CN114314521A - Method for controllable generation of oxygen vacancy in metal oxide - Google Patents
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 38
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 38
- 239000001301 oxygen Substances 0.000 title claims abstract description 31
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 21
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 20
- 239000010453 quartz Substances 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000002105 nanoparticle Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 5
- 239000011593 sulfur Substances 0.000 claims abstract description 5
- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 230000008569 process Effects 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims abstract description 3
- 238000002525 ultrasonication Methods 0.000 claims abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 239000008247 solid mixture Substances 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 description 7
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003574 free electron Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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Abstract
本发明公开了一种针对金属氧化物中氧空位可控生成的方法，包括以下步骤；步骤一，将金属氧化物与硫粉通过研磨混合均匀后，装入定制的石英管后，使用氢氧焰封管机将石英管抽真空并密封以隔绝空气；步骤二，分别在150℃、200℃、300℃、400℃的温度下依次煅烧一个小时，冷却至室温后，打开密封的石英管，取出粉末混合物产物；步骤三，将步骤二得到的粉末混合物产物置于一定量的三氯甲烷溶剂(50毫升)中进行超声、离心，重复三次此过程以去除多余硫单质，然后在真空条件下干燥，最终得到金属氧化物纳米颗粒。本发明通过改变硫粉含量和煅烧温度以达到精确控制金属氧化物中氧空位生成的浓度。
The invention discloses a method for the controllable generation of oxygen vacancies in metal oxides. The flame-sealing machine evacuates and seals the quartz tube to isolate the air; in step 2, calcining at 150°C, 200°C, 300°C, and 400°C for one hour respectively, and after cooling to room temperature, open the sealed quartz tube, Take out the powder mixture product; step 3, place the powder mixture product obtained in step 2 in a certain amount of chloroform solvent (50 ml) for ultrasonication and centrifugation, repeat this process three times to remove excess sulfur element, and then under vacuum conditions After drying, metal oxide nanoparticles are finally obtained. The present invention achieves precise control of the concentration of oxygen vacancies generated in the metal oxide by changing the content of sulfur powder and the calcination temperature.
Description
技术领域technical field
本发明涉及生成氧空位技术领域，特别涉及一种针对金属氧化物中氧空位可控生成的方法。The invention relates to the technical field of generating oxygen vacancies, in particular to a method for the controllable generation of oxygen vacancies in metal oxides.
背景技术Background technique
氧空位的生成会伴随着自由电子的产生，这些自由电子的存在可极大地提高金属氧化物导电性，这提升了金属氧化物在储能领域的应用潜力。另外，氧空位的存在可以降低电子和空穴的辐合几率，从而提高金属氧化物的光催化性能，使其在光催化等领域具有更广泛的应用。目前，生成氧空位的方法大多采用在还原性气氛(包括氩气、氢气、真空等)中高温煅烧(≥500℃)的后处理手段为主，此方法主要是通过煅烧温度来调控氧空位浓度，调控参数单一，且产生的氧空位浓度控制不精准。同时，高温条件还可能会导致金属氧化物纳米颗粒形貌(包括微观形貌、粒径、颗粒聚集状态等)或者晶体结构的改变而影响其性能。因此，在尽可能低的温度条件下，在不改变金属氧化物形貌和晶体结构的前提下，寻求一种精准控制氧空位浓度生成的技术迫在眉睫。The generation of oxygen vacancies is accompanied by the generation of free electrons, and the existence of these free electrons can greatly improve the conductivity of metal oxides, which enhances the application potential of metal oxides in the field of energy storage. In addition, the existence of oxygen vacancies can reduce the convergence probability of electrons and holes, thereby improving the photocatalytic properties of metal oxides, making them more widely used in photocatalysis and other fields. At present, most of the methods for generating oxygen vacancies use post-treatment methods of high temperature calcination (≥500°C) in a reducing atmosphere (including argon, hydrogen, vacuum, etc.), and this method mainly controls the oxygen vacancy concentration by calcination temperature. , the control parameters are single, and the resulting oxygen vacancy concentration is not controlled accurately. At the same time, high temperature conditions may also lead to changes in the morphology (including microscopic morphology, particle size, particle aggregation state, etc.) or crystal structure of metal oxide nanoparticles, which affects their properties. Therefore, it is urgent to seek a technology to precisely control the generation of oxygen vacancies at the lowest possible temperature without changing the morphology and crystal structure of metal oxides.
发明内容SUMMARY OF THE INVENTION
为了克服上述现有技术的不足，本发明的目的在于提供一种针对金属氧化物中氧空位可控生成的方法，基于硫单质较低的熔点和还原性，通过改变硫粉含量和煅烧温度以达到精确控制金属氧化物中氧空位生成的浓度，以解决上述背景技术中所提出的问题。In order to overcome the above-mentioned deficiencies of the prior art, the object of the present invention is to provide a method for the controllable generation of oxygen vacancies in metal oxides. Accurate control of the concentration of oxygen vacancies generated in metal oxides can be achieved to solve the problems raised in the above-mentioned background art.
为了实现上述目的，本发明采用的技术方案是：In order to achieve the above object, the technical scheme adopted in the present invention is:
一种针对金属氧化物中氧空位可控生成的方法，包括以下步骤；A method for the controllable generation of oxygen vacancies in metal oxides, comprising the following steps;
步骤一，将金属氧化物与硫粉通过研磨混合均匀后，装入定制的石英管后，使用氢氧焰封管机将石英管抽真空并密封以隔绝空气；Step 1, after the metal oxide and the sulfur powder are uniformly mixed by grinding, and then loaded into a custom-made quartz tube, the quartz tube is evacuated and sealed by a hydrogen-oxygen flame tube sealing machine to isolate the air;
步骤二，分别在150℃、200℃、300℃、400℃的温度下依次煅烧一个小时，冷却至室温后，打开密封的石英管，取出粉末混合物产物；Step 2, calcining at 150°C, 200°C, 300°C, and 400°C respectively for one hour, after cooling to room temperature, open the sealed quartz tube, and take out the powder mixture product;
步骤三，将步骤二得到的粉末混合物产物置于一定量的三氯甲烷溶剂(50毫升)中进行超声、离心，重复三次此过程以去除多余硫单质，然后在真空条件下干燥，最终得到金属氧化物纳米颗粒。In step 3, the powder mixture product obtained in step 2 is placed in a certain amount of chloroform solvent (50 ml) for ultrasonication and centrifugation, and this process is repeated three times to remove excess sulfur element, and then dried under vacuum conditions to finally obtain metal. oxide nanoparticles.
所述步骤一中金属氧化物为氧化钛(TiO2)、氧化锌(ZnO)、氧化铈(CeO2)、氧化锆(ZrO2)、氧化锡(SnO2)中的一种或其他金属氧化物。In the step 1, the metal oxide is one of titanium oxide (TiO 2 ), zinc oxide (ZnO), cerium oxide (CeO 2 ), zirconium oxide (ZrO 2 ), tin oxide (SnO 2 ) or other metal oxides thing.
所述步骤一中金属氧化物与硫粉比例为1:2(0.1g:0.2g)、1:1(0.1g:0.2g)、1:0.5(0.1g:0.05g)。In the step 1, the ratio of metal oxide to sulfur powder is 1:2 (0.1g:0.2g), 1:1 (0.1g:0.2g), 1:0.5 (0.1g:0.05g).
所述步骤一中研磨后的粒径要求为1微米以下。In the step 1, the particle size after grinding is required to be less than 1 micron.
所述石英管定制的条件为：直径1cm，总长度18cm，在10cm处收口。The conditions for customizing the quartz tube are: diameter 1 cm, total length 18 cm, and the end is closed at 10 cm.
所述步骤二得到的粉末混合物产物为未反应的硫粉(淡黄色)与部分还原的金属氧化物(灰色)的固体混合物。The powder mixture product obtained in the second step is a solid mixture of unreacted sulfur powder (light yellow) and partially reduced metal oxide (gray).
所述步骤三中粉末混合物产物在三氯甲烷溶剂中，超声10分钟，5000转离心5分钟。In the third step, the powder mixture product is in a chloroform solvent, ultrasonicated for 10 minutes, and centrifuged at 5000 rpm for 5 minutes.
所述步骤三中真空条件下60℃干燥12个小时。In the third step, drying was performed at 60° C. for 12 hours under vacuum conditions.
所述步骤三中金属氧化物纳米颗粒为颜色均一的灰色固体粉末状产物。In the third step, the metal oxide nanoparticles are gray solid powder products with uniform color.
本发明的有益效果：Beneficial effects of the present invention:
(1)本发明所制备的含有不同浓度氧空位的金属氧化物纳米颗粒表现出了其导电性能不同程度的提高，以及电子空穴辐合几率的降低，从而表现出其电化学电容性能和光催化性能的提升；(1) The metal oxide nanoparticles containing different concentrations of oxygen vacancies prepared by the present invention show different degrees of improvement in their electrical conductivity and reduction in the probability of electron-hole convergence, thereby showing their electrochemical capacitance performance and photocatalytic performance. performance improvement;
(2)本发明将氧空位引入的同时，还可能引入了硫元素相关的点缺陷，此类缺陷的引入也会对光催化性能有所影响。(2) While introducing oxygen vacancies in the present invention, point defects related to sulfur element may also be introduced, and the introduction of such defects will also affect the photocatalytic performance.
附图说明Description of drawings
图1为TiO2在300℃处理后的照片。(a)未加入硫粉；(b)加入硫粉。Figure 1 is a photograph of TiO2 after treatment at 300 °C. (a) without adding sulfur powder; (b) adding sulfur powder.
图2为TiO2在300℃热处理后的X-射线粉末衍射图谱。黑线为未加入硫粉热处理后的衍射图谱(记为TiO2)，灰线为加入硫粉后热处理含有氧空位的TiO2粉末(记为TiO2-x)的衍射图谱。Figure 2 is the X-ray powder diffraction pattern of TiO2 after heat treatment at 300°C. The black line is the diffraction pattern of heat treatment without adding sulfur powder (denoted as TiO 2 ), and the gray line is the diffraction pattern of heat-treated TiO 2 powder containing oxygen vacancies (denoted as TiO 2-x ) after adding sulfur powder.
图3为加入硫粉和为加入硫粉并通过热处理条件后所得到的TiO2纳米颗粒在可见光下对罗丹明B(RhB)的分解示意图。Figure 3 is a schematic diagram of the decomposition of rhodamine B (RhB) under visible light by adding sulfur powder and TiO 2 nanoparticles obtained after adding sulfur powder and passing through heat treatment conditions.
具体实施方式Detailed ways
下面结合附图对本发明作进一步详细说明。The present invention will be further described in detail below in conjunction with the accompanying drawings.
如图1所示：As shown in Figure 1:
将1g二氧化钛粉末与1g硫粉研磨混合10分钟，置于上述定制的石英管中并封口以隔绝空气，然后在设定温度为300℃，升温速率为10℃/min的条件下煅烧1小时，降温到室温之后，将石英管中的混合粉末在三氯甲烷中超声10分钟，然后离心5分钟，最终在60℃下真空干燥12小时得到干燥的灰色的固体粉末(如图1中右图所示的实物照片)。1g of titanium dioxide powder and 1g of sulfur powder were ground and mixed for 10 minutes, placed in the above-mentioned custom quartz tube and sealed to isolate the air, and then calcined for 1 hour at a set temperature of 300°C and a heating rate of 10°C/min, After cooling to room temperature, the mixed powder in the quartz tube was sonicated in chloroform for 10 minutes, then centrifuged for 5 minutes, and finally vacuum-dried at 60°C for 12 hours to obtain a dry gray solid powder (as shown in the right picture in Figure 1). actual photos shown).
为了对比，将2g二氧化钛粉末(不加入硫粉)装入上述定制的石英管，以同样的煅烧条件处理之后，粉末的颜色为白色，热处理并未使其颜色发生变化，仍然呈现二氧化钛本身的颜色，即白色。(如图1中左图所示的实物照片)。For comparison, 2g of titanium dioxide powder (without adding sulfur powder) was put into the above-mentioned customized quartz tube, and after being treated with the same calcination conditions, the color of the powder was white, and the heat treatment did not change its color, but still showed the color of titanium dioxide itself , which is white. (The actual photo shown on the left in Figure 1).
如图2所示：将图1中的粉末样品分别压片，并通过X-射线粉末衍射仪以确定加入硫粉之后，300℃煅烧之后的二氧化钛结构是否变化。如图所示，黑色线为未加入硫粉热处理后的衍射图谱(记为TiO2)，灰色为加入硫粉热处理后所测得的衍射图谱(记为TiO2-x)。由衍射图谱的对比结果来看，硫粉的加入并未改变TiO2的晶体结构。As shown in Fig. 2: the powder samples in Fig. 1 were pressed into tablets respectively, and X-ray powder diffractometer was used to determine whether the structure of titanium dioxide changed after calcination at 300°C after adding sulfur powder. As shown in the figure, the black line is the diffraction pattern after heat treatment without adding sulfur powder (denoted as TiO 2 ), and the gray line is the diffraction pattern after heat treatment with sulfur powder added (denoted as TiO 2-x ). From the comparison results of diffraction patterns, the addition of sulfur powder did not change the crystal structure of TiO 2 .
如图3所示：对于300℃处理后的TiO2-x样品，其RhB在可见光下的分解率为71.2％，而处理前的TiO2样品25℃在可见光下的RhB分解率为69.3％。氧空位的存在捕获电子促进光生电子和空穴分离。提高了样品光催化活性。As shown in Figure 3: for the TiO2 -x sample treated at 300 °C, the RhB decomposition rate under visible light was 71.2%, while the RhB decomposition rate of the TiO2 sample before treatment at 25 °C was 69.3% under visible light. The presence of oxygen vacancies trapping electrons facilitates the separation of photogenerated electrons and holes. The photocatalytic activity of the sample was improved.
当硫单质的含量和煅烧温度不同时，所得到最终的金属氧化物粉末呈现出不同深浅的灰色，也就是说，通过调节这两个参数，可以得到含有不同浓度氧空位的金属氧化物，并且达到控制生成氧空位浓度的目的。When the sulfur content and calcination temperature are different, the obtained final metal oxide powder presents different shades of gray, that is to say, by adjusting these two parameters, metal oxides with different concentrations of oxygen vacancies can be obtained, and To achieve the purpose of controlling the concentration of generated oxygen vacancies.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114684864A (en) * | 2022-04-15 | 2022-07-01 | 东南大学 | Preparation method and application of transition metal oxide electrode material |
| CN114774980A (en) * | 2022-05-10 | 2022-07-22 | 浙江工业大学 | A kind of catalyst containing different valence vanadium oxides formed by controlling different calcination conditions and its synthesis method and application |
| CN114774980B (en) * | 2022-05-10 | 2023-11-21 | 浙江工业大学 | Catalyst containing vanadium oxide with different valence states and synthesis method and application thereof |
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