CN105728005A - Preparation method of carbon-doped indium oxide with complex serving as precursor - Google Patents
Preparation method of carbon-doped indium oxide with complex serving as precursor Download PDFInfo
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- CN105728005A CN105728005A CN201610155909.3A CN201610155909A CN105728005A CN 105728005 A CN105728005 A CN 105728005A CN 201610155909 A CN201610155909 A CN 201610155909A CN 105728005 A CN105728005 A CN 105728005A
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- 229910003437 indium oxide Inorganic materials 0.000 title claims abstract description 36
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002243 precursor Substances 0.000 title claims abstract description 11
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 15
- -1 indium (III)-terephthalic acid Chemical compound 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 229910052738 indium Inorganic materials 0.000 abstract description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 abstract description 2
- RJMMFJHMVBOLGY-UHFFFAOYSA-N indium(3+) Chemical compound [In+3] RJMMFJHMVBOLGY-UHFFFAOYSA-N 0.000 abstract 2
- 229910052809 inorganic oxide Inorganic materials 0.000 abstract 1
- 150000003504 terephthalic acids Chemical class 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- WXNZTHHGJRFXKQ-UHFFFAOYSA-N 4-chlorophenol Chemical compound OC1=CC=C(Cl)C=C1 WXNZTHHGJRFXKQ-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910001922 gold oxide Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
本发明涉及一种碳掺杂氧化铟及其制备方法，属于无机氧化物复合材料制备技术领域。本发明以铟(III)?对苯二甲酸配合物为前驱体制备碳掺杂氧化铟。具体步骤如下：首先将硝酸铟和对苯二甲酸混合于N,N’?二甲基甲酰胺(DMF)溶液中进行加热搅拌并通过离心分离、洗涤、干燥等步骤后得到铟(III)?对苯二甲酸配合物。进一步将铟(III)?对苯二甲酸配合物在氮气保护下进行热解即可制得所述碳掺杂氧化铟材料。The invention relates to a carbon-doped indium oxide and a preparation method thereof, belonging to the technical field of preparation of inorganic oxide composite materials. The invention uses indium (III)?terephthalic acid complex as a precursor to prepare carbon-doped indium oxide. The specific steps are as follows: first, mix indium nitrate and terephthalic acid in N,N'? dimethylformamide (DMF) solution, heat and stir, and then obtain indium(III)? Terephthalic acid complexes. The carbon-doped indium oxide material can be prepared by further pyrolyzing the indium(III)?terephthalic acid complex under nitrogen protection.
Description
技术领域 technical field
本发明涉及一种以配合物为前驱体的碳掺杂氧化铟纳米颗粒及其制备方法，属于无机纳米材料制备领域。 The invention relates to a carbon-doped indium oxide nanoparticle with a complex as a precursor and a preparation method thereof, belonging to the field of inorganic nanomaterial preparation.
背景技术 Background technique
氧化铟(In2O3)是一种重要的半导体材料，在光催化及气体传感等方面都具有优异的性能和重要的应用价值。为了提高氧化铟的性能，拓展其应用领域，科学家一方面不断对氧化铟进行形貌、尺寸的调控，提高其比表面积等微观性质。另一方面不断的尝试对氧化铟进行功能化修饰，将氧化铟和铂、钯等贵金属，氧化锡等异相氧化物以及石墨烯等碳材料进行复合。G. Y. Lu等人报道了金和氧化铟的复合纳米颗粒 (RSC Advances, 2015, 5, 545-551)，通过金粒子和氧化铟之间的协同作用促进二者接触面上的电子传递作用，大大的提高了其对甲醛气体的传感作用。此外，相关研究表明将半导体氧化物和石墨烯等碳材料进行复合可以有效提高半导体氧化物的电荷分离效率，碳材料良好的导电性能可以大大降低载流子重新结合的可能性，从而提高半导体材料的光吸收性能，进一步改善其光催化效率。 Indium oxide (In 2 O 3 ) is an important semiconductor material, which has excellent performance and important application value in photocatalysis and gas sensing. In order to improve the performance of indium oxide and expand its application fields, scientists continue to control the morphology and size of indium oxide to improve its microscopic properties such as specific surface area. On the other hand, continuous attempts have been made to functionalize indium oxide by combining indium oxide with noble metals such as platinum and palladium, heterogeneous oxides such as tin oxide, and carbon materials such as graphene. GY Lu et al reported the composite nanoparticles of gold and indium oxide (RSC Advances, 2015, 5, 545-551), through the synergistic effect between gold particles and indium oxide to promote electron transfer on the interface between the two, greatly improved its sensing effect on formaldehyde gas. In addition, related studies have shown that compounding semiconductor oxides and carbon materials such as graphene can effectively improve the charge separation efficiency of semiconductor oxides. The good electrical conductivity of carbon materials can greatly reduce the possibility of carrier recombination, thereby improving the efficiency of semiconductor materials. The light absorption performance further improves its photocatalytic efficiency.
现有的基于氧化铟的复合材料的制备主要采取两步法，乃至多步法。贵金属粒子、石墨烯以及其他异相氧化物等组分往往需要提前制备，然后作为模板剂等加入到第二步制备过程中，并通过高温热解等步骤最终获得复合材料。合成过程比较复杂，需要相对较高的制备成本，而且最终产物的形貌难以控制。所以有关氧化铟基复合材料的制备方法的探索仍具有重要的意义。 The preparation of existing indium oxide-based composite materials mainly adopts a two-step method, or even a multi-step method. Components such as noble metal particles, graphene, and other heterogeneous oxides often need to be prepared in advance, and then added to the second step of the preparation process as templates, etc., and finally obtain composite materials through high temperature pyrolysis and other steps. The synthesis process is relatively complicated, requiring relatively high preparation costs, and the morphology of the final product is difficult to control. Therefore, it is still of great significance to explore the preparation methods of indium oxide-based composite materials.
发明内容 Contents of the invention
针对现有技术缺陷，为了解决碳掺杂氧化铟制备过程复杂等问题，加强对碳掺杂氧化铟的形貌控制并进一步提高其性能，本发明提供了一种以铟(III)-对苯二甲酸配合物为前驱体的碳掺杂氧化铟的制备方法。 Aiming at the defects of the existing technology, in order to solve the problems such as the complicated preparation process of carbon-doped indium oxide, strengthen the control of the morphology of carbon-doped indium oxide and further improve its performance, the present invention provides an indium (III)-p-phenylene The invention discloses a method for preparing carbon-doped indium oxide with a dicarboxylic acid complex as a precursor.
本发明的目的是通过以下技术方案实现的，一种碳掺杂氧化铟的制备方法，包括以下步骤： The purpose of the present invention is achieved through the following technical solutions, a method for preparing carbon-doped indium oxide, comprising the following steps:
1）分别配制浓度为0.05-0.25摩尔/升的硝酸铟和对苯二甲酸的N,N’-二甲基甲酰胺(DMF)溶液并将二者混合后于50-60oC下搅拌10-30分钟，经离心清洗后得到乳白色铟(III)-对苯二甲酸配合物； 1) Prepare the N,N'-dimethylformamide (DMF) solution of indium nitrate and terephthalic acid with a concentration of 0.05-0.25 mol/liter respectively, mix them and stir at 50-60 o C for 10 -30 minutes, obtain milky white indium (III)-terephthalic acid complex after centrifugal cleaning;
2）将步骤1所得铟(III)-对苯二甲酸配合物转移至坩埚中，放入氮气保护的高温管式炉中并升温至500-700oC，加热90-180分钟得到黑色粉末状产物，即为碳掺杂氧化铟。 2) Transfer the indium(III)-terephthalic acid complex obtained in step 1 to a crucible, put it into a high-temperature tube furnace protected by nitrogen gas and raise the temperature to 500-700 o C, and heat for 90-180 minutes to obtain a black powder The product is carbon-doped indium oxide.
本发明的有益效果： Beneficial effects of the present invention:
（1）本发明提供了一种新型氧化铟材料的制备方法，即以相应配合物为前驱体进行热解，本方法通过调控配合物前驱体的形貌结构控制氧化物的形貌结构，有利于制备具有新颖形貌的氧化铟； (1) The present invention provides a preparation method of a new type of indium oxide material, that is, pyrolyzing the corresponding complex as a precursor. This method controls the morphology and structure of the oxide by regulating the morphology and structure of the complex precursor, and has Facilitate the preparation of indium oxide with novel morphology;
（2）本发明制备的产物为六方管状的氧化铟，产物形貌新颖，尺寸均匀； (2) The product prepared by the present invention is hexagonal tubular indium oxide with novel appearance and uniform size;
（3）本发明制备的氧化铟具有良好的紫外可见光吸收性能； (3) The indium oxide prepared by the present invention has good ultraviolet and visible light absorption properties;
（4）本发明制备的氧化铟对4-氯苯酚表现出良好的光催化降解性能； (4) The indium oxide prepared by the present invention exhibits good photocatalytic degradation performance on 4-chlorophenol;
（5）本发明的制备仅需实验室常用的普通设备，不需专用设备，工艺过程简便易行。 (5) The preparation of the present invention only needs ordinary equipment commonly used in laboratories, and does not require special equipment, and the process is simple and easy.
附图说明 Description of drawings
图1为本发明方法所制备的铟(III)-对苯二甲酸配合物前驱体用日本电子JEOL-1400透射电子显微镜观察后拍摄的透射电镜（TEM）照片； Figure 1 is a transmission electron microscope (TEM) photo taken after observing the indium(III)-terephthalic acid complex precursor prepared by the method of the present invention with a JEOL-1400 transmission electron microscope;
图2为本发明方法所制备的碳掺杂氧化铟用日本电子JEOL-1400透射电子显微镜观察后拍摄的透射电镜（TEM）照片； Figure 2 is a transmission electron microscope (TEM) photo taken after observing the carbon-doped indium oxide prepared by the method of the present invention with a JEOL-1400 transmission electron microscope;
图3是本发明方法所制备的碳掺杂氧化铟的X射线衍射（XRD）图； Fig. 3 is an X-ray diffraction (XRD) diagram of carbon-doped indium oxide prepared by the method of the present invention;
图4是本发明方法所制备的碳掺杂氧化铟的X射线光电子能谱图； Fig. 4 is the X-ray photoelectron spectrum diagram of the carbon-doped indium oxide prepared by the method of the present invention;
图5是本发明方法所制备的碳掺杂氧化铟用日本Shimadzu UV-3101PC型紫外-可见-近红外分光光度计（UV-Vis-NIR）测试所得的紫外可见吸收光谱图。 Fig. 5 is an ultraviolet-visible absorption spectrum diagram obtained by testing the carbon-doped indium oxide prepared by the method of the present invention with a Japanese Shimadzu UV-3101PC ultraviolet-visible-near-infrared spectrophotometer (UV-Vis-NIR).
具体实施方式 detailed description
下面通过具体实施实例并结合附图对本发明的内容作进一步详细说明，但这些实施例并不限制本发明的保护范围。 The content of the present invention will be further described in detail below through specific implementation examples and in conjunction with the accompanying drawings, but these embodiments do not limit the protection scope of the present invention.
实施例Example 11
首先将浓度为0.1摩尔每升的硝酸铟和对苯二甲酸的DMF溶液混合，然后于50oC下搅拌20分钟，得到乳白色混浊液。将上述浊液在3000转/分钟条件下离心10分钟后，移去离心管中无色溶液，得到乳白色沉淀产物，即为铟(III)-对苯二甲酸配合物。将洗净干燥后的配合物前驱体转移至坩埚中并放入高温管式炉中。在氮气保护下升温至500oC并保温150分钟，自然降温至室温得到黑色粉末，即为碳掺杂氧化铟产品。 First, mix indium nitrate with a concentration of 0.1 moles per liter and a DMF solution of terephthalic acid, and then stir at 50 o C for 20 minutes to obtain a milky white turbid solution. After the above turbid solution was centrifuged at 3000 rpm for 10 minutes, the colorless solution in the centrifuge tube was removed to obtain a milky white precipitated product, which was indium(III)-terephthalic acid complex. The cleaned and dried complex precursor was transferred to a crucible and placed in a high temperature tube furnace. Under the protection of nitrogen, the temperature was raised to 500 o C and kept for 150 minutes, and the temperature was naturally cooled to room temperature to obtain a black powder, which is a carbon-doped indium oxide product.
实施例Example 22
首先将浓度为0.15摩尔每升的硝酸铟和对苯二甲酸的DMF溶液混合，然后于60oC下搅拌10分钟，得到乳白色混浊液。将上述浊液在3000转/分钟条件下离心10分钟后，移去离心管中无色溶液，得到乳白色沉淀产物，即为铟(III)-对苯二甲酸配合物。将洗净干燥后的配合物前驱体转移至坩埚中并放入高温管式炉中。在氮气保护下升温至600oC并保温90分钟，自然降温至室温得到黑色粉末，即为碳掺杂氧化铟产品。 First, mix indium nitrate with a concentration of 0.15 moles per liter and a DMF solution of terephthalic acid, and then stir at 60 o C for 10 minutes to obtain a milky white turbid solution. After the above turbid solution was centrifuged at 3000 rpm for 10 minutes, the colorless solution in the centrifuge tube was removed to obtain a milky white precipitated product, which was indium(III)-terephthalic acid complex. The cleaned and dried complex precursor was transferred to a crucible and placed in a high temperature tube furnace. Under the protection of nitrogen, the temperature was raised to 600 o C and kept for 90 minutes, and the temperature was naturally cooled to room temperature to obtain a black powder, which is a carbon-doped indium oxide product.
实施例Example 33
首先将浓度为0.2摩尔每升的硝酸铟和对苯二甲酸的DMF溶液混合，然后于50oC下搅拌20分钟，得到乳白色混浊液。将上述浊液在3000转/分钟条件下离心10分钟后，移去离心管中无色溶液，得到乳白色沉淀产物，即为铟(III)-对苯二甲酸配合物。将洗净干燥后的配合物前驱体转移至坩埚中并放入高温管式炉中。在氮气保护下升温至700oC并保温60分钟，自然降温至室温得到黑色粉末，即为碳掺杂氧化铟产品。 First, the DMF solution of indium nitrate with a concentration of 0.2 moles per liter and terephthalic acid was mixed, and then stirred at 50 o C for 20 minutes to obtain a milky white cloudy solution. After the above turbid solution was centrifuged at 3000 rpm for 10 minutes, the colorless solution in the centrifuge tube was removed to obtain a milky white precipitated product, which was indium(III)-terephthalic acid complex. The cleaned and dried complex precursor was transferred to a crucible and placed in a high temperature tube furnace. Under the protection of nitrogen, the temperature was raised to 700 o C and kept for 60 minutes, and the temperature was naturally cooled to room temperature to obtain a black powder, which is a carbon-doped indium oxide product.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108821330A (en) * | 2018-08-01 | 2018-11-16 | 济南大学 | A kind of preparation method of the indium oxide hollow pipe with hierarchical structure |
| CN109019672A (en) * | 2018-08-01 | 2018-12-18 | 济南大学 | A kind of porous oxidation indium micro-pipe preparation method with unique morphology |
| CN109205686A (en) * | 2018-11-21 | 2019-01-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Nickel oxide based on MOF/indium sesquioxide heterojunction nanometer material preparation method and product and application |
| CN110002492A (en) * | 2018-02-06 | 2019-07-12 | 中国科学院金属研究所 | A method of preparing nonmetal doping metal oxide |
| CN114733546A (en) * | 2022-03-28 | 2022-07-12 | 云南锡业集团（控股）有限责任公司研发中心 | Preparation method of nitrogen-doped carbon-loaded indium nanoparticles |
| CN114751444A (en) * | 2022-04-22 | 2022-07-15 | 齐鲁工业大学 | Porous indium oxide nanotube and synthesis method and application thereof |
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| CN108821330A (en) * | 2018-08-01 | 2018-11-16 | 济南大学 | A kind of preparation method of the indium oxide hollow pipe with hierarchical structure |
| CN109019672A (en) * | 2018-08-01 | 2018-12-18 | 济南大学 | A kind of porous oxidation indium micro-pipe preparation method with unique morphology |
| CN109205686A (en) * | 2018-11-21 | 2019-01-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Nickel oxide based on MOF/indium sesquioxide heterojunction nanometer material preparation method and product and application |
| CN114733546A (en) * | 2022-03-28 | 2022-07-12 | 云南锡业集团（控股）有限责任公司研发中心 | Preparation method of nitrogen-doped carbon-loaded indium nanoparticles |
| CN114751444A (en) * | 2022-04-22 | 2022-07-15 | 齐鲁工业大学 | Porous indium oxide nanotube and synthesis method and application thereof |
| CN114751444B (en) * | 2022-04-22 | 2023-09-19 | 齐鲁工业大学 | A porous indium oxide nanotube and its synthesis method and application |
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