effects 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229920002545 silicone oil Polymers 0.000 claims description 7
- 235000010216 calcium carbonate Nutrition 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 230000010287 polarization Effects 0.000 claims description 6
- 239000012043 crude product Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- -1 oxide Chemical compound 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 10
- 238000001035 drying Methods 0.000 description 10
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 10
- 229910052808 lithium carbonate Inorganic materials 0.000 description 5
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 description 5
- 235000015320 potassium carbonate Nutrition 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 description 5
- 235000017550 sodium carbonate Nutrition 0.000 description 5
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910012519 LiSbO3 Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
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
- C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
-
- 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
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
-
- 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
- C04B2235/3248—Zirconates or hafnates, e.g. zircon
-
- 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
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
- C04B2235/3267—MnO2
-
- 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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/442—Carbonates
-
- 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
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)
- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明公开了一种铌酸钾钠基无铅压电陶瓷及其制备方法,铌酸钾钠基无铅压电陶瓷的通式为(1‑x)(Na,K,Li)(Nb,Ta)O3‑xCaZrO3‑yMnO2,0≤x≤0.1,0≤y≤0.04,其中x为CaZrO3的占原料总量的原子百分比,y为MnO2占原料总量的质量百分比,所述铌酸钾钠基无铅压电陶瓷具有280‑360pC/N的压电常数d33,所述铌酸钾钠基无铅压电陶瓷的反向压电常数d33*在室温至150℃的温度范围内的波动不超过10%。本发明通过本方法,可以有效制备得到具有优异压电性能与温度稳定性的铌酸钾钠基无铅压电陶瓷,且其压电常数d33达280‑360pC/N,其压电性能的温度稳定性非常优异,在室温至150℃的温度范围内保持在±10%的波动范围之内。
Description
技术领域
本发明涉及功能陶瓷材料技术领域,具体为一种铌酸钾钠基无铅压电陶瓷及其制备方法。
背景技术
压电材料由于具有正、逆压电效应而可实现机械能与电能的相互转换,因此作为一种重要的功能材料被广泛应用于驱动器、传感器等高新技术领域,目前,锆钛酸铅基压电陶瓷因其性能的优越性而成为应用最广泛的压电材料,但是该体系材料中含有大量有毒的铅,在生产、使用及废弃处理过程中均会给人类健康和生态环境带来严重的危害,因此,研发性能优异的无铅压电陶瓷材料成为一项紧迫且具有重大实用意义的课题。
2004年,日本的Saito等人在Nature杂志上报道了利用织构方法制备的经掺杂改性的铌酸钾钠基压电陶瓷,其压电系数d33达416pC/N,可以与含铅压电陶瓷相媲美,该里程碑式的重大突破掀起了研究铌酸钾钠基无铅压电陶瓷的热潮,并使得铌酸钾钠基无铅压电陶瓷被认为是最具潜力替代含铅压电陶瓷的体系之一,目前,大部分关于铌酸钾钠基无铅压电陶瓷的研究仍专注于通过掺杂改性在室温附近形成多晶型相变区以提高其压电性能,但是,由于多晶型相变区的存在,使得铌酸钾钠基无铅压电陶瓷压电性能的温度稳定性很差,例如,对LiSbO3掺杂的铌酸钾钠无铅压电陶瓷,其反向压电系数d33* 在室温下为355pm/V,而当温度升高至50℃时急剧下降至250pm/V,降幅达 30%,压电性能对温度如此强烈的敏感性使铌酸钾钠基无铅压电陶瓷难以实现实用化。
发明内容
本发明的目的在于提供一种铌酸钾钠基无铅压电陶瓷及其制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:一种铌酸钾钠基无铅压电陶瓷,铌酸钾钠基无铅压电陶瓷的通式为(1-x)(Na,K,Li)(Nb,Ta) O3-xCaZrO3-yMnO2,0≤x≤0.1,0≤y≤0.04,其中x为CaZrO3的占原料总量的原子百分比,y为MnO2占原料总量的质量百分比。
优选的,所述铌酸钾钠基无铅压电陶瓷具有280-360pC/N的压电常数d33。
优选的,所述铌酸钾钠基无铅压电陶瓷的反向压电常数d33*在室温至 150℃的温度范围内的波动不超过10%。
一种铌酸钾钠基无铅压电陶瓷的制备方法,其制备方法包括以下步骤:
A、将预定比例的原料混合并进行球磨,得到混合粉料,其中,原料包括碳酸盐、氧化物、CaCO3、ZrO2以及MnO2;
B、将混合粉料进行预烧结,得到经过预烧结的粉料;
C、将经过预烧结的粉料进行二次球磨,得到经过二次球磨的粉料;
D、将经过二次球磨的粉料进行冷压成型和冷等静压处理,得到陶瓷粗坯;
E、将陶瓷粗坯进行烧结,得到陶瓷粗品;
F、将陶瓷粗品进行极化处理,得到铌酸钾钠基无铅压电陶瓷。
优选的,所述预球磨和二次球磨是分别独立地在球磨罐中采用无水乙醇作为介质进行球磨12-24h而进行的,以得到成分均匀且细化的粉体,由此可以进一步提高铌酸钾钠基无铅压电陶瓷的综合性能。
优选的,所述预烧结是在空气中,750-850℃的温度下进行的,由此可以使得碳化物和氧化物中的碳元素和部分氧元素烧蚀掉,以便制备得到具有优异压电性能与温度稳定性的铌酸钾钠基无铅压电陶瓷。
优选的,所述冷压成型是在30-50MPa的压力下进行的,且冷等静压是在 200-300MPa的压力下进行的,由此可以进一步提高铌酸钾钠基无铅压电陶瓷的温度稳定性。
优选的,所述烧结是在空气中,1080-1160℃的温度下进行的,由此可以进一步提高铌酸钾钠基无铅压电陶瓷的温度稳定性。
优选的,所述极化处理包括:将陶瓷粗品置于在120℃的硅油中,并以 3-4kV/mm的直流电场强度进行极化处理30min,由此可以赋予压电陶瓷以宏观压电性能。
与现有技术相比,本发明的有益效果如下:
本发明通过本方法,可以有效制备得到具有优异压电性能与温度稳定性的铌酸钾钠基无铅压电陶瓷,且其压电常数d33达280-360pC/N,其压电性能的温度稳定性非常优异,在室温至150℃的温度范围内保持在±10%的波动范围之内。
附图说明
图1为压电陶瓷不同电场下单向应变值随温度的变化关系图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种铌酸钾钠基无铅压电陶瓷,铌酸钾钠基无铅压电陶瓷的通式为(1-x) (Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,0≤x≤0.1,0≤y≤0.04,其中x为CaZrO3 的占原料总量的原子百分比,y为MnO2占原料总量的质量百分比。
一种铌酸钾钠基无铅压电陶瓷的制备方法,其制备方法包括以下步骤:
A、按照(1-x)(Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,其中x=0,y=0.02,将分析纯的Li2CO3,Na2CO3,K2CO3,Nb2O5,Ta2O5,MnO2粉体按化学计量比配料;
B、配好的原料加入到以无水乙醇为介质的球磨罐中,球磨12-24h,烘干后得到混合粉料;
C、将混合粉料在空气中850℃预烧4h;
D、将预烧后的粉再次球磨12-24h并烘干;
E、将二次球磨过的预烧合成粉在50MPa下冷压成型为直径10mm、厚度 1.5mm的圆片,然后在200MPa下冷等静压;
F、将冷等静压后的圆片在空气中1110℃-1150℃烧结2h;
G、将烧结后的陶瓷片上银电极,在120℃硅油中,电场强度为3kV/mm的直流电场下极化30min。
制备的铌酸钾钠基无铅压电陶瓷的性能参数见表1,其压电性能的温度稳定性见图1。
实施例2
一种铌酸钾钠基无铅压电陶瓷,铌酸钾钠基无铅压电陶瓷的通式为(1-x) (Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,0≤x≤0.1,0≤y≤0.04,其中x为CaZrO3 的占原料总量的原子百分比,y为MnO2占原料总量的质量百分比。
一种铌酸钾钠基无铅压电陶瓷的制备方法,其制备方法包括以下步骤:
A、按照(1-x)(Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,其中x=0.03, y=0.01,将分析纯的Li2CO3,Na2CO3,K2CO3,Nb2O5,Ta2O5,CaCO3,ZrO2, MnO2粉体按化学计量比配料;
B、配好的原料加入到以无水乙醇为介质的球磨罐中,球磨12-24h,烘干后得到混合粉料;
C、将混合粉料在空气中850℃预烧4h;
D、将预烧后的粉再次球磨12-24h并烘干;
E、将二次球磨过的预烧合成粉在50MPa下冷压成型为直径10mm、厚度 1.5mm的圆片,然后在200MPa下冷等静压;
F、将冷等静压后的圆片在空气中1100℃-1140℃烧结2h;
G、将烧结后的陶瓷片上银电极,在120℃硅油中,电场强度为3kV/mm的直流电场下极化30min。
制备的铌酸钾钠基无铅压电陶瓷的性能参数见表1。
实施例3
一种铌酸钾钠基无铅压电陶瓷,铌酸钾钠基无铅压电陶瓷的通式为(1-x) (Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,0≤x≤0.1,0≤y≤0.04,其中x为CaZrO3 的占原料总量的原子百分比,y为MnO2占原料总量的质量百分比。
一种铌酸钾钠基无铅压电陶瓷的制备方法,其制备方法包括以下步骤:
A、按照(1-x)(Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,其中x=0.05, y=0.02,将分析纯的Li2CO3,Na2CO3,K2CO3,Nb2O5,Ta2O5,CaCO3,ZrO2, MnO2粉体按化学计量比配料;
B、配好的原料加入到以无水乙醇为介质的球磨罐中,球磨12-24h,烘干后得到混合粉料;
C、将混合粉料在空气中900℃预烧4h;
D、将预烧后的粉再次球磨12-24h并烘干;
E、将二次球磨过的预烧合成粉在50MPa下冷压成型为直径10mm、厚度 1.5mm的圆片,然后在200MPa下冷等静压;
F、将冷等静压后的圆片在空气中1080℃-1130℃烧结2h;
G、将烧结后的陶瓷片上银电极,在120℃硅油中,电场强度为4kV/mm的直流电场下计划30min。
极化后的铌酸钾钠基无铅压电陶瓷的压电系数d33高达345pC/N,机电耦合因数kP可达0.47。最重要的是该体系的无铅压电陶瓷具有很优异的温度稳定性,在室温至150℃的温度范围内,其压电性能波动范围在±10%之内。
实施例4
一种铌酸钾钠基无铅压电陶瓷,铌酸钾钠基无铅压电陶瓷的通式为(1-x) (Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,0≤x≤0.1,0≤y≤0.04,其中x为CaZrO3 的占原料总量的原子百分比,y为MnO2占原料总量的质量百分比。
一种铌酸钾钠基无铅压电陶瓷的制备方法,其制备方法包括以下步骤:
A、按照(1-x)(Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,其中x=0.08, y=0.01,将分析纯的Li2CO3,Na2CO3,K2CO3,Nb2O5,Ta2O5,CaCO3,ZrO2, MnO2粉体按化学计量比配料;
B、配好的原料加入到以无水乙醇为介质的球磨罐中,球磨12-24h,烘干后得到混合粉料;
C、将混合粉料在空气中950℃预烧4h;
D、将预烧后的粉再次球磨12-24h并烘干;
E、将二次球磨过的预烧合成粉在50MPa下冷压成型为直径10mm、厚度 1.5mm的圆片,然后在200MPa下冷等静压;
F、将冷等静压后的圆片在空气中1080℃-1120℃烧结2h;
G、将烧结后的陶瓷片上银电极,在120℃硅油中,电场强度为3.5kV/mm 的直流电场下极化30min。
制备的铌酸钾钠基无铅压电陶瓷的性能参数见表1。
实施例5
一种铌酸钾钠基无铅压电陶瓷,铌酸钾钠基无铅压电陶瓷的通式为(1-x) (Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,0≤x≤0.1,0≤y≤0.04,其中x为CaZrO3 的占原料总量的原子百分比,y为MnO2占原料总量的质量百分比。
一种铌酸钾钠基无铅压电陶瓷的制备方法,其制备方法包括以下步骤:
A、按照(1-x)(Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,其中x=0.05, y=0.04,将分析纯的Li2CO3,Na2CO3,K2CO3,Nb2O5,Ta2O5,CaCO3,ZrO2, MnO2粉体按化学计量比配料;
B、配好的原料加入到以无水乙醇为介质的球磨罐中,球磨12-24h,烘干后得到混合粉料;
C、将混合粉料在空气中900℃预烧4h;
D、将预烧后的粉再次球磨12-24h并烘干;
E、将二次球磨过的预烧合成粉在50MPa下冷压成型为直径10mm、厚度 1.5mm的圆片,然后在200MPa下冷等静压;
F、将冷等静压后的圆片在空气中1060℃-1080℃烧结2h;
G、将烧结后的陶瓷片上银电极,在120℃硅油中,电场强度为4kV/mm的直流电场下极化30min。
制备的铌酸钾钠基无铅压电陶瓷的性能参数见表1。
表1
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (9)
1.一种铌酸钾钠基无铅压电陶瓷,其特征在于:铌酸钾钠基无铅压电陶瓷的通式为(1-x)(Na,K,Li)(Nb,Ta)O3-xCaZrO3-yMnO2,0≤x≤0.1,0≤y≤0.04,其中x为CaZrO3的占原料总量的原子百分比,y为MnO2占原料总量的质量百分比。
2.根据权利要求1所述的一种铌酸钾钠基无铅压电陶瓷,其特征在于:所述铌酸钾钠基无铅压电陶瓷具有280-360pC/N的压电常数d33。
3.根据权利要求1所述的一种铌酸钾钠基无铅压电陶瓷,其特征在于:所述铌酸钾钠基无铅压电陶瓷的反向压电常数d33*在室温至150℃的温度范围内的波动不超过10%。
4.一种铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于:其制备方法包括以下步骤:
A、将预定比例的原料混合并进行球磨,得到混合粉料,其中,原料包括碳酸盐、氧化物、CaCO3、ZrO2以及MnO2;
B、将混合粉料进行预烧结,得到经过预烧结的粉料;
C、将经过预烧结的粉料进行二次球磨,得到经过二次球磨的粉料;
D、将经过二次球磨的粉料进行冷压成型和冷等静压处理,得到陶瓷粗坯;
E、将陶瓷粗坯进行烧结,得到陶瓷粗品;
F、将陶瓷粗品进行极化处理,得到铌酸钾钠基无铅压电陶瓷。
5.根据权利要求4所述的一种铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于:所述预球磨和二次球磨是分别独立地在球磨罐中采用无水乙醇作为介质进行球磨12-24h而进行的。
6.根据权利要求4所述的一种铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于:所述预烧结是在空气中,750-850℃的温度下进行的。
7.根据权利要求4所述的一种铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于:所述冷压成型是在30-50MPa的压力下进行的,且冷等静压是在200-300MPa的压力下进行的。
8.根据权利要求4所述的一种铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于:所述烧结是在空气中,1080-1160℃的温度下进行的。
9.根据权利要求4所述的一种铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于:所述极化处理包括:将陶瓷粗品置于在120℃的硅油中,并以3-4kV/mm的直流电场强度进行极化处理30min。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111582108.2A CN114368968A (zh) | 2021-12-22 | 2021-12-22 | 一种铌酸钾钠基无铅压电陶瓷及其制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111582108.2A CN114368968A (zh) | 2021-12-22 | 2021-12-22 | 一种铌酸钾钠基无铅压电陶瓷及其制备方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN114368968A true CN114368968A (zh) | 2022-04-19 |
Family
ID=81140850
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202111582108.2A Pending CN114368968A (zh) | 2021-12-22 | 2021-12-22 | 一种铌酸钾钠基无铅压电陶瓷及其制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114368968A (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114988871A (zh) * | 2022-05-16 | 2022-09-02 | 清华大学 | 一种铌酸钾钠基无铅压电陶瓷及其制备方法和应用 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103274689A (zh) * | 2013-06-14 | 2013-09-04 | 清华大学 | 铌酸钾钠基无铅压电陶瓷及其制备方法 |
US20170141292A1 (en) * | 2014-04-11 | 2017-05-18 | Ngk Spark Plug Co., Ltd. | Lead-free piezoelectric ceramic composition, piezoelectric element using the same, and method of manufacturing lead-free piezoelectric ceramic composition |
-
2021
- 2021-12-22 CN CN202111582108.2A patent/CN114368968A/zh active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103274689A (zh) * | 2013-06-14 | 2013-09-04 | 清华大学 | 铌酸钾钠基无铅压电陶瓷及其制备方法 |
US20170141292A1 (en) * | 2014-04-11 | 2017-05-18 | Ngk Spark Plug Co., Ltd. | Lead-free piezoelectric ceramic composition, piezoelectric element using the same, and method of manufacturing lead-free piezoelectric ceramic composition |
Non-Patent Citations (2)
Title |
---|
MIN ZHANG等: "Temperature dependent phase structure and enhanced electrical properties of CaZrO3-modified (K,Na,Li) (Nb,Ta)O3 lead-free piezoelectric ceramics", 《CERAMICS INTERNATIONAL》 * |
RONGXIA HUANG等: "The enhanced piezoelectric property of (Li,K,Na)(Nb,Ta)O3 lead-free ceramics induced by rare earth oxide doping", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114988871A (zh) * | 2022-05-16 | 2022-09-02 | 清华大学 | 一种铌酸钾钠基无铅压电陶瓷及其制备方法和应用 |
CN114988871B (zh) * | 2022-05-16 | 2023-07-14 | 清华大学 | 温度稳定型铌酸钾钠基无铅压电陶瓷及其制备方法和应用 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110272270B (zh) | 一种具有低介电损耗及高温稳定性的铁酸铋-钛酸钡基高温无铅压电陶瓷及其制备方法 | |
CN107698252B (zh) | 一种陶瓷材料作为高温稳定压电能量收集材料的应用及制备方法 | |
CN105272244A (zh) | 一种铌酸钾钠基无铅压电陶瓷及其制备方法 | |
CN103274689A (zh) | 铌酸钾钠基无铅压电陶瓷及其制备方法 | |
CN110981468B (zh) | 一种钛酸铋钠基压电陶瓷的制备方法 | |
CN109796205B (zh) | 一种铋层状结构钛钽酸铋高温压电陶瓷材料及其制备方法 | |
CN107098699A (zh) | 宽烧结温区及宽组分调节的无铅压电织构陶瓷及制备方法 | |
Qaiser et al. | High‐temperature multilayer actuators based on CuO added BiScO3–PbTiO3 piezoceramics and Ag electrodes | |
CN108623303A (zh) | 一种抗还原铌酸钾钠基无铅压电陶瓷及其制备方法 | |
CN101429027A (zh) | 一种铌酸钾钠基无铅压电陶瓷及其低温烧结制备方法 | |
CN114368968A (zh) | 一种铌酸钾钠基无铅压电陶瓷及其制备方法 | |
CN114409400A (zh) | 一种铌酸钾钠基无铅压电陶瓷及其制备方法 | |
CN107903055B (zh) | 一种梯度掺杂钛酸铋钠基多层无铅压电陶瓷 | |
CN111925208A (zh) | 一种铌酸锂钠基无铅压电陶瓷及其制备方法 | |
CN113582692A (zh) | 低温烧结的铌酸钾钠基无铅压电陶瓷材料及其制备方法 | |
CN113582689B (zh) | 一种用于叠层致动器低温共烧压电陶瓷材料及其制备方法 | |
CN113511893B (zh) | 一种bnt基三层结构的高储能密度陶瓷及其制备方法 | |
CN114276138A (zh) | 铌酸钾钠基无铅压电陶瓷及其制备方法 | |
CN112159227B (zh) | 一种铌酸钾钠基无铅压电陶瓷及其制作工艺 | |
CN111517788A (zh) | 一种具有高剩余极化强度的铌酸钾钠陶瓷材料的制备方法 | |
CN107021754B (zh) | 分散剂改性弛豫型铌镍锆钛酸铅压电陶瓷及其制备方法 | |
CN105060882A (zh) | 一种压电陶瓷材料及其制备方法 | |
CN105218092B (zh) | 一种同时具备大位移及低滞后的锆钛酸铅基压电陶瓷材料及其制备方法 | |
CN115385675A (zh) | 一种高居里温度兼具储能特性的铁酸铋基无铅铁电陶瓷材料及其制备方法 | |
CN104944944B (zh) | Re2x/3(Ba0.06Bi0.47Na0.47)1‑xMeyTi1‑yO3无铅反铁电高储能密度陶瓷及其制备方法 |
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 | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220419 |