CN104341003A - 一种TiO2纳米纱布的制备方法 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract 19
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 40
- 239000002253 acid Substances 0.000 claims description 25
- 239000000758 substrate Substances 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- -1 perfluoroethylene-propylene Chemical group 0.000 claims description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 6
- 239000002121 nanofiber Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 229910003705 H2Ti3O7 Inorganic materials 0.000 abstract 1
- 229910020293 Na2Ti3O7 Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 abstract 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 231100001240 inorganic pollutant Toxicity 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Inorganic Chemistry (AREA)
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Abstract
本发明属于无机纳米材料制备领域,旨在提供一种TiO2纳米纱布的制备方法。本发明包括如下步骤:钛酸钠(Na2Ti3O7)纳米纱布的制备、钛酸(H2Ti3O7)纳米纱布的制备、TiO2纳米纱布的制备。本发明的有益效果是:本发明中所制得的TiO2纳米纱布具有开放的形态,外来分子或离子可以接触整个TiO2纳米纱布。与普通的纳米TiO2粉末相比,具有一定的宏观效应,且其性能更为优越,制作方法简单,成本低;此类TiO2纳米纱布使得TiO2纳米纤维展现出了独特的整流效应和长程导电性。可以在高温过滤、电子器件、光催化等方面具有广泛的应用。
Description
技术领域
本发明属于无机纳米材料制备领域,具体涉及一种TiO2纳米纱布的制备方法。
背景技术
近三十年来纳米技术的高速发展,纳米材料的研究已在世界范围内掀起了一阵阵新的浪潮。较一维的纳米结构而言,有序的二维和三维纳米材料具有更优异的整体协同性质。
碱金属钛酸盐如钛酸钠(Na2Ti3O7)的晶型结构由Ti-O6八面体通过共边和共顶点组成,再形成层状结构,层与层之间的空隙被Na+占据,而Na+可以很容易地被质子或各种金属离子(Li+,Cd2+,Ru3+等)所替代。因此Na2Ti3O7在功能性有机物的吸附和重金属或放射性离子的去除等领域有着非常广泛的应用。但是钛酸盐在光催化活性、结构缺陷、光生电子的湮灭等方面不如TiO2理想。
TiO2是一种宽带半导体,室温下禁带宽度大于3.2eV。基于能带理论,TiO2在波长小于387.5nm的紫外光照射下,价带上的电子获得光子的能量而跃迁到导带,形成光生电子(e-),而同时在价带中形成了光生空穴(h+)。光生电子(e-)具有高的还原性,可以去除水体中的金属离子;而分布在表面的光生空穴(h+)能将OH-和H2O氧化成OH自由基。OH自由基具有强氧化性,能氧化大部分的有机污染物和无机污染物,最终分解为CO2、H2O和无机物,并将各种有害气体如SO2、H2S、NO和NO2等转化成无毒无害物质。TiO2表现出了优异的光催化氧化性质,但是纳米TiO2颗粒因为过于细小,在水溶液中容易团聚、不易沉降、难以回收;并且光致电子和光致空穴容易发生复合导致光量子效率很低;还有报道证实,纳米粒子对人体存在生物毒性,从而限制了其实际应用。随着对纳米材料研究的不断深入,研究人员发现现有的一维纳米材料并不能完全满足实际应用的需要。
发明内容
本发明要解决的技术问题是,克服现有技术中的不足,提供一种TiO2纳米纱布的制备方法。
为解决技术问题,本发明的解决方案是:
提供一种TiO2纳米纱布的制备方法,包括如下步骤:
步骤(1):钛酸钠(Na2Ti3O7)纳米纱布的制备
称取0.02~0.05g钛酸四正丁酯滴加入30~40mL的8~12M的NaOH溶液中,超声处理15~30min,直至形成稳定均一的混合物,然后转移到高压反应釜内,而该反应釜内侧附一层洁净的耐碱耐高温基底,封闭拧紧高压反应釜,置于预热的180~200℃烘箱内反应,水热反应36~60h后自然冷却至室温,将高压反应釜内基底整体取出,浸泡到去离子水中,在基底上分离出一层纱布,用去离子水洗涤至中性即得到钛酸钠纳米纱布,生成的纳米纱布长度为7.5~10cm,宽度为4.5~6cm,厚度约为0.05~0.1mm;
步骤(2):钛酸(H2Ti3O7)纳米纱布的制备
将步骤(1)制得的钛酸钠纳米纱布在0.1M的HCl溶液或HNO3溶液中浸泡,使钛酸钠中的Na+被H+取代,浸泡时间不低于12h,用去离子水洗涤至中性即得到钛酸纳米纱布;
步骤(3):TiO2纳米纱布的制备
将步骤(2)制得的钛酸纳米纱布经过500~700℃温度下退火处理2~3h,即得到TiO2纳米纱布。
本发明中,所述步骤(1)中的基底是具有平行纹路的聚四氟乙烯板或聚全氟乙丙烯板,并且使用时,需要保持其洁净度。
本发明中,所述步骤(1)中的水热反应即为水热合成,在水热合成过程中,钛酸四正丁酯在碱性条件下水解生成超长钛酸钠纳米纤维,同时以基底的平行纹路为框架来引导超长钛酸钠纳米纤维的自组装,最终形成具有宏观形态的钛酸钠纳米纱布。
与现有技术相比,本发明的有益效果是:
本发明中所制得的TiO2纳米纱布具有开放的形态,外来分子或离子可以接触整个TiO2纳米纱布。与普通的纳米TiO2粉末相比,具有一定的宏观效应,且其性能更为优越,制作方法简单,成本低;
此类TiO2纳米纱布使得TiO2纳米纤维展现出了独特的整流效应和长程导电性。可以在高温过滤、电子器件、光催化等方面具有广泛的应用。
附图说明
图1是TiO2纳米纱布的X射线粉末衍射(XRD)图谱;
图2是典型TiO2纳米纱布的扫描电镜(SEM)照片,其中:a是TiO2纳米纱布的整体扫描电镜照片;b是TiO2纳米纱布的局部放大扫描电镜照片。
具体实施方式
以下的实施例可以使本专业技术领域的技术人员更全面的了解本发明,但不以任 何方式限制本发明:
实施例1
一种TiO2纳米纱布,其主要成分是TiO2纳米纤维,具体制备工艺过程步骤如下:
步骤(1):钛酸钠(Na2Ti3O7)纳米纱布的制备
称取0.05g钛酸四正丁酯滴加入40mL NaOH(12M)溶液中,超声处理25min,直至形成稳定均一的混合物,然后转移到高压反应釜内,而该反应釜内侧附一层洁净的聚全氟乙丙烯板基底,封闭拧紧高压反应釜,置于预热的190℃烘箱内反应48h;反应完毕后自然冷却至室温,将高压反应釜内基底整体取出,浸泡到去离子水中,在基底上分离出一层纱布,用去离子水洗涤至中性即得到钛酸钠纳米纱布,生成的钛酸钠纳米纱布长度为10cm,宽度为6cm,厚度约为0.1mm。
步骤(2):钛酸(H2Ti3O7)纳米纱布的制备
将上述钛酸钠纳米纱布在0.1M的HCl溶液中浸泡,使钛酸盐中的Na+被H+取代,浸泡时间不低于12h,用去离子水洗涤至中性即得到钛酸纳米纱布。
步骤(3):TiO2纳米纱布的制备
将所得到的钛酸纳米纱布经过500℃温度下退火处理2h,即得到TiO2纳米纱布。
实施例2
制备步骤同实施例1,不同之处是:将所得到的钛酸纳米纱布经过500℃温度下退火处理3h,得到TiO2纳米纱布。
实施例3
制备步骤同实施例1,不同之处是:将所得到的钛酸纳米纱布经过600℃温度下退火处理2h,得到TiO2纳米纱布。
实施例4
制备步骤同实施例1,不同之处是:将所得到的钛酸纳米纱布经过600℃温度下退火处理3h,得到TiO2纳米纱布。
实施例5
制备步骤同实施例1,不同之处是:将所得到的钛酸纳米纱布经过700℃温度下退火处理3h,得到TiO2纳米纱布。
实施例6
制备步骤同实施例1,不同之处是:称取0.02g钛酸四正丁酯滴加入30mL NaOH(8M)溶液中,超声处理15min,直至形成稳定均一的混合物,然后转移到高压反应釜内,而该反应釜内侧附一层洁净的聚全氟乙丙烯板基底,封闭拧紧高压反应釜,置于预热的180℃烘箱内反应36h;反应完毕后自然冷却至室温,将高压反应釜内基底整体取出,浸泡到去离子水中,在基底上分离出一层纱布,用去离子水洗涤至中性即得到 钛酸钠纳米纱布,生成的钛酸钠纳米纱布长度为7.5cm,宽度为4.5cm,厚度约为0.05mm。
实施例7
制备步骤同实施例1,不同之处是:称取0.035g钛酸四正丁酯滴加入35mL NaOH(10M)溶液中,超声处理25min,直至形成稳定均一的混合物,然后转移到高压反应釜内,而该反应釜内侧附一层洁净的聚四氟乙烯板基底,封闭拧紧高压反应釜,置于预热的190℃烘箱内反应48h。反应完毕后自然冷却至室温,将高压反应釜内基底整体取出,浸泡到去离子水中,在基底上分离出一层纱布,用去离子水洗涤至中性即得到钛酸钠纳米纱布,生成的钛酸钠纳米纱布长度为8cm,宽度为5.25cm,厚度约为0.07mm。
实施例8
制备步骤同实施例1,不同之处是:称取0.05g钛酸四正丁酯滴加入40mL NaOH(12M)溶液中,超声处理30min,直至形成稳定均一的混合物,然后转移到高压反应釜内,而该反应釜内侧附一层洁净的聚四氟乙烯板基底,封闭拧紧高压反应釜,置于预热的200℃烘箱内反应60h;反应完毕后自然冷却至室温,将高压反应釜内基底整体取出,浸泡到去离子水中,在基底上分离出一层纱布,用去离子水洗涤至中性即得到钛酸钠纳米纱布,生成的钛酸钠纳米纱布长度为10cm,宽度为6cm,厚度约为0.1mm。
实施例9
制备步骤同实施例6,不同之处是:将所得到的钛酸纳米纱布经过500℃温度下退火处理3h,得到TiO2纳米纱布。
实施例10
制备步骤同实施例6,不同之处是:将所得到的钛酸纳米纱布经过600℃温度下退火处理2h,得到TiO2纳米纱布。
实施例11
制备步骤同实施例6,不同之处是:将所得到的钛酸纳米纱布经过600℃温度下退火处理3h,得到TiO2纳米纱布。
实施例12
制备步骤同实施例6,不同之处是:将所得到的钛酸纳米纱布经过700℃温度下退火处理3h,得到TiO2纳米纱布。
实施例13
制备步骤同实施例7,不同之处是:将所得到的钛酸纳米纱布经过500℃温度下退火处理3h,得到TiO2纳米纱布。
实施例14
制备步骤同实施例7,不同之处是:将所得到的钛酸纳米纱布经过600℃温度下退火处理2h,得到TiO2纳米纱布。
实施例15
制备步骤同实施例7,不同之处是:将所得到的钛酸纳米纱布经过600℃温度下退火处理3h,得到TiO2纳米纱布。
实施例16
制备步骤同实施例7,不同之处是:将所得到的钛酸纳米纱布经过700℃温度下退火处理3h,得到TiO2纳米纱布。
实施例17
制备步骤同实施例8,不同之处是:将所得到的钛酸纳米纱布经过500℃温度下退火处理3h,得到TiO2纳米纱布。
实施例18
制备步骤同实施例8,不同之处是:将所得到的钛酸纳米纱布经过600℃温度下退火处理2h,得到TiO2纳米纱布。
实施例19
制备步骤同实施例8,不同之处是:将所得到的钛酸纳米纱布经过600℃温度下退火处理2.5h,得到TiO2纳米纱布。
实施例20
制备步骤同实施例8,不同之处是:将所得到的钛酸纳米纱布经过700℃温度下退火处理3h,得到TiO2纳米纱布。
因此,本发明的实际范围不仅包括所公开的实施例,还包括在权利要求书之下实施或者执行本发明的所有等效方案。
Claims (2)
1.一种TiO2纳米纱布的制备方法,其特征在于,所述制备方法包括如下步骤:
步骤(1):钛酸钠纳米纱布的制备
称取0.02~0.05g钛酸四正丁酯滴加入30~40mL的8~12M的NaOH溶液中,超声处理15~30min,直至形成稳定均一的混合物,然后转移到高压反应釜中,且该高压反应釜内侧附有一层耐碱耐高温的基底,封闭拧紧高压反应釜,置于预热的180~200℃烘箱内反应,水热反应36~60h后自然冷却至室温,将高压反应釜内基底整体取出,浸泡到去离子水中,在基底上分离出一层纱布,用去离子水洗涤至中性即得到钛酸钠纳米纱布,生成的钛酸钠纳米纱布长度为7.5~10cm,宽度为4.5~6cm,厚度约为0.05~0.1mm;
步骤(2):钛酸纳米纱布的制备
将步骤(1)制得的钛酸钠纳米纱布在0.1M的HCl溶液或HNO3溶液中浸泡,使钛酸钠中的Na+被H+取代,浸泡时间不低于12h,用去离子水洗涤至中性即得到钛酸纳米纱布;
步骤(3):TiO2纳米纱布的制备
将步骤(2)制得的钛酸纳米纱布经过500~700℃温度下退火处理2~3h,即得到TiO2纳米纱布。
2.根据权利要求1所述的制备方法,其特征在于,所述步骤(1)中的基底为具有平行纹路的聚四氟乙烯板或聚全氟乙丙烯板。
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DEEPAK K. PATTANAYAK等: "Nanostructured positively charged bioactive TiO2 layer formed on Ti metal by NaOH, acid and heat treatments", 《J MATER SCI: MATER MED》, 14 June 2011 (2011-06-14), pages 1803 - 1812, XP 019932194, DOI: doi:10.1007/s10856-011-4372-x * |
DONG-SEOK SEO等: "Hydrothermal synthesis of Na2Ti6O13 and TiO2 whiskers", 《JOURNAL OF CRYSTAL GROWTH》, 21 December 2004 (2004-12-21), pages 2371 - 2376 * |
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