CN103408064B - Method for preparing indium oxide cubes through microwave-assisted hydrothermal method - Google Patents
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- 229910003437 indium oxide Inorganic materials 0.000 title claims abstract description 57
- 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 54
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 27
- 239000002243 precursor Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- IGUXCTSQIGAGSV-UHFFFAOYSA-K indium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[In+3] IGUXCTSQIGAGSV-UHFFFAOYSA-K 0.000 claims abstract description 24
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000004202 carbamide Substances 0.000 claims abstract description 23
- 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 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000003760 magnetic stirring Methods 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 150000002484 inorganic compounds Chemical class 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 12
- 238000001354 calcination Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 7
- 230000035484 reaction time Effects 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 230000005672 electromagnetic field Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 229910021617 Indium monochloride Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 150000002471 indium Chemical class 0.000 description 1
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical compound [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 description 1
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000007144 microwave assisted synthesis reaction Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明属无机纳米材料制备技术领域，涉及纳米氧化铟立方块的制备方法，尤其涉及微波辅助水热法制备氧化铟立方块的方法。本发明先配制硝酸铟与尿素的混合溶液，然后在微波下反应再经离心洗涤生成氢氧化铟前驱物，最后经高温焙烧制得而成，所述的配制硝酸铟与尿素的混合溶液是称取硝酸铟与尿素的摩尔比为1∶1~10，加入去离子水溶解，磁力搅拌30min后成均匀无色透明溶液。利用微波辅助反应制备出形貌相对均一的氧化铟，产物为立方块纳米结构，微波反应可将时间缩短到几十分钟，并能在较短时间内达到纯相，晶型较好。本发明工艺简单，重现性好，且所用原材料均为无机化合物，价廉易得，成本较低，符合环境友好要求，便于工业化生产。
The invention belongs to the technical field of preparation of inorganic nanometer materials, and relates to a method for preparing nanometer indium oxide cubes, in particular to a method for preparing indium oxide cubes by a microwave-assisted hydrothermal method. The present invention firstly prepares the mixed solution of indium nitrate and urea, then reacts under microwave and then centrifuges and washes to generate the precursor of indium hydroxide, and finally prepares the mixed solution of indium nitrate and urea. Take the molar ratio of indium nitrate and urea as 1:1~10, add deionized water to dissolve, and stir magnetically for 30 minutes to form a uniform colorless and transparent solution. Indium oxide with relatively uniform morphology is prepared by microwave-assisted reaction, and the product is a cubic nanostructure. The microwave reaction can shorten the time to tens of minutes, and can reach a pure phase in a short period of time, and the crystal form is better. The invention has simple process and good reproducibility, and the raw materials used are all inorganic compounds, which are cheap and easy to obtain, have low cost, meet the requirement of environmental friendliness, and are convenient for industrialized production.
Description
技术领域 technical field
本发明属无机纳米材料制备技术领域，涉及纳米氧化铟（In2O3）立方块的制备，尤其涉及一种微波辅助水热法制备氧化铟立方块的方法。 The invention belongs to the technical field of preparation of inorganic nanometer materials, and relates to the preparation of nano-indium oxide (In 2 O 3 ) cubes, in particular to a method for preparing indium oxide cubes by a microwave-assisted hydrothermal method.
背景技术 Background technique
纳米氧化铟（In2O3）是一类重要的n 型半导体材料，其带隙宽度为3.6~3.75eV，具有高电导性和可见光透过率，而且氧化铟在化学、生物传感、太阳能电池、光催化、光电子和平板显示器等领域具有广泛的应用。氧化铟的制备方法主要有气相法、固相法和液相法。气相法对设备参数的要求较高，产率较低，不能用于工业大批量生产；固相法得到的纳米粒子粒度一般不太均一，其应用也受到限制。目前应用较广的是液相法，由于液相法所需温度不高，有利于大规模生产。 Nano-indium oxide (In 2 O 3 ) is an important n-type semiconductor material with a bandgap width of 3.6~3.75eV, high electrical conductivity and visible light transmittance, and indium oxide is used in chemical, biological sensing, solar energy It has a wide range of applications in the fields of batteries, photocatalysis, optoelectronics and flat panel displays. The preparation methods of indium oxide mainly include gas phase method, solid phase method and liquid phase method. The gas-phase method has high requirements on equipment parameters and low yield, so it cannot be used in industrial mass production; the particle size of nanoparticles obtained by the solid-phase method is generally not uniform, and its application is also limited. At present, the liquid phase method is widely used, because the temperature required for the liquid phase method is not high, which is conducive to large-scale production.
液相法在目前的文献报道中主要包括沉淀法和水热/溶剂热法，但都存在制备前驱液耗时较长的缺陷，比如授权公告号为CN101857263B所公开的水热法制备形貌可控纳米氧化铟的方法，将可溶性铟盐（InCl3·4H2O）与尿素,加入去离子水,在磁力搅拌下配置成均匀无色透明溶液，然后在120～140℃下保温反应12～24小时制备前驱液；再比如申请公布号为CN102826593A所公开的氧化铟（In2O3）纳米材料的制备方法，在柠檬酸和尿素作为添加剂的条件下，氯化铟在120～200℃下经水热反应6～48小时制备氢氧化铟（In(OH)3）纳米颗粒，然后进行热焙烧处理得到氧化铟（In2O3）球状纳米材料。 The liquid phase method mainly includes precipitation method and hydrothermal/solvothermal method in the current literature reports, but there is a defect that it takes a long time to prepare the precursor liquid. For example, the hydrothermal method disclosed by the authorized announcement number CN101857263B can The method of controlling nano-indium oxide is to mix soluble indium salt (InCl 3 4H 2 O) and urea, add deionized water, and configure it into a uniform colorless and transparent solution under magnetic stirring, and then keep it warm at 120-140°C for 12- Prepare the precursor solution within 24 hours; another example is the preparation method of indium oxide (In 2 O 3 ) nanomaterials disclosed in the application publication number CN102826593A. Under the condition of citric acid and urea as additives, indium chloride is heated at 120-200°C Indium hydroxide (In(OH) 3 ) nanoparticles are prepared through hydrothermal reaction for 6-48 hours, and then thermally calcined to obtain indium oxide (In 2 O 3 ) spherical nanomaterials.
微波加热是通过微波与物质相互作用而转变的。在电磁场的作用下，物质中微观粒子能产生极化。与传统的外部加热方式相比，微波加热是使加热物体本身成为发热物体，这种整体加热方式，不需要热传导的过程，因此能在短时间内达到均匀加热。微波加热是介质材料自身损耗电场能量而发热，故微波电磁场作用下的不同介质材料的热效应不一样。水分子具有极强的极性，是吸收微波的最好介质，其他很多非极性物质则在微波内不能吸收微波，故而微波具有选择性加热的特点，同时它还具有加热速度快，节能高效，易于控制，安全无害等优点，能提高反应速率，缩短反应时间，节省能源，而且，利用微波辅助合成，易于得到一维的纳米结构。 Microwave heating is transformed by the interaction of microwaves with matter. Under the action of an electromagnetic field, microscopic particles in matter can be polarized. Compared with the traditional external heating method, microwave heating makes the heating object itself a heating object. This overall heating method does not require the process of heat conduction, so it can achieve uniform heating in a short time. Microwave heating is the heating of the dielectric material itself due to the loss of electric field energy, so the thermal effects of different dielectric materials under the microwave electromagnetic field are different. Water molecules have extremely strong polarity and are the best medium for absorbing microwaves. Many other non-polar substances cannot absorb microwaves in microwaves, so microwaves have the characteristics of selective heating. At the same time, it also has fast heating speed, energy saving and high efficiency. , easy to control, safe and harmless, etc., can increase the reaction rate, shorten the reaction time, save energy, and, using microwave-assisted synthesis, it is easy to obtain a one-dimensional nanostructure.
发明内容 Contents of the invention
本发明是为了解决水热/溶剂热法制备前驱液耗时较长的技术问题，公开了一种微波辅助水热法制备氧化铟立方块的方法。 The invention aims to solve the technical problem of long time-consuming preparation of a precursor liquid by a hydrothermal/solvothermal method, and discloses a method for preparing indium oxide cubes by a microwave-assisted hydrothermal method.
本发明采用低温下经微波辅助反应制备出形貌相对均一的氧化铟（In2O3）立方块，其技术方案是配制硝酸铟与尿素的混合溶液，然后在微波下反应再经离心洗涤生成氢氧化铟（In(OH)3）前驱物，最后经高温焙烧制得而成。 The invention adopts microwave-assisted reaction at low temperature to prepare indium oxide (In 2 O 3 ) cubes with relatively uniform morphology. Indium hydroxide (In(OH) 3 ) precursor is finally made by high temperature calcination.
本发明所公开的微波辅助水热法制备氧化铟立方块的方法，所述的配制硝酸铟与尿素的混合溶液是按照硝酸铟（In(NO3）3·4.5 H2O) 与尿素的摩尔比为1:1~10，优选1:0.5～2，不包括1:2称取，加入去离子水溶解，磁力搅拌30 min后成均匀无色透明溶液。 In the method for preparing indium oxide cubes by a microwave-assisted hydrothermal method disclosed in the present invention, the mixed solution of indium nitrate and urea is prepared according to the molar ratio of indium nitrate (In(NO 3 ) 3 ·4.5 H 2 O) and urea The ratio is 1:1~10, preferably 1:0.5~2, excluding 1:2. Weigh, add deionized water to dissolve, and magnetically stir for 30 minutes to form a uniform colorless and transparent solution.
本发明的较优实施例中，所述的配制硝酸铟与尿素的混合溶液是按照硝酸铟（In(NO3）3·4.5 H2O) 与尿素的摩尔比为1:7称取，加入去离子水溶解，磁力搅拌30 min后成均匀无色透明溶液。 In a preferred embodiment of the present invention, the mixed solution of preparing indium nitrate and urea is weighed according to the molar ratio of indium nitrate (In(NO 3 ) 3 ·4.5 H 2 O) to urea is 1:7, adding Dissolved in deionized water and magnetically stirred for 30 min to form a uniform colorless and transparent solution.
本发明所公开的微波辅助水热法制备氧化铟立方块的方法，所述的在微波下反应是将上述所得的均匀无色透明溶液转移至石英容器内，放置在微波反应器中，升温至80～100℃，功率为600W～1000W加热15～120min，自然冷却，收集微波产物。 The microwave-assisted hydrothermal method disclosed in the present invention prepares indium oxide cubes. The reaction under microwave is to transfer the uniform colorless and transparent solution obtained above into a quartz container, place it in a microwave reactor, and heat up to 80～100℃, heating at 600W～1000W power for 15～120min, cooling naturally, collecting microwave products.
本发明所公开的微波辅助水热法制备氧化铟立方块的方法，所述的离心洗涤是将所述微波产物离心分离，用去离子水和无水乙醇分别洗涤三次后，在60℃空气中干燥6 h，得到氢氧化铟（In(OH)3）前驱物。 In the method for preparing indium oxide cubes by microwave-assisted hydrothermal method disclosed in the present invention, the centrifugal washing is to centrifugally separate the microwave products, wash them with deionized water and absolute ethanol three times respectively, and then wash them in 60°C air After drying for 6 h, the precursor of indium hydroxide (In(OH) 3 ) was obtained.
本发明所公开的微波辅助水热法制备氧化铟立方块的方法，所述的高温焙烧是将所得的氢氧化铟（In(OH)3）前驱物在马弗炉350～550℃空气气氛下焙烧60～120min ，即可得到淡黄色的氧化铟（In2O3）立方块。 In the method for preparing indium oxide cubes by microwave-assisted hydrothermal method disclosed in the present invention, the high-temperature calcination is to place the obtained indium hydroxide (In(OH) 3 ) precursor in an air atmosphere of 350-550°C in a muffle furnace After roasting for 60-120 minutes, light yellow indium oxide (In 2 O 3 ) cubes can be obtained.
根据微波辅助水热法制备氧化铟立方块的方法制得的氧化铟纳米立方块，长度和宽度均约为200～400 nm，厚度约为50～200 nm。 The indium oxide nanocubes prepared by the microwave-assisted hydrothermal method have a length and width of about 200-400 nm, and a thickness of about 50-200 nm.
本发明所公开的微波辅助水热法与传统的水热法相比，能较大幅度提高反应速率，缩短反应时间，节省能源。反应时间可由普通的水热反应时间几小时甚至几十小时缩短到几十分钟，并能在较短时间内达到纯相。 Compared with the traditional hydrothermal method, the microwave-assisted hydrothermal method disclosed by the invention can greatly increase the reaction rate, shorten the reaction time and save energy. The reaction time can be shortened from several hours or even tens of hours to tens of minutes for ordinary hydrothermal reaction, and the pure phase can be achieved in a short time.
本发明对微波反应时间进行调控，将反应时间调整为15min、30min、60min和120min，由实验发现微波反应15min时微波产物已经达到了纯相。 The present invention regulates the microwave reaction time, and adjusts the reaction time to 15 minutes, 30 minutes, 60 minutes and 120 minutes. It is found from experiments that the microwave product has reached the pure phase when the microwave reaction is 15 minutes.
本发明中氧化铟（In2O3）的结构由X-射线衍射仪确定，X-射线衍射图中没有其他物质的峰存在，该图谱表明，由微波辅助水热法所制备的各个时段的氧化铟（In2O3）均为纯相氧化铟（In2O3），其与标准氧化铟（In2O3）卡片（01-0929）相吻合。 The structure of indium oxide (In 2 O 3 ) in the present invention is determined by X-ray diffractometer, and there are no peaks of other substances in the X-ray diffraction diagram. Indium Oxide (In 2 O 3 ) are pure phase Indium Oxide (In 2 O 3 ), which coincides with the standard Indium Oxide (In 2 O 3 ) Card (01-0929).
场发射扫描电镜（SEM）测试表明，在室温下，由微波辅助水热法所制备的氧化铟（In2O3）长度和宽度约为200～400 nm，厚度约为50～200 nm。 Field emission scanning electron microscopy (SEM) tests show that at room temperature, the length and width of indium oxide (In 2 O 3 ) prepared by microwave-assisted hydrothermal method are about 200-400 nm, and the thickness is about 50-200 nm.
对氧化铟（In2O3）表面元素的价态进行分析，452.1 eV, 444.2 eV这两个强峰分别对应与In2O3中的In 3d3/2和In3d5/2，531.6 eV 则对应于In2O3中的O 1s,而且在主峰附近并没有其它小峰的出现，表明产物的表面并未有被氧化的现象。因此通过本方案制备出来的氧化铟（In2O3）立方块，比较稳定。 The valence state of the surface elements of indium oxide (In 2 O 3 ) was analyzed, and the two strong peaks at 452.1 eV and 444.2 eV corresponded to In 3d 3/2 and In3d 5/2 in In 2 O 3 respectively, and the peak at 531.6 eV was It corresponds to O 1s in In 2 O 3 , and there are no other small peaks around the main peak, indicating that the surface of the product has not been oxidized. Therefore, the indium oxide (In 2 O 3 ) cubes prepared by this scheme are relatively stable.
本发明所用的硝酸铟（In(NO3）3·4.5 H2O)和尿素都是分析纯，实验未做进一步提纯。 The indium nitrate (In(NO 3 ) 3 ·4.5 H 2 O) and urea used in the present invention are both analytically pure, and no further purification was performed in the experiment.
有益效果Beneficial effect
本发明使用微波辅助水热法制取氧化铟（In2O3），方法简单，反应时间可由普通的水热反应时间几小时甚至几十小时缩短到几十分钟，并能在较短时间内达到纯相，反应物晶型较好。利用简单的微波辅助反应制备出形貌相对均一的氧化铟（In2O3），形貌为立方块状纳米结构，该材料具有化学稳定性好等优点。本发明工艺简单，重现性好，且所用原材料均为无机化合物，价廉易得，成本低，符合环境友好要求，便于工业化生产。 The invention uses a microwave-assisted hydrothermal method to prepare indium oxide (In 2 O 3 ), the method is simple, and the reaction time can be shortened from several hours or even dozens of hours to tens of minutes by ordinary hydrothermal reaction time, and can reach Pure phase, the crystal form of the reactant is better. Indium oxide (In 2 O 3 ) with a relatively uniform morphology was prepared by a simple microwave-assisted reaction. The morphology is a cubic nanostructure. The material has the advantages of good chemical stability. The invention has simple process and good reproducibility, and the raw materials used are all inorganic compounds, which are cheap and easy to obtain, low in cost, meet the requirement of environmental friendliness, and are convenient for industrialized production.
附图说明 Description of drawings
图1 各时段氧化铟（In2O3）立方块的X射线衍射分析图（XRD）。 Fig. 1 X-ray diffraction analysis pattern (XRD) of indium oxide (In 2 O 3 ) cubes at different time periods.
图2 氧化铟（In2O3）立方块的扫描电镜图（SEM）。 Figure 2 Scanning electron microscope (SEM) of indium oxide (In 2 O 3 ) cubes.
图3 氧化铟（In2O3）立方块的X射线光电子能谱分析图（XPS）， Figure 3 X-ray photoelectron spectroscopy (XPS) of indium oxide (In 2 O 3 ) cubes,
其中图3a中452.1 eV, 444.2 eV这两个强峰分别对应与In2O3中的In 3d3/2和In3d5/2 ，图3b中531.6 eV 则对应于In2O3中的O 1s。 The two strong peaks at 452.1 eV and 444.2 eV in Figure 3a correspond to In 3d 3/2 and In3d 5/2 in In 2 O 3 respectively, and 531.6 eV in Figure 3b corresponds to O 1s in In 2 O 3 .
具体实施方式 Detailed ways
下面结合实施例对本发明进行详细说明，以使本领域技术人员更好地理解本发明，但本发明并不局限于以下实施例。 The present invention will be described in detail below in conjunction with the examples, so that those skilled in the art can better understand the present invention, but the present invention is not limited to the following examples.
实施例 1Example 1
一种氧化铟（In2O3）立方块的制备方法，是按照下述步骤进行： A method for preparing indium oxide (In 2 O 3 ) cubes is carried out according to the following steps:
A、称取摩尔比为1:0.5硝酸铟（In(NO3）3·4.5 H2O)与尿素，溶解在100 mL去离子水中，在磁力搅拌30 min后配置成均匀无色透明溶液； A. Weigh indium nitrate (In(NO 3 ) 3 4.5 H 2 O) and urea with a molar ratio of 1:0.5, dissolve them in 100 mL deionized water, and prepare a uniform colorless and transparent solution after magnetic stirring for 30 min;
B、将步骤A所得的溶液转移至容量为250mL的石英容器中，放置在微波反应器中，升温至80 ℃，功率为600W加热15min后，自然冷却，收集微波产物； B. Transfer the solution obtained in step A to a quartz container with a capacity of 250mL, place it in a microwave reactor, heat up to 80°C, heat it at 600W for 15min, cool it naturally, and collect the microwave product;
C、将步骤B所得的微波产物离心分离，用去离子水和无水乙醇分别洗涤三次； C, centrifuging the microwave product obtained in step B, washing with deionized water and absolute ethanol three times respectively;
D、将步骤C所得离心分离后的产物在60℃空气中干燥6 h，得到氢氧化铟（In(OH)3）前驱物； D. Dry the centrifuged product obtained in step C in air at 60°C for 6 h to obtain an indium hydroxide (In(OH) 3 ) precursor;
E、将步骤D所得的氢氧化铟（In(OH)3）前驱物在马弗炉350 ℃空气气氛下煅烧60min ，即可得到淡黄色的氧化铟（In2O3）立方块。 E. Calcining the indium hydroxide (In(OH) 3 ) precursor obtained in step D in an air atmosphere at 350°C in a muffle furnace for 60 minutes to obtain pale yellow indium oxide (In 2 O 3 ) cubes.
氧化铟（In2O3）纳米立方块的XRD图谱见附图1，产物形貌分析见附图2，X射线光电子能谱分析图见附图3。 The XRD pattern of indium oxide (In 2 O 3 ) nanocubes is shown in attached drawing 1, the product morphology analysis is shown in attached drawing 2, and the X-ray photoelectron spectroscopy analysis chart is shown in attached drawing 3.
附图1中各时段的衍射峰的位置和相对强度均与JCPDS（粉末衍射标准联合委员会）卡片(01-0929)相吻合，且XRD图谱中没有其它衍射杂峰，说明本发明制备出的In2O3物相是纯的。 The positions and relative intensities of the diffraction peaks in each period in accompanying drawing 1 are all consistent with the JCPDS (Joint Committee on Powder Diffraction Standards) card (01-0929), and there are no other diffraction peaks in the XRD spectrum, indicating that the prepared In The 2 O 3 phase is pure.
附图2中，场发射扫描电镜（SEM）测试表明，在室温下，由微波辅助水热法所制备的氧化铟（In2O3）长度和宽度均约为200～400 nm，厚度约为50～200 nm。 In Figure 2, the field emission scanning electron microscope (SEM) test shows that at room temperature, the length and width of indium oxide (In 2 O 3 ) prepared by the microwave-assisted hydrothermal method are about 200-400 nm, and the thickness is about 50-200nm.
附图3中，由微波辅助水热法制备的形貌相对均一的氧化铟（In2O3），对其产物表面的元素的价态进行了分析，附图3a中，452.1 eV, 444.2 eV这两个强峰分别对应与In2O3中的In 3d3/2和In3d5/2，附图3b中，531.6 eV 则对应于In2O3中的O 1s,而且在主峰附近并没有其它小峰的出现，表明产物的表面并未有被氧化的现象。因此通过本方法制备出来的氧化铟（In2O3）立方块，比较稳定。 In Figure 3, indium oxide (In 2 O 3 ) with relatively uniform morphology prepared by microwave-assisted hydrothermal method, the valence state of the elements on the surface of the product was analyzed, in Figure 3a, 452.1 eV, 444.2 eV These two strong peaks correspond to In 3d 3/2 and In3d 5/2 in In 2 O 3 respectively. In Figure 3b, 531.6 eV corresponds to O 1s in In 2 O 3 , and there is no The appearance of other small peaks indicates that the surface of the product is not oxidized. Therefore, the indium oxide (In 2 O 3 ) cubes prepared by this method are relatively stable.
实施例 2Example 2
一种氧化铟（In2O3）立方块的制备方法，是按照下述步骤进行： A method for preparing indium oxide (In 2 O 3 ) cubes is carried out according to the following steps:
A、称取摩尔比为1:7硝酸铟（In(NO3）3·4.5 H2O)与尿素，溶解在100 mL去离子水中，在磁力搅拌30 min后配置成均匀无色透明溶液； A. Weigh indium nitrate (In(NO 3 ) 3 4.5 H 2 O) and urea with a molar ratio of 1:7, dissolve them in 100 mL deionized water, and prepare a uniform colorless and transparent solution after magnetic stirring for 30 min;
B、将步骤A所得的溶液转移至容量为250mL的石英容器中，放置在微波反应器中，升温至100 ℃，功率为1000W加热120min后，自然冷却，收集微波产物； B. Transfer the solution obtained in step A to a quartz container with a capacity of 250mL, place it in a microwave reactor, heat up to 100°C, heat it for 120min with a power of 1000W, cool it naturally, and collect the microwave product;
C、将步骤B所得的微波产物离心分离，用去离子水和无水乙醇分别洗涤三次； C, centrifuging the microwave product obtained in step B, washing with deionized water and absolute ethanol three times respectively;
D、将步骤C所得离心分离后的产物在60℃空气中干燥6 h，得到氢氧化铟（In(OH)3）前驱物； D. Dry the centrifuged product obtained in step C in air at 60°C for 6 h to obtain an indium hydroxide (In(OH) 3 ) precursor;
E、将步骤D所得的氢氧化铟（In(OH)3）前驱物在马弗炉550 ℃空气气氛下煅烧120min ，即可得到淡黄色的氧化铟（In2O3）立方块。 E. Calcining the indium hydroxide (In(OH) 3 ) precursor obtained in step D in an air atmosphere at 550°C in a muffle furnace for 120 min to obtain pale yellow indium oxide (In 2 O 3 ) cubes.
实施例 3Example 3
一种氧化铟（In2O3）立方块的制备方法，是按照下述步骤进行： A method for preparing indium oxide (In 2 O 3 ) cubes is carried out according to the following steps:
A、称取摩尔比为1:0.9硝酸铟（In(NO3）3·4.5 H2O)与尿素，溶解在100 mL去离子水中，在磁力搅拌30 min后配置成均匀无色透明溶液； A. Weigh indium nitrate (In(NO 3 ) 3 4.5 H 2 O) and urea with a molar ratio of 1:0.9, dissolve them in 100 mL deionized water, and make a uniform colorless and transparent solution after magnetic stirring for 30 min;
B、将步骤A所得的溶液转移至容量为250mL的石英容器中，放置在微波反应器中，升温至90 ℃，功率为800W加热90min后，自然冷却，收集微波产物； B. Transfer the solution obtained in step A to a quartz container with a capacity of 250mL, place it in a microwave reactor, heat up to 90°C, and heat it for 90min at a power of 800W, then cool naturally and collect the microwave product;
C、将步骤B所得的微波产物离心分离，用去离子水和无水乙醇分别洗涤三次； C, centrifuging the microwave product obtained in step B, washing with deionized water and absolute ethanol three times respectively;
D、将步骤C所得离心分离后的产物在60℃空气中干燥6 h，得到氢氧化铟（In(OH)3）前驱物； D. Dry the centrifuged product obtained in step C in air at 60°C for 6 h to obtain an indium hydroxide (In(OH) 3 ) precursor;
E、将步骤D所得的氢氧化铟（In(OH)3）前驱物在马弗炉400 ℃空气气氛下煅烧90min ，即可得到淡黄色的氧化铟（In2O3）立方块。 E. Calcining the indium hydroxide (In(OH) 3 ) precursor obtained in step D in an air atmosphere at 400°C in a muffle furnace for 90 minutes to obtain pale yellow indium oxide (In 2 O 3 ) cubes.
实施例 4Example 4
一种氧化铟（In2O3）立方块的制备方法，是按照下述步骤进行： A method for preparing indium oxide (In 2 O 3 ) cubes is carried out according to the following steps:
A、称取摩尔比为1:7硝酸铟（In(NO3）3·4.5 H2O)与尿素，溶解在100 mL去离子水中，在磁力搅拌30 min后配置成均匀无色透明溶液； A. Weigh indium nitrate (In(NO 3 ) 3 4.5 H 2 O) and urea with a molar ratio of 1:7, dissolve them in 100 mL deionized water, and prepare a uniform colorless and transparent solution after magnetic stirring for 30 min;
B、将步骤A所得的溶液转移至容量为250mL的石英容器中，放置在微波反应器中，升温至100 ℃，功率为600W加热120min后，自然冷却，收集微波产物； B. Transfer the solution obtained in step A to a quartz container with a capacity of 250mL, place it in a microwave reactor, raise the temperature to 100°C, and heat it for 120min with a power of 600W, then cool naturally, and collect the microwave product;
C、将步骤B所得的微波产物离心分离，用去离子水和无水乙醇分别洗涤三次； C, centrifuging the microwave product obtained in step B, washing with deionized water and absolute ethanol three times respectively;
D、将步骤C所得离心分离后的产物在60℃空气中干燥6 h，得到氢氧化铟（In(OH)3）前驱物； D. Dry the centrifuged product obtained in step C in air at 60°C for 6 h to obtain an indium hydroxide (In(OH) 3 ) precursor;
E、将步骤D所得的氢氧化铟（In(OH)3）前驱物在马弗炉550 ℃空气气氛下煅烧120min ，即可得到淡黄色的氧化铟（In2O3）立方块。 E. Calcining the indium hydroxide (In(OH) 3 ) precursor obtained in step D in an air atmosphere at 550°C in a muffle furnace for 120 min to obtain pale yellow indium oxide (In 2 O 3 ) cubes.
实施例 5Example 5
一种氧化铟（In2O3）立方块的制备方法，是按照下述步骤进行： A method for preparing indium oxide (In 2 O 3 ) cubes is carried out according to the following steps:
A、称取摩尔比为1:0.5硝酸铟（In(NO3）3·4.5 H2O)与尿素，溶解在100 mL去离子水中，在磁力搅拌30 min后配置成均匀无色透明溶液； A. Weigh indium nitrate (In(NO 3 ) 3 4.5 H 2 O) and urea with a molar ratio of 1:0.5, dissolve them in 100 mL deionized water, and prepare a uniform colorless and transparent solution after magnetic stirring for 30 min;
B、将步骤A所得的溶液转移至容量为250mL的石英容器中，放置在微波反应器中，升温至80 ℃，功率为600W加热120min后，自然冷却，收集微波产物； B. Transfer the solution obtained in step A to a quartz container with a capacity of 250mL, place it in a microwave reactor, raise the temperature to 80°C, and heat it for 120min with a power of 600W, then cool it naturally and collect the microwave product;
C、将步骤B所得的微波产物离心分离，用去离子水和无水乙醇分别洗涤三次； C, centrifuging the microwave product obtained in step B, washing with deionized water and absolute ethanol three times respectively;
D、将步骤C所得离心分离后的产物在60℃空气中干燥6 h，得到氢氧化铟（In(OH)3）前驱物； D. Dry the centrifuged product obtained in step C in air at 60°C for 6 h to obtain an indium hydroxide (In(OH) 3 ) precursor;
E、将步骤D所得的氢氧化铟（In(OH)3）前驱物在马弗炉550 ℃空气气氛下煅烧120min ，即可得到淡黄色的氧化铟（In2O3）立方块。 E. Calcining the indium hydroxide (In(OH) 3 ) precursor obtained in step D in an air atmosphere at 550°C in a muffle furnace for 120 min to obtain pale yellow indium oxide (In 2 O 3 ) cubes.
实施例 6Example 6
一种氧化铟（In2O3）立方块的制备方法，是按照下述步骤进行： A method for preparing indium oxide (In 2 O 3 ) cubes is carried out according to the following steps:
A、称取摩尔比为1:4硝酸铟（In(NO3）3·4.5 H2O)与尿素，溶解在100 mL去离子水中，在磁力搅拌30 min后配置成均匀无色透明溶液； A. Weigh indium nitrate (In(NO 3 ) 3 4.5 H 2 O) and urea with a molar ratio of 1:4, dissolve them in 100 mL deionized water, and prepare a uniform colorless and transparent solution after magnetic stirring for 30 min;
B、将步骤A所得的溶液转移至容量为250mL的石英容器中，放置在微波反应器中，升温至100 ℃，功率为800W加热120min后，自然冷却，收集微波产物； B. Transfer the solution obtained in step A to a quartz container with a capacity of 250mL, place it in a microwave reactor, raise the temperature to 100°C, and heat it for 120min with a power of 800W, then cool it naturally and collect the microwave product;
C、将步骤B所得的微波产物离心分离，用去离子水和无水乙醇分别洗涤三次； C, centrifuging the microwave product obtained in step B, washing with deionized water and absolute ethanol three times respectively;
D、将步骤C所得离心分离后的产物在60℃空气中干燥6 h，得到氢氧化铟（In(OH)3）前驱物； D. Dry the centrifuged product obtained in step C in air at 60°C for 6 h to obtain an indium hydroxide (In(OH) 3 ) precursor;
E、将步骤D所得的氢氧化铟（In(OH)3）前驱物在马弗炉400 ℃空气气氛下煅烧100min ，即可得到淡黄色的氧化铟（In2O3）立方块。 E. Calcining the indium hydroxide (In(OH) 3 ) precursor obtained in step D in an air atmosphere at 400°C in a muffle furnace for 100 min to obtain pale yellow indium oxide (In 2 O 3 ) cubes.
实施例7Example 7
一种氧化铟（In2O3）立方块的制备方法，是按照下述步骤进行： A method for preparing indium oxide (In 2 O 3 ) cubes is carried out according to the following steps:
A、称取摩尔比为1:1的硝酸铟（In(NO3）3·4.5 H2O)与尿素，溶解在100 mL去离子水中，在磁力搅拌30 min后配置成均匀无色透明溶液； A. Weigh indium nitrate (In(NO 3 ) 3 4.5 H 2 O) and urea with a molar ratio of 1:1, dissolve in 100 mL of deionized water, and make a uniform colorless and transparent solution after magnetic stirring for 30 min ;
B、将步骤A所得的溶液转移至容量为250mL的石英的容器中，放置在微波反应器中，升温至80 ℃，功率为600W 加温60min后，自然冷却，收集微波产物； B. Transfer the solution obtained in step A to a quartz container with a capacity of 250mL, place it in a microwave reactor, heat up to 80°C, and heat it for 60min with a power of 600W, then cool naturally, and collect the microwave product;
C、将步骤B所得的微波产物离心分离，用去离子水和无水乙醇分别洗涤三次； C, centrifuging the microwave product obtained in step B, washing with deionized water and absolute ethanol three times respectively;
D、将步骤C所得离心分离后的产物在60℃空气中干燥6 h，得到氢氧化铟前驱液； D, drying the centrifuged product obtained in step C in air at 60° C. for 6 h to obtain an indium hydroxide precursor;
E、将步骤D所得的氢氧化铟前驱液在马弗炉350 ℃空气气氛下煅烧60min ，即可得到淡黄色的氧化铟（In2O3）立方块。 E. Calcining the indium hydroxide precursor solution obtained in step D in an air atmosphere at 350°C in a muffle furnace for 60 minutes to obtain pale yellow indium oxide (In 2 O 3 ) cubes.
实施例8Example 8
一种氧化铟（In2O3）立方块的制备方法，是按照下述步骤进行： A method for preparing indium oxide (In 2 O 3 ) cubes is carried out according to the following steps:
A、称取摩尔比为1:10的硝酸铟（In(NO3）3·4.5 H2O)与尿素，溶解在100 mL去离子水中，在磁力搅拌30 min后配置成均匀无色透明溶液； A. Weigh indium nitrate (In(NO 3 ) 3 4.5 H 2 O) and urea with a molar ratio of 1:10, dissolve in 100 mL of deionized water, and make a uniform colorless and transparent solution after magnetic stirring for 30 min ;
B、将步骤A所得的溶液转移至容量为250mL的石英的容器中，放置在微波反应器中，升温至100 ℃，功率为1000W 加温240min后，自然冷却，收集微波产物； B. Transfer the solution obtained in step A to a quartz container with a capacity of 250mL, place it in a microwave reactor, raise the temperature to 100°C, and heat it for 240min with a power of 1000W, then cool naturally and collect the microwave product;
C、将步骤B所得的微波产物离心分离，用去离子水和无水乙醇分别洗涤三次； C, centrifuging the microwave product obtained in step B, washing with deionized water and absolute ethanol three times respectively;
D、将步骤C所得离心分离后的产物在60℃空气中干燥6 h，得到氢氧化铟前驱液； D, drying the centrifuged product obtained in step C in air at 60° C. for 6 h to obtain an indium hydroxide precursor;
E、将步骤D所得的氢氧化铟前驱液在马弗炉550 ℃空气气氛下煅烧240min ，即可得到淡黄色的氧化铟（In2O3）立方块。 E. Calcining the indium hydroxide precursor solution obtained in step D in a muffle furnace at 550 °C in an air atmosphere for 240 min to obtain pale yellow indium oxide (In 2 O 3 ) cubes.
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。 The above is only an embodiment of the present invention, and does not limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made by the description of the present invention, or directly or indirectly used in other related technical fields, shall be the same as The theory is included in the patent protection scope of the present invention.
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|---|
| "Thermal Decomposition of Indium(III) Hydroxide Prepared by the Microwave-Assisted Hydrothermal Method";Nobuyoshi Koga et al.;《J. Am. Ceram. Soc.》;20081231;第91卷;第4052-4058页 * |
| 微波水解法制备In2O3纳米颗粒及气敏性能研究;徐甲强等;《电子元件与材料》;20060630;第25卷(第6期);第33-35页 * |
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