CN106521627A - 一种铌酸钾钠基压电单晶及其制备方法 - Google Patents
一种铌酸钾钠基压电单晶及其制备方法 Download PDFInfo
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- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000013078 crystal Substances 0.000 title abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 6
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011734 sodium Substances 0.000 claims description 22
- 238000005245 sintering Methods 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 206010013786 Dry skin Diseases 0.000 claims description 3
- 229920001903 high density polyethylene Polymers 0.000 claims description 3
- 239000004700 high-density polyethylene Substances 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract description 2
- 235000010216 calcium carbonate Nutrition 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 19
- 238000005516 engineering process Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 229910002976 CaZrO3 Inorganic materials 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910003781 PbTiO3 Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling 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
- 238000002109 crystal growth method Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/30—Niobates; Vanadates; Tantalates
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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Abstract
本发明提供一种铌酸钾钠基压电单晶,以CaCO3、ZrO2、Li2CO3和Bi2O3作为掺杂原料,以K0.5Na0.5NbO3为主体材料组成,化学式为:xCaZrO3‑(1–x)(99.6K0.5Na0.5NbO3‑0.4LiBiO3),式中x表示体系中摩尔含量,其中0﹤x≤0.005。其制备方法包括:(1)所用原料均置于烘箱中烘干;(2)按化学式称量原料,球磨;(3)将产物烘干,预烧;(4)再以无水乙醇为介质球磨后烘干;(5)将烘干的粉料过筛后,压制成圆坯;(6)将压制好的圆坯烧结获得单晶。本发明的优点是显著地提高了铌酸钾钠基单晶的压电性能,其压电常数d 33最高达到488 pC/N。
Description
技术领域
本发明涉及无铅压电材料,具体是一种铌酸钾钠基压电单晶及其制备方法。
背景技术
以由铁电体与反铁电体组成的PbZrO3-PbTiO3(PZT)固溶体系为代表的铅基压电陶瓷广泛应用在换能器、驱动器和谐振器等领域。由于在PZT系陶瓷中有毒的氧化铅含量超过原料总质量的60%以上,给人类生存环境带来了严重危害,压电陶瓷的无铅化是人类发展的迫切希望。与当前研究的其它体系无铅压电陶瓷相比,铌酸钾钠(K0.5Na0.5NbO3,KNN)系压电陶瓷因具有介电常数小、压电性能高、频率常数大、密度小、居里温度高及组成元素对人体友好等特点,被认为是很有前途替代PZT的无铅压电材料之一。
一般,按陶瓷的结晶形态,陶瓷可分为多晶与单晶两大类。单晶陶瓷因为不受晶粒大小、晶粒取向、晶界与气孔率等的影响,从而比多晶陶瓷拥有更加优异的性能,如具有更加优异的介电、压电与光学性能等。对PZT系陶瓷来说,单晶的压电常数比多晶要高出一个数量级,S.E. Park等人于1996年研究的PZN-PT单晶在非极轴方向<001>上d 33达到2500pC/N,机电耦合系数k33大于90%(参考文献:Park S E, Shrout T R. Ultrahigh strain andpiezoelectric behavior in relaxor based ferroelectric single crystals. J ApplPhys, 1997, 82(4):1804-1811.)。但就当前的技术来讲,如顶部籽晶溶体生长(TSSG)法等,在制备高质量、大尺寸的单晶压电陶瓷方面仍存在晶体生长速度缓慢、晶体成分分布不均匀、晶体结构缺陷控制困难导致材料性能波动以及制备成本过高等一系列问题。
K0.5Na0.5NbO3基陶瓷的压电性能不仅与掺杂成分有关,还与结晶取向密切相关,特别是单晶体。通常,单晶的铁电、压电、介电等性能远远优于同类的陶瓷材料,因此K0.5Na0.5NbO3基无铅压电单晶也有望获得更好的性能。由于Na2O和K2O在约900℃时便开始挥发,而传统的单晶制备方法需要长时间在高温环境下生长,具有晶体生长速度缓慢、制备周期长的缺点。这导致在生长K0.5Na0.5NbO3基单晶过程中,不可避免的引起K和Na元素的挥发,从而引起晶体成分不均匀、晶体结构缺陷难以控制、材料性能下降等。传统的陶瓷固相烧结技术能克服传统单晶生长法的缺点,是制备陶瓷最简便、易控制材料质量也是成本最低的常用技术。如何将这种多晶材料制备工艺的优势与单晶材料的结构性能优点相结合,创立、发展一种制备过程简便、成本低廉、性能优异的K0.5Na0.5NbO3基压电单晶的生长新技术和新方法,具有重要的研究意义和应用价值。
2009年,发明人在针对K0.5Na0.5NbO3基无铅压电陶瓷掺杂改性的研究过程中发现:在K0.5Na0.5NbO3基陶瓷中引入微量含铋(Bi)元素的复合氧化物时,采用传统的陶瓷制备工艺在常规条件下制备出K0.5Na0.5NbO3基单晶,实现陶瓷到单晶的转变[1. 江民红,刘心宇,邓满姣,陈国华. 铌酸钾钠织构陶瓷与铌酸钾钠单晶的制备方法. 中国,发明专利,申请号:201010247474.8;2. Minhong Jiang, Clive A. Randall, HanzhengGuo,GuanghuiRao, RongTu, ZhengfeiGu, Gang Cheng, Xinyu Liu, Jinwei Zhang, andYongxiang Li, Seed-Free Solid-State Growth of Large Lead-Free PiezoelectricSingle Crystals: (Na1/2K1/2)NbO3, Journal of the American Ceramic Society,2015, 98 (10):2988–2996.]。该现有技术与传统的晶体生长技术相比,该方法操作简便、设备简单,成本低,生长晶体组分的均匀性好、体系多样,适合生长组分熔点不同、宽范围溶解度、挥发性强、冷却阶段易发生破坏性相变的晶体。
现有技术存在以下问题:所制备的K0.5Na0.5NbO3基铁电压电单晶的压电常数仍较低等缺点,如d 33约为260 pC/N,该值虽然比纯K0.5Na0.5NbO3陶瓷材料高了2-3倍,但是对于晶体来讲仍不是十分理想。
发明内容
为了解决上述技术问题,本发明的目的是提供一种铌酸钾钠基压电单晶及其制备方法,以提高铌酸钾钠基单晶的压电性能。通过在99.6K0.5Na0.5NbO3-0.4LiBiO3基单晶的基础上适量掺入CaZrO3,实现显著提高铌酸钾钠基单晶的压电性能的目的。
实现本发明的具体技术方案如下:
K0.5Na0.5NbO3基铁电压电单晶以CaCO3、ZrO2、Li2CO3和Bi2O3作为掺杂原料,以K0.5Na0.5NbO3为主体材料组成,化学式为:xCaZrO3-(1–x)(99.6K0.5Na0.5NbO3-0.4LiBiO3),式中x表示体系中摩尔含量,其中0﹤x≤0.005。
本发明制备方法的具体步骤包括
步骤(1)所用原料Na2CO3 (99.8%)、K2CO3 (99%)、Nb2O5 (99.5%)、CaCO3(99%)、ZrO2(99%)、Li2CO3 (97%)和Bi2O3 (99%)均置于120℃的烘箱中烘干4~6 h;
步骤(2)按化学式的成分质量比称量原料装入HDPE材质的球磨瓶中,以无水乙醇为介质球磨24 h;
步骤(3)将球磨后产物取出,烘干,然后在850℃下预烧10 h;
步骤(4)然后再以无水乙醇为介质球磨24 h后烘干;
步骤(5)将烘干的粉料过100目筛后,在100 MPa的压力下压制成直径为14mm以上,厚度为2~3mm的圆坯;
步骤(6)将压制好的圆坯在1090-1115℃下保温15 h以上烧结获得单晶。
本发明制备方法采用传统陶瓷的制备工艺进行制备,包括湿磨、烘干、烧成、二次球磨、造粒、压制成型、烧结,与现有技术不同的是:
1. 以无水乙醇为介质湿磨24小时,烘干后在850℃保温10小时预合成瓷料;
2. 瓷料经二次球磨24小时,烘干后过100目筛,再在100MPa的压力下压制成型为14mm以上,厚度为2~3mm2素坯试样;
3. 将素坯试样水平放置于高温电炉中,在1090~1115℃保温烧结15小时以上,烧结后,随炉冷却至室温,即可获得铌酸钾钠基压电单晶。
本发明本发明与现有技术相比的优点是:在99.6K0.5Na0.5NbO3-0.4LiBiO3基单晶的基础上适量掺入CaZrO3,显著地提高了铌酸钾钠基单晶的压电性能,使其压电常数d 33最高达到488 pC/N。
附图说明:
图1为实施例中制备的K0.5Na0.5NbO3单晶样品相片;
图2为实施例中制备的K0.5Na0.5NbO3单晶样品的粉末XRD图谱。
具体实施方式
本发明通过实施例对本发明内容作进一步详细说明,但不是对本发明的限制。
实施例:
采用Na2CO3 (99.8%)、K2CO3 (99%)、Nb2O5 (99.5%)、CaCO3(99%)、ZrO2(99%)、Li2CO3(97%)和Bi2O3 (99%)为原料,用无籽固相生长技术制备K0.5Na0.5NbO3基无铅压电单晶。所有原料在称量配料前均置于120℃的烘箱中烘干6 h;准确称量后,将原料装入HDPE材质的球磨瓶中,以无水乙醇为介质球磨24 h,烘干后在850℃下预烧10 h,再以无水乙醇为介质球磨24 h后烘干;将烘干的粉料过100目筛后,在100 MPa的压力下压制成直径为50mm、厚度为3mm的圆坯;在1110℃保温52 h烧结,制得K0.5Na0.5NbO3基单晶。测试得其压电常数d 33达到488 pC/N。所制备的晶体样品如图1所示,其粉末衍射结果如图2所示。
Claims (5)
1.一种铌酸钾钠基压电单晶,其特征在于:所述铌酸钾钠基压电单晶以CaCO3、ZrO2、Li2CO3和Bi2O3作为掺杂原料,以K0.5Na0.5NbO3为主体材料组成,化学式为:xCaZrO3-(1–x)(99.6K0.5Na0.5NbO3-0.4LiBiO3),式中x表示体系中摩尔含量,其中0﹤x≤0.005。
2.根据权利要求1所述铌酸钾钠基压电单晶的制备方法,其特征在于包括以下步骤:
步骤(1)所用原料Na2CO3、K2CO3 、Nb2O5、CaCO3、ZrO2、Li2CO3 和Bi2O3均置于烘箱中烘干;
步骤(2)按化学式的成分质量比称量原料装入HDPE材质的球磨瓶中,以无水乙醇为介质球磨24 h;
步骤(3)将球磨后产物取出,烘干,预烧;
步骤(4)然后再以无水乙醇为介质球磨24 h后烘干;
步骤(5)将烘干的粉料过100目筛后,在100 MPa的压力下压制成直径为14mm以上,厚度为2~3mm的圆坯;
步骤(6)将压制好的圆坯烧结获得单晶。
3.根据权利要求2所述的制备方法,其特征在于:所述步骤(1)烘干温度为120℃,烘干时间为4~6 h。
4.根据权利要求2所述的制备方法,其特征在于:所述步骤(2)预烧温度为850℃,预烧时间为10 h。
5.根据权利要求2所述的制备方法,其特征在于:所述步骤(6)烧结温度为1090-1115℃,烧结时保温时间为15 h。
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CN107098699A (zh) * | 2017-03-28 | 2017-08-29 | 同济大学 | 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 |
CN107675257A (zh) * | 2017-11-13 | 2018-02-09 | 桂林电子科技大学 | 一种低损耗铁电压电单晶材料及其制备方法 |
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Application publication date: 20170322 Assignee: Guilin Xianjingkuangbao Technology Development Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2023980046674 Denomination of invention: A potassium sodium niobate based piezoelectric single crystal and its preparation method Granted publication date: 20190108 License type: Common License Record date: 20231109 |