CN105834448A - 一步法制备Ag@TiO2纳米复合材料 - Google Patents
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 21
- 235000019441 ethanol Nutrition 0.000 claims abstract description 13
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 26
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 12
- 239000002105 nanoparticle Substances 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- APQHKWPGGHMYKJ-UHFFFAOYSA-N Tributyltin oxide Chemical compound CCCC[Sn](CCCC)(CCCC)O[Sn](CCCC)(CCCC)CCCC APQHKWPGGHMYKJ-UHFFFAOYSA-N 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 238000006266 etherification reaction Methods 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 abstract 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 13
- 239000000203 mixture Substances 0.000 description 9
- 239000002131 composite material Substances 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000013528 metallic particle Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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Abstract
本发明涉及一种一步制备Ag@TiO2纳米复合材料的方法，属于材料化学合成领域。本发明工艺过程中，乙醇既作为溶剂又作为还原剂，在高温高压的水热环境下，乙醇的羟基将Ag+还原成单质Ag颗粒，同时乙醇间醚化反应生成的H2O也促进了钛酸正丁酯（TBOT）的水解。为了降低体系的表面能，水解产生的TiO2小粒子逐渐与生成的Ag纳米颗粒一起聚集成球，并将其包覆到TiO2球内；随着反应的进行，最终得到了球状Ag@TiO2纳米复合材料。该方法具有操作简单，原料易得，成本低，过程可控等优点。通过此方法制备的球状Ag@TiO2纳米复合材料，在光催化和表面增强拉曼效应等领域有着潜在的应用前景。
Description
技术领域
本发明涉及一种一步法制备Ag@TiO2纳米复合材料的方法，属于材料化学合成领域。
背景技术
随着纳米技术的发展，以半导体金属氧化物为基础的拥有灵活的化学组成和良好形貌结构的异质纳米材料已经引起了科学家极大的研究兴趣，并被广泛应用于生物医药、光催化和纳米器件等领域。当前，多种异质结构如半导体-半导体、金属-半导体和金属-金属等已被研究和开发出来。特别地，贵金属-半导体异质结，因其在光催化和表面拉曼增强等领域具有广阔的应用前景而成为最受欢迎的异质结之一。通过将金属与半导体氧化物进行结合，一方面可增强光催化氧化还原反应进程，因为金属较高的费米能级能够有效地分离半导体光激发电子与空穴对；同时金属可以作为一个光电子容器，提高了界面电荷转移过程，并且阻缓了半导体光激发电子与空穴的复合。
在众多半导体金属氧化物中，二氧化钛（TiO2）兼具高的光催化活性、成本低、毒性小以及良好的化学和热稳定性等优点，成为最有潜力的半导体纳米材料之一。相比于金属纳米粒子简单附着于TiO2表面的金属-TiO2复合材料，拥有核壳结构或限域空间内的金属@TiO2材料展现出更为优异的光催化活性。这是因为这种结构能够使TiO2与金属粒子之间连接更为紧密，从而增强了两种物质之间的界面相互作用，提高了颗粒间电荷分离效率。同时这种异质结构能够避免金属颗粒在光催化反应中发生溶解或泄漏，确保了该材料的循环稳定性。尽管多种金属@TiO2复合纳米粒子（如Au、Ag、Pt等）已经被开发出来，然而目前制备金属@TiO2复合纳米材料的路线还是典型的两步法，主要包括金属纳米颗粒的合成以及后续TiO2壳层的包覆。这种合成路线通常要求精确控制金属颗粒的均匀性以及TiO2壳层的厚度。此外，在包覆过程中还需要稳定剂来防止金属粒子团聚，这就导致TiO2与金属之间出现一有机层，那将进一步阻碍粒子间电荷的分离和传输，造成光催化性能的降低。
发明内容
本发明的目的是提供一种Ag@TiO2纳米复合材料的制备方法。
本发明以钛酸正丁酯（TBOT）为钛源，硝酸银、乙醇等为原料，采用一步水热法制备了球状形貌的Ag@TiO2纳米复合材料。
为达到上述目的，本发明采用以下技术方案：
一步法制备Ag@TiO2纳米复合材料的方法，其特征在于该方法的具体步骤为：
a.将钛酸正丁酯和硝酸银溶于无水乙醇中混合均匀，其中硝酸银的浓度为0.08~0.12mol/L；所述的钛酸正丁酯和硝酸银的摩尔比是22:1~35:1；
a.将步骤a所得溶液在180 ℃条件下反应12~18 h，反应完成后，产物经离心分离、乙醇和去离子水洗涤后，烘干即得Ag@TiO2纳米复合材料。
本发明的工艺过程中，乙醇既作为溶剂也作为还原剂，在高温高压的水热环境下，乙醇的羟基将Ag+还原成单质Ag颗粒，同时乙醇间醚化反应生成的H2O也促进了TBOT的水解。为了降低体系的表面能，水解产生的TiO2小粒子逐渐与生成的Ag纳米颗粒一起聚集成球，同时Ag纳米颗粒被TiO2包覆到球内。随着反应的进行，最终得到了球状Ag@TiO2纳米复合材料。
本发明方法具有操作简单，原料易得，成本低，过程可控等优点。通过此方法制备的Ag@TiO2复合材料，在光催化和表面增强拉曼等领域有着潜在的应用前景。
附图说明
图1为本发明实施例1中所得Ag@TiO2纳米复合材料的XRD谱图。
图2为本发明实施例1中所得Ag@TiO2纳米复合材料的TEM图片。
图3为本发明实施例1中所得Ag@TiO2纳米复合材料的STEM图片和相应的元素分布。
具体实施方式
所有实施例均按上述技术方案的操作步骤进行操作。
实施例1
a.分别量取30 mL无水乙醇、0.12 mL 钛酸正丁酯（TBOT）溶液和0.12 mL 硝酸银（AgNO3）溶液（0.1 mol/L），放入50 mL平底烧瓶中混合搅拌10 min；
b.将上述溶液转移到50 mL的带聚四氟乙烯内衬的高压反应釜中，在180 ℃条件下反应12 h，反应完成后，将产物从反应釜中取出，经过离心、乙醇和去离子水反复洗涤后，在60℃下烘干，即得本发明制备的球状Ag@TiO2纳米复合材料。
将所制备的样品进行物性表征，其部分结果如附图所示。从TEM照片可以看出，制得的Ag@TiO2纳米复合材料是由很多TiO2小颗粒堆积组成的球形结构，其粒径在200~250 nm左右。其中，氧化钛内部的Ag纳米颗粒尺寸在10~15 nm。
实施例2
本实施例的制备过程和步骤与实施例1完全相同，不同在于a步骤：
a.分别量取20 mL无水乙醇、0.1 mL 钛酸正丁酯（TBOT）溶液和0.12 mL 硝酸银（AgNO3）溶液（0.1 mol/L），放入50 mL平底烧瓶中混合搅拌10 min；
所得结果与实施例1基本相似，不同在于得到的复合材料中，Ag颗粒核心尺寸明显变大为20~50 nm。
实施例3
本实施例的制备过程和步骤与实施例1完全相同，不同在于a和b步骤：
a.分别量取30 mL无水乙醇、0.1 mL 钛酸正丁酯（TBOT）溶液和0.1 mL 硝酸银（AgNO3）溶液（0.1 mol/L），放入50 mL平底烧瓶中混合搅拌10 min；
b.将上述溶液转移到50 mL的带聚四氟乙烯内衬的高压反应釜中，在180 ℃条件下反应18 h，反应完成后，将产物从反应釜中取出，经过离心、乙醇和去离子水反复洗涤后，在60℃下烘干，即得本发明制备的Ag@TiO2复合材料。
所得结果与实施例1基本相似，不同在于得到的产物是空心核壳结构，粒径在180~200 nm之间，Ag颗粒尺寸为20 nm左右。
参见附图，图1为本发明实施例1所得Ag@TiO2纳米复合材料的XRD谱图。XRD分析：在日本RigaKu D/max-2550型X射线衍射仪上进行；采用CuKα衍射。从图1 中可知，本发明所得球状Ag@TiO2纳米复合材料具有典型的锐钛矿结构，与标准谱图（JCPDF No. 21-1272）相一致。同时，在2θ = 44.3、64.4和77.4°出现的衍射峰分别对应Ag面心立方结构的（200），（220）和（311）晶面，说明Ag纳米颗粒被成功包覆到TiO2中。
参见附图，图2为本发明实施例1所得Ag@TiO2纳米复合材料的透射电镜（TEM）图片。TEM分析：采用日本电子株式会社JEOL-200CX 型透射电子显微镜观察材料形貌。从TEM图片可以看出，制得的Ag@TiO2复合材料拥有较好的球形形貌，主要由许多TiO2小颗粒堆积组成，其粒径尺寸在200到250 nm之间。其中，氧化钛球内部的Ag颗粒尺寸在10~15 nm。
参见附图，图3为本发明实施例1所得Ag@TiO2纳米复合材料的扫描透射电镜（STEM）图片和相应的元素Map分析。STEM分析：采用日本电子株式会社JEM-2010F型透射电子显微镜观察材料形貌。从中可知，只有Ti、Ag和O元素的信号被检测到，说明产品高的化学纯度。同时可以观察到Ag颗粒均匀分散在TiO2球体的内部，进一步证实Ag纳米颗粒被成功包覆。
Claims (1)
1.一步法制备Ag@TiO2纳米复合材料的方法，其特征在于该方法的具体步骤为：
a.将钛酸正丁酯和硝酸银溶于无水乙醇中混合均匀，其中硝酸银的浓度为0.08~0.12mol/L；所述的钛酸正丁酯和硝酸银的摩尔比是22:1~35:1；
b.将步骤a所得溶液在180 ℃条件下反应12~18 h，反应完成后，产物经过离心分离、乙醇和去离子水洗涤后，烘干，即得Ag@TiO2纳米复合材料。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793236A (zh) * | 2017-05-05 | 2018-11-13 | 国家电投集团科学技术研究院有限公司 | 钛酸盐纳米材料及其制备方法 |
| CN110605117A (zh) * | 2019-07-30 | 2019-12-24 | 北京氦舶科技有限责任公司 | 一种原子级分散的Ag负载纳米TiO2催化剂的制备方法 |
| CN110961620A (zh) * | 2019-12-13 | 2020-04-07 | 武汉工程大学 | 一种用于sers检测的纳米材料及其制备方法和用途 |
| CN111744474A (zh) * | 2020-06-19 | 2020-10-09 | 湖南工业大学 | 一种纳米复合材料、其制备方法及用途 |
| CN113600184A (zh) * | 2021-08-19 | 2021-11-05 | 曹洋 | 一种二氧化钛包覆金属纳米材料的合成方法及其应用 |
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| CN108793236A (zh) * | 2017-05-05 | 2018-11-13 | 国家电投集团科学技术研究院有限公司 | 钛酸盐纳米材料及其制备方法 |
| CN110605117A (zh) * | 2019-07-30 | 2019-12-24 | 北京氦舶科技有限责任公司 | 一种原子级分散的Ag负载纳米TiO2催化剂的制备方法 |
| CN110961620A (zh) * | 2019-12-13 | 2020-04-07 | 武汉工程大学 | 一种用于sers检测的纳米材料及其制备方法和用途 |
| CN111744474A (zh) * | 2020-06-19 | 2020-10-09 | 湖南工业大学 | 一种纳米复合材料、其制备方法及用途 |
| CN111744474B (zh) * | 2020-06-19 | 2022-09-09 | 湖南工业大学 | 一种纳米复合材料、其制备方法及用途 |
| CN113600184A (zh) * | 2021-08-19 | 2021-11-05 | 曹洋 | 一种二氧化钛包覆金属纳米材料的合成方法及其应用 |
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