CN106631016B - 一种铌酸钾钠体系纳米线材料及其制备方法 - Google Patents
一种铌酸钾钠体系纳米线材料及其制备方法 Download PDFInfo
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- 239000002070 nanowire Substances 0.000 title claims abstract description 33
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 title claims description 27
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 239000011734 sodium Substances 0.000 claims abstract description 11
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000007790 solid phase Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 5
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 241000282414 Homo sapiens Species 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- VQFRLYRLYWAVAQ-UHFFFAOYSA-N [Ba].[Na].[K] Chemical compound [Ba].[Na].[K] VQFRLYRLYWAVAQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
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- 239000002808 molecular sieve Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 235000012149 noodles Nutrition 0.000 description 1
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- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供一种铌酸钾钠体系纳米线以Na2CO3、K2CO3、Li2CO3、Nb2O5、Bi2O3为原料，按照化学式99.6K0.5Na0.5NbO3‑0.4LiBiO3进行配料。其制备方法包括：（1）所有原料在称量配料前均置于烘箱中烘干；（2）准确称量后，以无水乙醇为介质球磨；（3）将球磨后产物取出，烘干，预烧；（4）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）将压制好的圆坯固相烧结，在烧结体中获得铌酸钾钠体系纳米线。本发明的优点是可采用传统陶固相烧结法获得铌酸钾钠基纳米线。
Description
技术领域
本发明涉及压电纳米材料领域，具体是一种铌酸钾钠体系纳米线材料及其制备方法。
背景技术
纳米技术作为21世纪一个重要新兴科技领域，在理论与实践上正经历着高速发展，大量新型纳米材料与器件不断被开发出来, 并在生物医学、国防以及日常生活的各个领域展现前所未有的应用前景。将基于压电效应的纳米材料技术用到纳米发电机、THz通信、生物医学传感器等方面正受到国际上极大的关注。特别是纳米发电机，《Science》、《Advance materials》杂志给予了专门报道。在有关纳米压电材料的应用上，铌酸钾钠体系具有综合性能优异的优势，如压电系数、机电耦合系数和居里温度高及组成元素对人类友好，这在作为植入人体的生物医疗器械方面尤为重要。
从压电式纳米换能器的效率方面来讲，除了在一定程度上受系统集成组装的质量影响外，最主要的影响因素应该是其核心部件—压电材料的压电性能，高压电系数的压电材料将表现出更高的压电性能。事实上，除了ZnO外，还包括现在应用最多的铅基压电陶瓷（如PZT），以及目前研究很热的几类无铅压电材料（如铌酸钾钠体系、钛酸钡钾钠体系等），后面这几类压电材料的压电性能都远高于ZnO。当然，由于铅基压电陶瓷含铅且含铅量高于60%（质量比）不利于人类环境保护而即将被淘汰，特别是作为植入人体的医疗器械，更不应该采用。作为替代，无铅压电材料的研究及尽早开发自然十分迫切。比较目前研究比较热的几类无铅压电材料，铌酸钾钠体系由于具有很好综合性能优势，如高的压电系数、高的机电耦合系数、高的居里温度和组成元素对人类友好，而成为首选材料之一。
目前，无铅压电材料研究报道最多的是块体陶瓷材料，但是在微纳技术领域则恰恰需要相应的具有微纳米尺寸的材料，例如在微型马达、生物医药传感器、监控、生物活体探测和太赫兹波通信等方面。从上述研究报道来看，目前针对铌酸钾钠纳米线的制备方法主要有模板生长法、水热法、溶胶-凝胶法、熔盐法和静电纺丝法等。虽然每种方法各有优点，但也各自存在一些问题。
模板生长法可以采用AAO、碳纳米管、分子筛和硅纳米线等模板进行辅助生长，具有纳米线排列可控、对材料结构限制少等优点，但是存在所制备的纳米线通常是多晶，不易获得单晶，且产物中因模板的存在易引入杂质的技术问题。
水热法和溶胶-凝胶法等液相法具有低温、低成本优势，及产量高和均匀性好等优点，但是存在产物长径比较低、尺寸较大，工艺复杂且产物纯度不高的技术问题。此外，水热法还存在只能用于制备对水或溶剂不敏感的化合物的技术问题。
此外，如果不结合使用模板生长法而单纯采用液相法，生长出来的铌酸钾钠纳米线则杂乱无章排列。
迄今为止，有关铌酸钾钠体系，特别是99.6K0.5Na0.5NbO3-0.4LiBiO3体系纳米线的固相制备技术还没有相关报道。
发明内容
本发明的目的是提供一种铌酸钾钠体系纳米线材料及其制备方法。针对现有技术存在的技术问题，本发明采用传统的固相烧结法，在不需要额外提供气相、异质模板和催化剂的的条件下，实现铌酸钾钠体系纳米线的可控生长，使合成的铌酸钾钠体系纳米线直接从同质基体中生长，不引入外界杂质，实现产物的纯洁。
为了实现上述发明目的，本发明采用的技术方案为：
一种铌酸钾钠体系纳米线材料，是以Na2CO3、K2CO3、Li2CO3、Nb2O5、Bi2O3为原料，按照化学式99.6K0.5Na0.5NbO3-0.4LiBiO3进行配料，经传统陶瓷固相烧结工艺烧制而成的纳米线材料。
铌酸钾钠体系纳米线材料的制备方法，包括以下步骤：
步骤（1）所有原料Na2CO3、K2CO3、Li2CO3、Nb2O5、Bi2O3在称量配料前均置于烘箱中烘干，所述烘干的温度为120℃；
步骤（2）按化学式99.6K0.5Na0.5NbO3-0.4LiBiO3的成分质量比称量原料，装入球磨瓶中，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，所述预烧的温度为850℃，预烧的时间为6h，预烧的升温速率为2℃/min；
步骤（4）然后再以无水乙醇为介质球磨24h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26 mm，2 mm厚的圆坯；
步骤（6）将压制好的圆坯固相烧结，在烧结体中获得铌酸钾钠体系纳米线材料，所述烧结的温度为1100℃，烧结时的保温时间为18h。
本发明铌酸钾钠体系纳米线材料经SEM电镜检测证实为纳米线结构。
本发明相对于现有技术，具有以下优点：
（1）采用传统的固相烧结法，在不需要额外提供气相的条件下，实现铌酸钾钠体系纳米线的可控生长；
（2）使合成的铌酸钾钠体系纳米线直接从同质基体中生长，不需要异质模板和催化剂，不会引入外界杂质，产物纯洁；
（3）在此方法制备的基础上，也可以利用化学拓扑法通过后续的液相、水热或气相辅助生长继续调控铌酸钾钠体系纳米线的长径比。
此外，实验研究显示，本发明技术关键在于化学成分、烧结工艺（特别是烧结温度）和实验环境等因素的精确控制。通过调控，可以实现99.6K0.5Na0.5NbO3-0.4LiBiO3体系纳米线的制取。本发明方法合成的铌酸钾钠体系纳米线后，将可能赋予它新的特性或功能，从而拓展铌酸钾钠体系纳米线的应用范畴，因此，本发明具有广阔的应用前景。
附图说明
图1为实施例中制备的铌酸钾钠体系纳米线材料的SEM图。
具体实施方式
本发明通过实施例，结合说明书附图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：
铌酸钾钠体系纳米线材料的制备方法，包括以下步骤：
步骤（1）所有原料Na2CO3、K2CO3、Li2CO3、Nb2O5、Bi2O3在称量配料前均置于烘箱中烘干，所述烘干的温度为120℃；
步骤（2）按化学式99.6K0.5Na0.5NbO3-0.4LiBiO3，即(1-x)K0.5Na0.5NbO3-xLiBiO3，其中x=0.004的成分质量比称量原料，装入球磨瓶中，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，所述预烧的温度为850℃，预烧的时间为6h，预烧的升温速率为2℃/min；
步骤（4）然后再以无水乙醇为介质球磨24h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26 mm，2 mm厚的圆坯；
步骤（6）将压制好的圆坯固相烧结，在烧结体中获得铌酸钾钠体系纳米线材料，所述烧结的温度为1100℃，烧结时的保温时间为18h。
经SEM电镜检测，结果如图1所示，所得铌酸钾钠体系纳米线材料为纳米线结构。
Claims (1)
1.一种铌酸钾钠体系纳米线材料的制备方法，其特征在于包括以下步骤：
步骤（1）所有原料Na2CO3、K2CO3、Li2CO3、Nb2O5、Bi2O3在称量配料前均置于烘箱中烘干，所述步骤（1）烘干的温度为120℃；
步骤（2）按化学式99.6K0.5Na0.5NbO3-0.4LiBiO3的成分质量比称量原料，装入球磨瓶中，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，所述步骤（3）预烧的温度为850℃，预烧的时间为6 h，预烧的升温速率为2℃/min；
步骤（4）然后再以无水乙醇为介质球磨24h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26 mm，2 mm厚的圆坯；
步骤（6）将压制好的圆坯固相烧结，在烧结体中获得铌酸钾钠体系纳米线材料，所述步骤（6）烧结的温度为1100℃，烧结时的保温时间为18h。
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Application publication date: 20170510 Assignee: Guilin Xianjingkuangbao Technology Development Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2023980046674 Denomination of invention: A potassium sodium niobate system nanowire material and its preparation method Granted publication date: 20191213 License type: Common License Record date: 20231109 Application publication date: 20170510 Assignee: Guilin Sensing Material Technology Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2023980046110 Denomination of invention: A potassium sodium niobate system nanowire material and its preparation method Granted publication date: 20191213 License type: Common License Record date: 20231107 |