CN108993539B - Method for improving indium sulfide photocatalysis - Google Patents
Method for improving indium sulfide photocatalysis Download PDFInfo
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- GKCNVZWZCYIBPR-UHFFFAOYSA-N sulfanylideneindium Chemical compound [In]=S GKCNVZWZCYIBPR-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 43
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 11
- 238000007146 photocatalysis Methods 0.000 title description 4
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 47
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 60
- 239000000243 solution Substances 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- ZOMNDSJRWSNDFL-UHFFFAOYSA-N sulfanylidene(sulfanylideneindiganylsulfanyl)indigane Chemical compound S=[In]S[In]=S ZOMNDSJRWSNDFL-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 22
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 17
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 17
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000725 suspension Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 13
- 239000004570 mortar (masonry) Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 238000005485 electric heating Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 230000002194 synthesizing effect Effects 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000011534 incubation Methods 0.000 claims 2
- 230000015556 catabolic process Effects 0.000 description 24
- 238000006731 degradation reaction Methods 0.000 description 24
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 21
- 229940012189 methyl orange Drugs 0.000 description 21
- 239000011941 photocatalyst Substances 0.000 description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910001449 indium ion Inorganic materials 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- -1 sulfur ions Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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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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- C02F2101/34—Organic compounds containing oxygen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention relates to a method for improving the photocatalytic efficiency of indium sulfide, which comprises the step of carrying out hydrothermal treatment on indium sulfide after the indium sulfide is synthesized, wherein the hydrothermal treatment time is 4-24 hours. The photocatalytic efficiency of the indium sulfide subjected to hydrothermal treatment is remarkably improved.
Description
Technical Field
The invention relates to the field of photocatalysis, in particular to a method for improving indium sulfide photocatalysis.
Background
With the progress of science and technology and the improvement of the living standard of human beings, the problems of energy shortage and environmental pollution are more and more prominent. The semiconductor photocatalyst can utilize solar energy to catalyze and degrade waste water, thereby gaining attention of all social circles. beta-In2S3Is an n-type semiconductor and has the characteristics of high carrier mobility, low toxicity and high stability. In2S3The forbidden band width of the photocatalyst is about 1.9-2.2eV, and the photocatalyst is an excellent visible light photocatalyst. In2S3The nano particles have important application value in the aspects of photocatalytic degradation of organic dyes and photocatalytic dissociation of water to produce hydrogen under the conditions of solar fuel cells and visible light.
Disclosure of Invention
The invention aims to provide a method for improving the photocatalytic efficiency of indium sulfide, which comprises the step of carrying out hydrothermal treatment on indium sulfide after the indium sulfide is synthesized, wherein the hydrothermal treatment time is 4-24 hours.
Further, after hydrothermal treatment for 4-24 hours, the degradation rate of indium sulfide serving as a photocatalyst for photocatalytic degradation of 50ml of 10mg/L methyl orange solution under visible light of a 350W xenon lamp is over 84%, further over 90%, and further over 93%
Further, the time of the hydrothermal treatment is 4 hours or 16-24 hours;
further, the time of the hydrothermal treatment is 4 hours, 8 hours, 12 hours, 16 hours, 20 hours, or 24 hours.
Further, the method for synthesizing indium sulfide comprises the following steps: dropwise adding the indium chloride solution into the citric acid aqueous solution, wherein the solvent is deionized water, stirring is required in the dropwise adding process, and stirring is performed under constant magnetic force after dropwise adding; then dropwise adding a sodium sulfide solution into a solution system of indium chloride and citric acid, and magnetically stirring to obtain a yellow suspension; then, the product was centrifuged, washed repeatedly with absolute ethanol and deionized water, vacuum dried, and ground to obtain orange-colored indium sulfide powder particles.
Further, the method for synthesizing indium sulfide comprises the following steps: dropwise adding the indium chloride solution into the citric acid aqueous solution, wherein the solvent is deionized water, stirring is required in the dropwise adding process, and stirring is carried out for 2 hours under constant magnetic stirring after dropwise adding; then dropwise adding a sodium sulfide solution into a solution system of indium chloride and citric acid, and magnetically stirring for 1 hour to obtain a yellow suspension; then, centrifuging the product, repeatedly washing the product for 4-5 times by using absolute ethyl alcohol and deionized water, drying the product in a vacuum drying oven at the temperature of 60 ℃, and finally grinding the product by using a mortar to obtain orange indium sulfide powder particles.
Further, the volume ratio of the indium chloride solution to the citric acid aqueous solution to the sodium sulfide solution is 1: 2: 1.
further, the concentration ratio of the indium chloride solution to the citric acid aqueous solution to the sodium sulfide solution is 1: (0.1-0.15): 2, further 14: 1.9: 28.
further, the hydrothermal treatment process comprises the following steps: weighing indium sulfide powder, dispersing the indium sulfide powder in deionized water, carrying out ultrasonic treatment, transferring the uniform suspension liquid into a high-pressure reaction kettle, placing the high-pressure reaction kettle in an electric heating forced air drying oven, and keeping the temperature at constant temperature; and after the reaction is finished, naturally cooling to room temperature, centrifugally separating the product, washing the product with absolute ethyl alcohol and deionized water respectively, finally drying in vacuum, and grinding to obtain the hydrothermally treated indium sulfide powder.
In the synthesis method of the indium sulfide, the sodium sulfide solution is dropwise added into a solution system of indium chloride and citric acid and stirred, the reaction is more sufficient and uniform through dropwise addition and stirring, and the dropwise addition sequence is more favorable for the sulfur ions in the sodium sulfide to be fully combined with the indium ions to form the indium sulfide.
Further, the hydrothermal treatment process comprises the following steps: weighing 500 mg of indium sulfide powder, dispersing the indium sulfide powder in 40ml of deionized water, carrying out ultrasonic treatment for 1 hour, transferring the uniform suspension into a 100ml high-pressure reaction kettle, placing the reaction kettle in an electric heating blowing drying box, carrying out heat preservation for 4-24 hours at a constant temperature of 140 ℃, and further carrying out heat preservation for 4 hours or 16-24 hours; and after the reaction is finished, naturally cooling to room temperature, washing the product after centrifugal separation three times by using absolute ethyl alcohol and deionized water respectively, finally drying in a vacuum drying oven at 60 ℃ for 8 hours, and grinding by using a mortar to obtain the indium sulfide powder after hydrothermal treatment.
Further, the method comprises the steps of: dropwise adding 25ml of indium chloride solution with the concentration of 0.112mol/L into 50ml of citric acid aqueous solution with the concentration of 15.2mmol/L, wherein the solvent is deionized water, stirring is required in the dropwise adding process, and stirring is carried out for two hours under constant magnetic stirring after dropwise adding; then 25ml of sodium sulfide solution with the concentration of 0.224mol/L is dropwise added into a solution system of indium chloride and citric acid, and the mixture is magnetically stirred for one hour to obtain yellow suspension; then centrifuging the product, repeatedly washing the product for 4-5 times by using absolute ethyl alcohol and deionized water, drying the product in a vacuum drying oven at the temperature of 60 ℃, and finally grinding the product by using a mortar to obtain orange indium sulfide powder particles; weighing 500 mg of indium sulfide powder, dispersing the indium sulfide powder in 40ml of deionized water, carrying out ultrasonic treatment for 1 hour, transferring the uniform suspension into a 100ml high-pressure reaction kettle, placing the reaction kettle in an electric heating blowing dry box, carrying out heat preservation for 4-24 hours at a constant temperature of 140 ℃, and further carrying out heat preservation for 4 hours or 16-24 hours; and after the reaction is finished, naturally cooling to room temperature, washing the product after centrifugal separation three times by using absolute ethyl alcohol and deionized water respectively, finally drying in a vacuum drying oven at 60 ℃ for 8 hours, and grinding by using a mortar to obtain the indium sulfide powder after hydrothermal treatment.
Compared with the prior art, the synthesis method of indium sulfide is simple, is more beneficial to manual operation, has good repeatability, does not use strong acid such as nitric acid and the like in the synthesis process, and is safer in the experimental process; the indium sulfide prepared by the method can obviously improve the photocatalytic efficiency of the indium sulfide after hydrothermal treatment according to the method, and has good repeatability.
Drawings
FIGS. 1-6 are graphs showing the photo-degradation of methyl orange by indium sulfide after hydrothermal treatment for 4-24 hours in example 2, wherein C represents the concentration of methyl orange at a certain time point, C0Represents the concentration of methyl orange before reaching the adsorption-desorption equilibrium, Blank represents Blank group, In2S3The indium sulfide groups which are not hydrothermally treated are shown, and the indium sulfide groups which are hydrothermally treated at the time are shown in 4h, 8h, 12h, 16h, 20h and 24h respectively, wherein:
FIG. 1 is a graph showing the degradation rate of methyl orange by indium sulfide after 4 hours of hydrothermal treatment in example 2; the three curves are a blank group, indium sulfide which is not subjected to hydrothermal treatment and degradation rate of the indium sulfide to methyl orange after hydrothermal treatment for 4 hours from top to bottom in sequence.
FIG. 2 is a graph showing the degradation rate of methyl orange by indium sulfide after 8 hours of hydrothermal treatment in example 2; the three curves are a blank group, indium sulfide which is not subjected to hydrothermal treatment and degradation rate of the indium sulfide to methyl orange after hydrothermal treatment for 8 hours from top to bottom in sequence.
FIG. 3 is the degradation rate of indium sulfide on methyl orange after 12 hours of hydrothermal treatment in example 2; the three curves are a blank group, indium sulfide which is not subjected to hydrothermal treatment and degradation rate of the indium sulfide to methyl orange after hydrothermal treatment for 12 hours from top to bottom in sequence.
FIG. 4 is a graph showing the degradation rate of methyl orange by indium sulfide after 16 hours of hydrothermal treatment in example 2; the three curves are a blank group, indium sulfide which is not subjected to hydrothermal treatment and degradation rate of the indium sulfide to methyl orange after hydrothermal treatment for 16 hours from top to bottom in sequence.
FIG. 5 is the degradation rate of indium sulfide on methyl orange after 20 hours of hydrothermal treatment in example 2; the three curves are a blank group, indium sulfide which is not subjected to hydrothermal treatment and degradation rate of the indium sulfide to methyl orange after hydrothermal treatment for 20 hours from top to bottom in sequence.
FIG. 6 is the degradation rate of indium sulfide on methyl orange after 24 hours of hydrothermal treatment in example 2; the three curves are a blank group, indium sulfide which is not subjected to hydrothermal treatment and degradation rate of the indium sulfide to methyl orange 24 hours after the hydrothermal treatment from top to bottom in sequence.
Detailed Description
The invention is further illustrated below with reference to specific examples. It should be understood that the examples given herein are for illustrative purposes only and are not intended to limit the scope of the present invention.
The experimental procedures, in which specific conditions are not noted in the examples below, are generally carried out under conventional conditions or under conditions recommended by the manufacturers. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art.
In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only.
EXAMPLE 1 preparation of indium sulfide powder particles
Dropwise adding 25ml of indium chloride solution with the concentration of 0.112mol/L into 50ml of citric acid aqueous solution with the concentration of 15.2mmol/L, wherein the solvent is deionized water, stirring is required in the dropwise adding process, and stirring is carried out for two hours under constant magnetic stirring after dropwise adding; then 25ml of sodium sulfide solution with the concentration of 0.224mol/L is added dropwise into the solution system of indium chloride and citric acid, and the mixture is stirred magnetically for a while to obtain yellow suspension. And then centrifuging the product, repeatedly washing the product for 4-5 times by using absolute ethyl alcohol and deionized water, drying the product in a vacuum drying oven at the temperature of 60 ℃, and finally grinding the product by using a mortar to obtain orange indium sulfide powder particles.
Example 2 hydrothermal treatment of indium sulfide
500 mg of indium sulfide powder (prepared in example 1) was weighed and dispersed in 40ml of deionized water, followed by sonication for 1 hour, and the uniform suspension was transferred to a 100ml autoclave, which was placed in an electrothermal forced air drying oven and kept at a constant temperature of 140 ℃ for 4 to 24 hours (4, 8, 12, 16, 20, 24 hours), respectively. And after the reaction is finished, naturally cooling to room temperature, centrifugally separating the product, washing the product with absolute ethyl alcohol and deionized water for three times respectively, finally drying the product in a vacuum drying oven at the temperature of 60 ℃ for 8 hours, and grinding the product by using a mortar to obtain the indium sulfide powder after hydrothermal treatment.
The result of the photocatalytic experiment is as follows: indium sulfide which is not treated and is subjected to respective hydrothermal treatment for 4-24 hours is respectively used as a photocatalyst, 50ml of 10mg/L methyl orange solution is subjected to photocatalytic degradation under visible light illumination of a 350W xenon lamp for measurement, and the results after 50min degradation are shown in FIGS. 1-6 and Table 1.
TABLE 1 degradation rate of methyl orange by indium sulfide after hydrothermal treatment
The result shows that after 50min of degradation, the degradation rate of the indium sulfide on the methyl orange without hydrothermal treatment is only 10%, the degradation rate of the indium sulfide on the methyl orange after hydrothermal treatment for 4-24 hours is over 84%, and when the hydrothermal treatment time is 4 hours, the degradation rate of the indium sulfide on the methyl orange can reach 93.3%; in addition, the degradation time is prolonged to 2 hours, and the degradation rate of indium sulfide (subjected to hydrothermal treatment for 4 hours, 8 hours, 12 hours, 16 hours, 20 hours and 24 hours respectively) on methyl orange can reach 97%.
In addition, the present inventors tried to test the degradation effect of indium sulfide prepared by other methods (for example, the method shown below) on methyl orange under the same conditions as in example 2, and as a result, found that indium sulfide prepared by other methods could not achieve the excellent catalytic efficiency of the present invention, and could not achieve the degradation effect of the present invention even if the degradation time was extended to 3 hours.
Other methods
0.69 parts of In (NO)3)3·4.5H2O and 1.0 part of Na2S·9H2Adding 40 parts of deionized water respectively to prepare an indium nitrate aqueous solution and a sodium sulfide aqueous solution, adding the sodium sulfide aqueous solution into the indium nitrate aqueous solution under stirring, and controlling the adding speed to ensure that uniform sol is formed; then, adding 0.25 part of 1mol/L nitric acid solution, and adjusting the pH value of the sol to about 1-3; finally, the acid sol is filled into a reaction kettle, the filling degree of the reaction kettle is 80 percent, and the reaction lasts for 16 hours, 20 hours and 24 hours at 180 ℃; and after the reaction kettle is naturally cooled to room temperature, filtering the product, washing the product by using deionized water and alcohol, and drying the product in vacuum at the temperature of 55 ℃ to obtain 0.3 part of the indium sulfide photocatalyst.
It is to be understood that the invention described herein is not limited to particular methodologies, protocols, or reagents, as these may vary. The discussion and examples provided herein are presented solely for the purpose of describing particular embodiments and are not intended to limit the scope of the present invention, which is defined solely by the claims.
Claims (11)
1. A method for improving indium sulfide photocatalytic efficiency comprises the steps of carrying out hydrothermal treatment on orange indium sulfide powder particles after synthesizing the indium sulfide powder particles, wherein the hydrothermal treatment time is 4-24 hours;
the method for synthesizing indium sulfide comprises the following steps: dropwise adding an indium chloride solution into a citric acid aqueous solution, wherein the solvent is deionized water, stirring is required in the dropwise adding process, and stirring is performed under constant magnetic force after dropwise adding; then dropwise adding a sodium sulfide solution into a solution system of indium chloride and citric acid, and magnetically stirring to obtain a yellow suspension; and then, centrifuging the product, repeatedly washing the product with absolute ethyl alcohol and deionized water, drying the product in vacuum, and grinding the product to obtain orange indium sulfide powder particles.
2. The method according to claim 1, characterized in that the time of the hydrothermal treatment is 4 hours or 16-24 hours.
3. The method of claim 1, wherein the method of synthesizing indium sulfide comprises the steps of: dropwise adding an indium chloride solution into a citric acid aqueous solution, wherein the solvent is deionized water, stirring is required in the dropwise adding process, and stirring is carried out for 2 hours under constant magnetic stirring after dropwise adding; then dropwise adding a sodium sulfide solution into a solution system of indium chloride and citric acid, and magnetically stirring for 1 hour to obtain a yellow suspension; and then centrifuging the product, repeatedly washing the product for 4-5 times by using absolute ethyl alcohol and deionized water, drying the product in a vacuum drying oven at the temperature of 60 ℃, and finally grinding the product by using a mortar to obtain orange indium sulfide powder particles.
4. The method according to claim 1, wherein the volume ratio of the indium chloride solution, the citric acid aqueous solution and the sodium sulfide solution is 1: 2: 1.
5. the method according to claim 1, wherein the concentration ratio of the indium chloride solution, the citric acid aqueous solution and the sodium sulfide solution is 1: (0.1-0.15): 2.
6. the method according to claim 5, wherein the concentration ratio of the indium chloride solution, the citric acid aqueous solution and the sodium sulfide solution is 14: 1.9: 28.
7. the method according to any one of claims 1 to 6, characterized in that the hydrothermal treatment process comprises the steps of: weighing indium sulfide powder, dispersing the indium sulfide powder in deionized water, carrying out ultrasonic treatment, transferring the uniform suspension liquid into a high-pressure reaction kettle, placing the high-pressure reaction kettle in an electric heating forced air drying oven, and keeping the temperature at constant temperature; and after the reaction is finished, naturally cooling to room temperature, centrifugally separating the product, washing the product with absolute ethyl alcohol and deionized water respectively, finally drying in vacuum, and grinding to obtain the hydrothermally treated indium sulfide powder.
8. The method according to claim 6, wherein the hydrothermal treatment process comprises the steps of: weighing 500 mg of indium sulfide powder, dispersing the indium sulfide powder in 40ml of deionized water, carrying out ultrasonic treatment for 1 hour, transferring the uniform suspension into a 100ml high-pressure reaction kettle, placing the kettle in an electric heating air blowing drying box, carrying out heat preservation for 4-24 hours at a constant temperature of 140 ℃, naturally cooling to room temperature after the reaction is finished, carrying out centrifugal separation on products, washing the products with absolute ethyl alcohol and deionized water for three times respectively, finally drying in a vacuum drying box at 60 ℃ for 8 hours, and grinding the products with a mortar to obtain the indium sulfide powder after hydrothermal treatment.
9. The method of claim 8, wherein the incubation is for 4 hours or 16 to 24 hours.
10. Method according to claim 1, characterized in that it comprises the following steps: dropwise adding 25ml of indium chloride solution with the concentration of 0.112mol/L into 50ml of citric acid aqueous solution with the concentration of 15.2mmol/L, wherein the solvent is deionized water, stirring is required in the dropwise adding process, and stirring is carried out for two hours under constant magnetic stirring after dropwise adding; then 25ml of sodium sulfide solution with the concentration of 0.224mol/L is dropwise added into a solution system of indium chloride and citric acid, and the mixture is magnetically stirred for one hour to obtain yellow suspension; then, centrifuging the product, repeatedly washing the product for 4-5 times by using absolute ethyl alcohol and deionized water, drying the product in a vacuum drying oven at the temperature of 60 ℃, and finally grinding the product by using a mortar to obtain orange indium sulfide powder particles; weighing 500 mg of indium sulfide powder, dispersing the indium sulfide powder in 40ml of deionized water, carrying out ultrasonic treatment for 1 hour, transferring the uniform suspension into a 100ml high-pressure reaction kettle, placing the kettle in an electric heating air blowing drying box, carrying out heat preservation for 4-24 hours at a constant temperature of 140 ℃, naturally cooling to room temperature after the reaction is finished, carrying out centrifugal separation on products, washing the products with absolute ethyl alcohol and deionized water for three times respectively, finally drying in a vacuum drying box at 60 ℃ for 8 hours, and grinding the products with a mortar to obtain the indium sulfide powder after hydrothermal treatment.
11. The method of claim 10, wherein the incubation is for 4 hours or 16 to 24 hours.
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| Application Number | Priority Date | Filing Date | Title |
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