CN109400154B - 一种双铌源碱金属铌酸盐微纳米线材料及其制备方法 - Google Patents
一种双铌源碱金属铌酸盐微纳米线材料及其制备方法 Download PDFInfo
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- 229910052783 alkali metal Inorganic materials 0.000 title claims abstract description 27
- 150000001340 alkali metals Chemical class 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000010955 niobium Substances 0.000 claims abstract description 44
- 238000000498 ball milling Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 16
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- 229910052758 niobium Inorganic materials 0.000 claims abstract description 15
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 10
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- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 6
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- 238000013329 compounding Methods 0.000 claims abstract description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 7
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- 238000001878 scanning electron micrograph Methods 0.000 description 3
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- 239000007791 liquid phase Substances 0.000 description 2
- 239000002127 nanobelt Substances 0.000 description 2
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- 238000003980 solgel method Methods 0.000 description 2
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
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Abstract
本发明公开了一种双铌源碱金属铌酸盐微纳米线材料，以K2CO3、Na2CO3、Nb2O5、C10H5NbO20、BaCO3、Bi2O3为原料，按照化学式(1‑y)K z Na1‑ z Nb(C)x Nb(N)1‑x O3‑yBaBiO3进行配料，其中Nb(C)是指来自铌源C10H5NbO20的Nb元素；Nb(N)是指来自铌源Nb2O5的Nb元素；0＜x≤0.1，0＜y＜0.1,0.4≤z≤0.6，经传统陶瓷固相烧结工艺合成的微纳米线材料。其制备方法包括以下步骤：1）原料烘干；2）原料称取，进行球磨；3）球磨之后粉料的预烧；4）预烧后粉料的第二次球磨；5）压制成圆坯；6）圆坯的保温处理。本发明的优点是，采用双铌源后，可以提高压坯粉料的结晶度和微纳米线的生长速度；同时球磨介质可使用纯净水，无需使用无水乙醇，极大节约成本、减小对环境的污染和烘干过程中的安全隐患。
Description
技术领域
本发明涉及微纳米材料与技术领域，具体是一种双铌源碱金属铌酸盐微纳米线材料及其制备方法。
背景技术
一维无铅钙钛矿材料，包括纳米线、纳米棒和纳米管，在环保、能源、生物医学、国防以及日常生活的各个领域展现出前所未有的应用前景。目前，人们通过多种方法合成了众多的纳米材料，如纳米线、纳米条、纳米棒、纳米带等。合成微纳米材料的方法主要有水热法、熔盐法、溶胶—凝胶法、模板法等，但是每种方法都存在一定的问题。模板生长法具有可以控制纳米材料的形状和尺寸、合成方式简单、适用批量生产等，但是模板中容易引入杂质。此外，如果不结合使用模板生长法而单纯采用液相法，生长出来的纳米线则杂乱无章排列。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。
最近，我们发明了一种固相法制备铌酸盐微纳米线的方法[江民红，严亚飞，郝崇琰，李林，饶光辉，成钢，顾正飞，刘心宇，一种碱金属铌酸盐微纳米线材料及其制备方法，申请号：201611181133.9]；[江民红，金琦，严亚飞，韩胜男，李林，饶光辉，成钢，顾正飞，刘心宇，一种锂、锑掺杂的碱金属铌酸盐微纳米线材料及其制备方法，申请号：201711116853.1]。采用该固相法，在不需要额外提供气相、异质模板和催化剂的条件下，实现碱金属铌酸盐微纳米线的可控生长，使合成的碱金属铌酸盐微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。
但该现有技术存在以下技术问题：
1、由于本领域早期实验经验发现，采用纯净水作为球磨介质，会产生团聚现象，影响粉料的活性，因此，本领域常规手段是采用无水乙醇作为球磨介质，而采用无水乙醇作为球磨介质，直接产生了生产成本的提升和生产过程中的安全隐患，以及环境污染问题；
2、预烧温度较高，需要达到700-900 ℃，显然，更高的温度条件带来了更高的能源消耗、设备的要求以及生产安全问题。
因此，解决以上技术问题，可以有效降低材料的生产成本，提高生产过程的安全性。
发明内容
本发明的目的是提供一种双铌源碱金属铌酸盐微纳米线材料及其制备方法。
针对现有技术存在的问题，本发明采用了一下技术手段进行解决：
1、通过选择合适的双铌源作为原料，以及控制反应条件，达到有效提高压坯粉料的结晶度和微纳米线的生长速度的技术效果，且在实现以纯净水为球磨介质的条件下，实现微纳米线材料的制备，打破常规制备方法中，必须采用无水乙醇作为球磨介质才能得到微纳米材料的认知；
2、利用不同铌源在反应过程中的不同反应活性，控制、改变反应历程，具体为，利用C10H5NbO20可以在较低的温度下分解，产生高反应活性的铌，从而改变反应历程，最终实现降低预烧温度的技术效果。
从而实现极大地节约生产成本，减小环境污染和无水乙醇在烘干过程中存在的潜在安全问题；降低预烧温度，缩短高温段保温时间，进一步节约生产成本；并有效提高压坯粉料的结晶度和微纳米线的生长速度。
为了实现上述发明目的，本发明采用的技术方案为：
一种双铌源碱金属铌酸盐微纳米线材料，是以K2CO3、Na2CO3、Nb2O5、C10H5NbO20、BaCO3、Bi2O3为原料，按照化学式(1-y)K z Na1-z Nb(c)xNb(N)1-x O3-yBaBiO3进行配料，其中Nb（C）是指来自C10H5NbO20的Nb元素；Nb（N）是指来自Nb2O5的Nb元素；0＜x≤0.1，0＜y＜0.1，0.4≤z≤0.6，经传统陶瓷固相烧结工艺合成的微纳米线材料。
一种 双铌源碱金属铌酸盐微纳米线材料的制备方法，包括以下步骤：
步骤（1）所有原料K2CO3、Na2CO3、Nb2O5、C10H5NbO20、BaCO3、Bi2O3在称量配料前均置于烘箱中烘干，烘干温度为120 ℃；
步骤（2）按照化学式(1-y)K z Na1-z Nb(c)xNb(N)1-x O3-yBaBiO3成分质量比称量原料，其中Nb（C）是指来自C10H5NbO20的Nb元素；Nb（N）是指来自Nb2O5的Nb元素；0＜x≤0.1，0＜y＜0.1，0.4≤z≤0.6，装入球磨瓶中，以纯净水和氧化锆球为介质球磨24-36h；
步骤（3）将球磨之后的粉料取出、烘干、预烧，预烧温度是130℃保温3h再升温至425-550℃保温3h，预烧的升温速率为1 ℃/min；
步骤（4）然后将预烧后的粉料再次装入球磨瓶中，以纯净水和氧化锆球为球磨介质，进行第二次球磨18-24h；
步骤（5）将第二次球磨后的粉料取出、烘干、过200目筛后，在100MPa的压力下压制成直径16mm，厚3mm的圆坯；
步骤（6）将压制好的圆坯在1080-1120℃保温10-30h处理，即可制得双铌源碱金属铌酸盐微纳米线材料。
本发明双铌源碱金属铌酸盐微纳米线材料经SEM电镜检测证实为微纳米线结构。
本发明相对于现有技术，具有以下优点:
本发明采用采用了简单低成本的陶瓷工艺，即传统的固相烧结工艺进行制备。采用双铌源后，可以有效提高压坯粉料的结晶度和微纳米线的生长速度；同时球磨介质可使用纯净水，无需使用无水乙醇，极大地节约了成本，减小了对环境的污染和无水乙醇在烘干过程中存在的潜在危害；预烧温度降低了150-425℃，缩短了高温段保温时间，进一步节约了成本，易于产业化。
附图说明
图1为实施例1中制备双铌源碱金属铌酸盐微纳米线的SEM图；
图2为实施例2中制备双铌源碱金属铌酸盐微纳米线的SEM图；
图3为实施例3中制备双铌源碱金属铌酸盐微纳米线的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做进一步详细说明，但不是对本发明的限定。
实施例1
一种双铌源碱金属铌酸盐微纳米线材料的制备方法：
步骤（1）所有原料K2CO3、Na2CO3、Nb2O5、C10H5NbO20、BaCO3、Bi2O3在称量配料前均置于烘箱中烘干，烘干温度为120℃；
步骤（2）按照化学式(1-y)K z Na1-z Nb(c)xNb(N)1-x O3-yBaBiO3成分质量比称量原料，其中Nb（C）是指来自C10H5NbO20的Nb元素；Nb（N）是指来自Nb2O5的Nb元素；x = 0.01，y = 0.05， z= 0.54。装入球磨瓶中，以纯净水和氧化锆球为介质球磨24h；
步骤（3）将球磨之后的粉料取出、烘干、预烧，预烧温度是200℃保温3h再升温至500℃保温3h，升温速率为1min/℃；
步骤（4）然后将预烧后的粉料再次装入球磨瓶中，以纯净水和氧化锆球为球磨介质，进行第二次球磨18h；
步骤（5）将二次球磨后的粉料取出、烘干、过200目筛后，在100MPa的压力下压制成直径16mm，厚3mm的圆坯；
步骤（6）将压制好的圆坯在1112℃保温处理12h，即可制得双铌源碱金属铌酸盐微纳米线材料。
经SEM检测，所得双铌源碱金属铌酸盐微纳米线材料如图1所示。
实施例2
一种双铌源碱金属铌酸盐微纳米线材料的制备方法：
未特别说明的步骤与实施例1的制备方法相同，不同之处在于：步骤（6）中保温处理18h。
经SEM检测，所得双铌源碱金属铌酸盐微纳米线材料。
实施例3
一种双铌源碱金属铌酸盐微纳米线材料的制备方法：
未特别说明的步骤与实施例1的制备方法相同，不同之处在于：步骤（6）中保温处理24h。
经SEM检测，所得双铌源碱金属铌酸盐微纳米线材料如图3所示。
Claims (2)
1.一种双铌源碱金属铌酸盐微纳米线材料，其特征在于：所述碱金属铌酸盐微纳米线材料是以K2CO3、Na2CO3、Nb2O5、C10H5NbO20、BaCO3、Bi2O3为原料，按照化学式(1-y)K z Na1-z Nb(C) x Nb(N)1-x O3-yBaBiO3进行配料，其中Nb(C)是指来自铌源C10H5NbO20的Nb元素；Nb(N)是指来自铌源Nb2O5的Nb元素；0＜x≤0.1，0＜y＜0.1, 0.4≤z≤0.6，经传统陶瓷固相烧结工艺合成的微纳米线材料。
2.根据权利要求1所述的双铌源碱金属铌酸盐微纳米线材料的制备方法，其特征包括以下步骤：
步骤（1）所有原料K2CO3、Na2CO3、Nb2O5、C10H5NbO20、BaCO3、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）按照化学式(1-y)K z Na1-z Nb(c)x Nb(N)1-x O3-yBaBiO3成分质量比称量原料，装入球磨瓶中，以纯净水和氧化锆球为介质球磨24-36h；
步骤（3）将球磨之后的粉料取出、烘干、预烧；所述步骤（3）预烧的温度为130℃保温3h再升温至425-550℃保温3h，预烧的升温速率为1℃/min；
步骤（4）然后将预烧后的粉料再次装入球磨瓶中，以纯净水和氧化锆球为球磨介质，进行第二次球磨18-24h；
步骤（5）将第二次球磨后的粉料取出、烘干、过200目筛后，在100MPa的压力下压制成直径16mm，厚3mm的圆坯；
步骤（6）将压制好的圆坯在一定条件下保温处理，即可制得双铌源碱金属铌酸盐微纳米线材料；所述步骤（6）保温的温度为1080-1120℃，保温时间为10-30h，升温速率为1℃/min。
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Application publication date: 20190301 Assignee: Guilin Xianjingkuangbao Technology Development Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2023980046674 Denomination of invention: A dual niobium source alkali metal niobate micro nanowire material and its preparation method Granted publication date: 20210604 License type: Common License Record date: 20231109 |