CN107188237B - Fe、C共掺杂WO3多孔球及其制备方法和应用 - Google Patents
Fe、C共掺杂WO3多孔球及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于纳米材料技术领域，公开一种Fe、C共掺杂WO3多孔球及其制备方法和应用。将WCl6、Fe(NO3)3·6H2O、碳球加入到DMF中，室温下搅拌均匀后，将混合液转移到水热反应釜中，110~130℃溶剂热4~5 h，反应结束后离心、洗涤、干燥；其中，以质量体积比计，WCl6∶Fe(NO3)3·6H2O∶碳球∶DMF=0.9~1 g∶6.6~66.6 mg∶0.18~0.42 g∶50~70 mL；将干燥过的固体升温至400~650℃，煅烧1~2h，即得目标产物。本发明以碳球为模板，制备了Fe、C共掺杂的含ε相的WO3多孔球，提高对丙酮的选择性和灵敏度，为呼气中丙酮的检测提供了可能。
Description
技术领域
本发明属于纳米材料技术领域，具体涉及一种Fe、C共掺杂WO3多孔球及其制备方法和应用。
背景技术
呼气中大多数气体是新陈代谢的产物，其浓度的变化可反映身体状况，因此一些气体可作为特种疾病的生物标记物。丙酮是乙酰辅酶A的代谢产物，可作为糖尿病的生物标记物。健康人群呼气中丙酮含量为300−900 ppm，而糖尿病患者呼气中丙酮含量高于1800ppm，因此，通过呼气中丙酮含量的检测从而诊断糖尿病具有重要意义。
WO3作为一种典型的n-型半导体，被广泛应用到痕量丙酮的检测中，然而，WO3基气敏材料用于丙酮检测时仍然存在一些问题，比如灵敏度低、选择性差。WO3具有不同的晶相，包括单斜Ⅱ(ε-WO3)相、单斜Ⅰ(γ-WO3)相和正交(β-WO3)相等，其中ε-WO3由于具有铁电性而与极性较大的丙酮分子间具有较强的相互作用，从而对丙酮表现出高灵敏度和高选择性。
对WO3材料本身的形貌控制，也是提高其气敏性能的有效手段。构建分级结构能够最大化地促进气体的传输和扩散，有利于氧化物表面化学反应的加快进行。
发明内容
本发明的目的旨在提供一种Fe、C共掺杂WO3多孔球及其制备方法和应用。
为实现上述目的，本发明采取的技术方案如下：
Fe、C共掺杂WO3多孔球的制备方法，包括以下步骤：
S1、将WCl6、Fe(NO3)3·6H2O、碳球加入到DMF中，室温下搅拌均匀后，将混合液转移到水热反应釜中，110~130 ℃溶剂热4~5 h，反应结束后离心、洗涤、干燥；其中，以质量体积比计，WCl6∶Fe(NO3)3·6H2O∶碳球∶DMF = 0.9~1 g∶6.6~66.6 mg∶0.18~0.42 g∶50~70 mL；
S2、将干燥过的固体升温至400~650 ℃，煅烧1 ~2 h，即得目标产物。
较好地，S2中，以2~5 ℃/min的升温速率升温。
最佳地，所述制备方法，包括以下步骤：
S1、以质量体积比计，称取1 g WCl6、35.4 mg的Fe(NO3)3·6H2O、0.30 g碳球加入到60 mL DMF中，室温下搅拌均匀后，将混合液转移到水热反应釜中，120 ℃溶剂热4 h，反应结束后离心、洗涤、干燥；
S2、将干燥过的固体，以2 ℃/min的升温速率升温至450 ℃，煅烧1 h，即得目标产物。
前述制备方法制备的Fe、C共掺杂WO3多孔球。
所述Fe、C共掺杂WO3多孔球在检测丙酮气体中的应用。
本发明具有以下优点：
本发明以碳球为模板，制备了Fe、C共掺杂的含ε相的WO3多孔球，提高对丙酮的选择性和灵敏度，为呼气中丙酮的检测提供了可能。
附图说明
图1是W0和FW1−FW5样品的Raman图。
图2是FW3样品的XPS图。
图3是FW3样品的SEM图。
图4是FW3样品的TEM和HRTEM图。
图5是FW3样品的EDS图。
图6是W0、FW1−FW5和纯WO3样品的气敏性能图。
具体实施方式
下面结合具体实施例对本发明的技术方案作进一步解释说明，但本发明的保护范围并不局限于此。
实施例1
一种Fe、C共掺杂WO3多孔球的制备方法，包括以下步骤：
S1、称取1 g WCl6和6.6 mg的Fe(NO3)3·6H2O溶于30 mL DMF，再称取0.30 g碳球分散于30 mL DMF，在搅拌下将前溶液缓慢加入到后分散液中，室温下持续搅拌20 min后，将混合液转移到100 mL的水热反应釜中，120 ℃溶剂热4 h，反应结束后离心、洗涤、干燥；
S2、将干燥过的固体放入马弗炉中，以2 ℃/min的升温速率至450 ℃煅烧1 h，得目标产物。
实施例2
与实施例1的不同之处在于：S1中，加入Fe(NO3)3·6H2O的质量为21.0 mg。
实施例3
与实施例1的不同之处在于：S1中，加入Fe(NO3)3·6H2O的质量为35.4 mg。
实施例4
与实施例1的不同之处在于：S1中，加入Fe(NO3)3·6H2O的质量为50.7 mg。
实施例5
与实施例1的不同之处在于：S1中，加入Fe(NO3)3·6H2O的质量为66.6 mg。
对照例1
与实施例1的不同之处在于：S1中，加入Fe(NO3)3·6H2O的质量为0 mg，即不掺杂Fe。
将实施例1~5所得产物，依次命名为FW1−FW5，对照例1所得未掺杂Fe样品命名为W0；其中FW1代表实施例1产品，FW2代表实施例2产品，FW3代表实施例3产品，FW4代表实施例4产品，FW5代表实施例5产品。
产物表征
图1是W0和FW1−FW5样品的Raman图，图1（b）是图1（a）的局部放大图，a为W0样品，b−f依次为FW1−FW5样品。结果表明，掺杂FW1−FW5样品为ε和γ相的混合相，由图1(b)可知，掺杂Fe可使峰向低频率偏移，并且偏移程度随着掺杂量的增加而增大。证明Fe掺杂到WO3晶格中，并且引起材料中氧空位数量增加。
图2是FW3样品的XPS图，图2b C 1s中282.7 eV处的峰归属于W-C键，证明C掺杂到WO3晶格中，同时检测到Fe 2p的三个峰(图2d)，分别位于709.5、710.9和724.6 eV处，后两个峰分别归属于Fe3+ 2p3/2和Fe3+ 2p1/2，和Fe2O3中Fe 2p所在位置相比，掺杂到WO3晶格中的Fe的峰位置向高结合能方向移动。峰偏移证明Fe3+阳离子掺杂到了WO3晶格中替代W6+的位置。
图3是FW3样品的SEM图谱，图3(a)、(b)是FW3样品在不同放大倍数下的SEM图，且图3(b)样品经过氩离子抛光。从图3(a)可看出制备的WO3材料是球形形貌，由图3(b)可知球体内部呈现多孔结构。
图4(a)为FW3样品的TEM图，进一步表明材料为多孔结构，且由表面光滑的纳米颗粒组成。图4(b)、(c)为FW3的HRTEM图。图4(b)中晶格条纹清晰可见，说明样品的结晶度很好。通过计算可得晶面间距0.433 nm和0.368 nm分别对应于γ-WO3的(111)面和ε-WO3的(110)面，说明样品是ε相和γ相两相的混合相。图4(c)中发现晶格位错和切变等缺陷现象（如虚线矩形框所示），与晶格矩阵存在明显差别，缺陷的存在可能是由Fe掺杂生成的氧空位导致的。
图5为FW3样品的EDS图，6.4 KeV处的峰属于Fe的峰，证明Fe掺杂到WO3晶格中。
气敏性能测试
将实施例1~5 所得产物FW1-FW5以及对照例1所得产物W0研磨后滴加异丙醇混合成浆后，涂到陶瓷管表面，在马弗炉中以2 ℃/min的升温速率升温到380 ℃保持1 h，去除有机物，取出冷却到室温，即为气敏元件。采用WS-30A型号气敏测试仪（郑州炜盛电子科技有限公司），按照文献Sensors and Actuators B: Chemical, 209(2015) 622-629中的测试方法进行测试。
图6a是FW1-FW5对10 ppm丙酮气体的气敏性能图。由图6a可知：实施例3制备的Fe、C共掺杂WO3多孔球(FW3)在300 ℃工作温度下对丙酮的响应最高，达到17.7。
图6b是FW3、W0以及纯WO3（与实施例1相比，不添加Fe(NO3)3·6H2O和碳球，其它均同实施例1条件下所制备的产物）对不同浓度丙酮响应的对比图，结果表明：掺杂Fe后材料对丙酮的气敏性能明显提高。
图6c是FW3的选择性测试(气体浓度均为2 ppm)，结果表明：实施例3制备的Fe、C共掺杂WO3多孔球对丙酮具有良好的选择性。
图6d是FW3在不同湿度下对不同浓度丙酮的响应，结果表明：实施例3制备的Fe、C共掺杂WO3多孔球在高湿度下对丙酮也具有良好的响应。
图6e是FW3的稳定性测试，结果表明：实施例3制备的Fe、C共掺杂WO3多孔球对不同浓度的丙酮气体均具有良好的长时间稳定性。
Claims (4)
1.Fe、C共掺杂WO3多孔球的制备方法，其特征在于，包括以下步骤：
S1、将WCl6、Fe(NO3)3·6H2O、碳球加入到DMF中，室温下搅拌均匀后，将混合液转移到水热反应釜中，110~130 ℃溶剂热4~5 h，反应结束后离心、洗涤、干燥；其中，以质量体积比计，WCl6∶Fe(NO3)3·6H2O∶碳球∶DMF = 0.9~1 g∶6.6~66.6 mg∶0.18~0.42 g∶50~70 mL；
S2、将干燥过的固体升温至400~650 ℃，煅烧1 ~2 h，即得目标产物。
2.如权利要求1所述的制备方法，其特征在于：S2中，以2~5 ℃/min的升温速率升温。
3.如权利要求1所述的制备方法，其特征在于，包括以下步骤：
S1、以质量体积比计，称取1 g WCl6、35.4 mg的Fe(NO3)3·6H2O、0.30 g碳球加入到60mL DMF中，室温下搅拌均匀后，将混合液转移到水热反应釜中，120 ℃溶剂热4 h，反应结束后离心、洗涤、干燥；
S2、将干燥过的固体，以2 ℃/min的升温速率升温至450 ℃，煅烧1 h，即得目标产物。
4.如权利要求1~3之任一所述制备方法制备的Fe、C共掺杂WO3多孔球。
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| Application Number | Priority Date | Filing Date | Title |
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| CN106241879A (zh) * | 2016-07-20 | 2016-12-21 | 河南科技大学 | 一种纳米三氧化钨空心团聚球粉末的制备方法 |
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| CN106241879A (zh) * | 2016-07-20 | 2016-12-21 | 河南科技大学 | 一种纳米三氧化钨空心团聚球粉末的制备方法 |
Non-Patent Citations (5)
| Title |
|---|
| Ag Nanoparticle-Sensitized WO3 Hollow Nanosphere for Localized Surface Plasmon Enhanced Gas Sensors;Yao Yao et al.;《ACS Appl. Mater. Interfaces》;20160627;第8卷;第18165-18172页 |
| Ferroelectric WO3 Nanoparticles for Acetone Selective Detection;L. Wang et al.;《Chem. Mater.》;20080407;第20卷(第15期);第4794-4796页 |
| Highly enhanced acetone sensing performance of porous C-dopedWO3 hollow spheres by carbon spheres as templates;Jun-Yue Shen et al.;《Sensors and Actuators B》;20160812;第239卷;第597-607页 |
| Low-Temperature H2S Detection with Hierarchical Cr-Doped WO3 Microspheres;Yanrong Wang et al.;《ACS Appl. Mater. Interfaces》;20160323;第8卷;第9674-9683页 |
| Synthesis of Fe-doped WO3 nanostructures with high visible-light-driven photocatalytic activities;Hui Song et al.;《Applied Catalysis B》;20141115;第112-120页 |
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