CN115818587A - SiO (silicon dioxide) 2 SnSe/C composite material and preparation method thereof - Google Patents
SiO (silicon dioxide) 2 SnSe/C composite material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 21
- 235000012239 silicon dioxide Nutrition 0.000 title claims description 10
- 239000000377 silicon dioxide Substances 0.000 title claims description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 92
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims description 46
- 239000000243 solution Substances 0.000 claims description 40
- 239000000843 powder Substances 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 28
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 20
- 239000008103 glucose Substances 0.000 claims description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000002077 nanosphere Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 229910052711 selenium Inorganic materials 0.000 claims description 6
- 239000011669 selenium Substances 0.000 claims description 6
- -1 selenium ions Chemical class 0.000 claims description 6
- 229910001432 tin ion Inorganic materials 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- MFIWAIVSOUGHLI-UHFFFAOYSA-N selenium;tin Chemical compound [Sn]=[Se] MFIWAIVSOUGHLI-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004729 solvothermal method Methods 0.000 abstract description 2
- 229920000049 Carbon (fiber) Polymers 0.000 abstract 3
- 239000004917 carbon fiber Substances 0.000 abstract 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract 3
- 239000011248 coating agent Substances 0.000 abstract 2
- 238000000576 coating method Methods 0.000 abstract 2
- 239000002114 nanocomposite Substances 0.000 abstract 1
- 238000011049 filling Methods 0.000 description 18
- 239000002086 nanomaterial Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 150000003346 selenoethers Chemical class 0.000 description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000004108 freeze drying Methods 0.000 description 5
- 238000010532 solid phase synthesis reaction Methods 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012369 In process control Methods 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 238000010965 in-process control Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical compound [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a SiO 2 A/SnSe/C composite material and a preparation method thereof belong to the field of material preparation. By using a one-step solvothermal method on SiO 2 Tin selenide nano-particles with uniform particle size are grown on the surface of the template agentThe structure of the carbon coated carbon fiber is stabilized, the application potential of the carbon coated carbon fiber is improved, and carbon coating treatment is carried out on the carbon coated carbon fiber. The obtained product has uniform particle size and smooth coating. Due to its unique spherical nanocomposite structure, it is expected that it will have great potential for electrochemical applications. The method disclosed by the invention is mild in reaction condition, easy to implement, easy to control in process and wide in application prospect.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to SiO 2 a/SnSe/C composite material and a preparation method thereof.
Background
In recent years, nano materials are widely concerned by people, and have unique nano characteristics such as surface effect, volume effect, quantum tunneling effect and quantum size effect, and due to the effects, the nano materials have better performance in the fields of batteries, electrocatalysis and photocatalysis, energy storage and the like, so that the nano materials are researched by more and more people. The spherical silicon dioxide nano material has stable structure, lower thermal expansion coefficient and dielectric constant, and the silicon element has low price, is abundant in natural resources and is widely concerned. The current methods for preparing silicon dioxide nano spherical materials are mainly divided into liquid phase methods and solid phase methods. The solid phase method for synthesizing the nano material has the advantages of low cost, simple preparation process and large-scale preparation, but the solid phase method generally has the defects of high energy consumption, incapability of accurately controlling the shape and the size and the like, and limits the application range of the nano material. Compared with the solid phase method, the liquid phase method has the advantages of being capable of synthesizing the nano spherical material at the low temperature of 100-200 ℃, simple in equipment and operation, low in cost, capable of realizing the controllability of the size and the shape of the particle diameter of the nano material, capable of avoiding the hard agglomeration phenomenon and the like. At present, most of the existing methods for preparing selenide by using spherical template agent growth have relatively complex reaction steps, and usually, corresponding oxide or sulfide is generated firstly, and then selenide is obtained by adopting a further selenization mode, in particular to the preparation of tin selenide or tin sulfide. The methods have complex processes and complicated steps, and are not beneficial to batch production and industrial application.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the invention provides a SiO 2 The SnSe/C composite material and the preparation method thereof are used for solving the technical problem that the mass production and industrialization of selenide prepared by the growth of a template agent are difficult to realize.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a SiO 2 The preparation method of the/SnSe/C composite material comprises the following steps:
s1: mixing SiO 2 Mixing the nanosphere and the solvent, and adding SnCl 2 ·2H 2 O, obtaining a mixed solution A;
s2: mixing selenium powder and triethanolamine to obtain a mixed solution B; dropwise adding the mixed solution B into the solution A and stirring to obtain a mixed solution C;
s3: putting the mixed solution C into a reaction container for homogeneous reaction, and obtaining a black mixed solution D after the reaction is finished; centrifuging and washing the black mixed solution D to obtain black powder D; mixing the black powder D with a glucose solution, putting the mixture into a reaction vessel for homogeneous reaction to obtain reacted black powder, and carrying out heat treatment on the reacted black powder to obtain SiO 2 a/SnSe/C composite material.
Further, in S1, the SiO 2 Nanosphere, solvent and SnCl 2 ·2H 2 The dosage ratio of O is (20-80) mg: (20 to 60) mL: (0.1-10) g; the solvent is ethylene glycol or glycerol.
Further, in S1, the SiO 2 And mixing the nanospheres and the solvent in an ultrasonic dispersion mode, wherein the ultrasonic dispersion time is 20-80 min.
Furthermore, in S2, the dosage ratio of the selenium powder to the triethanolamine is (0.1-2) g: (2-8) mL; the molar ratio of tin ions to selenium ions in the mixed solution C is 1: (1-5).
Further, in S2, the stirring is performed by a magnetic stirrer, the stirring speed is 100-600 r/min, and the stirring time is 20-80 min.
Further, in S3, the mixed solution C occupies one third to two thirds of the total volume of the reaction vessel in the reaction vessel; placing the mixed solution C into a reaction kettle, sealing the reaction container, placing the reaction container into a phase reactor, carrying out homogeneous reaction, and cooling to room temperature after the reaction is finished to obtain a black mixed solution D, wherein the temperature of the homogeneous reaction is 100-220 ℃, and the reaction time is 1-7 h; the centrifugation and washing are carried out for 2-5 times by adopting ethanol and deionized water.
Further, in S3, the glucose solution is obtained by mixing glucose and deionized water; the dosage ratio of the glucose to the deionized water is (0.1-5) mg: (1-10) mL; the dosage ratio of the selenium powder to the glucose solution is (0.1-2) g: (1-2) mg.
Further, in S3, the black powder D and the glucose solution account for one third to two thirds of the total volume of the reaction kettle in the reaction kettle; and (3) placing the black powder D and the glucose solution into a reaction kettle, sealing the reaction kettle, placing the reaction kettle into a phase reactor, carrying out homogeneous reaction, and cooling to room temperature after the reaction is finished to obtain the reacted black powder, wherein the temperature of the homogeneous reaction is 100-220 ℃, and the reaction time is 2-7 h.
Further, in S3, the process parameters of the heat treatment are as follows: the temperature rising rate is 5-10 ℃/min, the temperature is 200-600 ℃, and the calcination is carried out for 1-5 h.
The invention also discloses SiO prepared by the preparation method 2 a/SnSe/C composite material.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a SiO 2 The preparation method of the/SnSe/C composite material is to use a one-step solvothermal method to prepare SiO 2 Form panelTin selenide nano-particles with uniform particle size are grown on the surface of the agent, so that the preparation of selenide by growing a spherical template agent is simplified; the method disclosed by the invention has the advantages of mild reaction conditions, easiness in realization and easiness in process control, and solves the technical problems of batch production and industrialization in the preparation of selenide by the growth of the template agent.
The invention also discloses SiO prepared by the preparation method 2 The structure of the existing SnSe material is not stable enough, the conductivity is not good enough, and the SnSe is coated with carbon and the carbon material is used as a supporting material, so that the SnSe can be kept stable in an electrode material better, the conductivity of the SnSe is increased, the application potential of the SnSe is improved, and the SnSe/C composite material is expected to have excellent effect in electrochemical application.
Drawings
FIG. 1 shows SiO prepared by the present invention 2 XRD pattern of/SnSe/C composite material;
FIG. 2 shows SiO prepared by the present invention 2 SEM image of/SnSe/C composite material.
Detailed Description
To make the features and effects of the present invention comprehensible to those skilled in the art, general description and definitions are made below with reference to terms and expressions mentioned in the specification and claims. 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 to which this invention belongs.
The theory or mechanism described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, i.e., the present disclosure may be practiced without being limited by any particular theory or mechanism.
All features defined herein as numerical ranges or percentage ranges, such as values, amounts, levels and concentrations, are for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to cover and specifically disclose all possible subranges and individual numerical values (including integers and fractions) within the range.
In this document, unless otherwise specified, "comprising," including, "" containing, "" having, "or the like, means" consisting of … … "and" consisting essentially of … …, "e.g.," a comprises a "means" a comprises a and the other "and" a comprises a only.
In this context, for the sake of brevity, not all possible combinations of features in the various embodiments or examples are described. Therefore, the respective features in the respective embodiments or examples may be arbitrarily combined as long as there is no contradiction between the combinations of the features, and all the possible combinations should be considered as the scope of the present specification.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out under conventional conditions or conditions recommended by the manufacturers. The various starting materials used in the examples which follow, unless otherwise indicated, are conventional commercial products having specifications which are conventional in the art. In the description of the present invention and the following examples, "%" represents weight percent, "parts" represents parts by weight, and proportions represent weight ratios, unless otherwise specified.
Example 1
SiO (silicon dioxide) 2 The preparation method of the/SnSe/C composite material comprises the following steps:
the SiO with good dispersity, good uniformity and particle size of about 300nm is prepared by using TEOS under alkaline condition and adopting a Stober method 2 Nanospheres;
s1: 20mg of SiO are weighed 2 Adding into 20mL of ethylene glycol, performing ultrasonic dispersion for 20min, and adding 0.1g of SnCl 2 ·2H 2 O, stirring toCompletely dissolving to obtain a solution A;
s2: adding 0.1g of selenium powder into 4ml of triethanolamine solvent, and stirring until the selenium powder is completely dissolved to obtain a solution B; and dropwise adding the solution B into the solution A, stirring by using a magnetic device at the stirring speed of 300r/min for 20min to form a mixed solution C, wherein the molar ratio of tin ions to selenium ions in the mixed solution C is 1:3;
s3: filling the obtained mixed solution C into a high-pressure reaction kettle, ensuring the volume filling ratio to be between one third and two thirds, then putting the sealed reaction kettle into a homogeneous reaction instrument, setting the temperature parameter to be 100 ℃, reacting for 1h, carrying out homogeneous reaction, and cooling to room temperature after the reaction is finished to obtain a black mixed solution D; centrifuging and washing the obtained black mixed solution D by using absolute ethyl alcohol and deionized water respectively for 3 times, and drying the centrifuged substance in a freeze drying oven for 6 hours to obtain black powder D;
mixing the black powder D with 0.1mg of glucose solution, and then filling the mixture into a high-pressure reaction kettle, wherein the volume filling ratio is ensured to be between one third and two thirds. Placing the sealed reaction kettle into a homogeneous reactor, setting the temperature parameter to be 100 ℃, the reaction time to be 2 hours, carrying out homogeneous reaction, obtaining black powder after the reaction is finished, placing the obtained black powder after the reaction into a tubular furnace for heat treatment, wherein the temperature of the tubular furnace is 600 ℃, the heating rate is 10 ℃/min, and the calcination time is 5 hours, and finally obtaining SiO 2 a/SnSe/C composite material.
Example 2
SiO (silicon dioxide) 2 The preparation method of the/SnSe/C composite material comprises the following steps:
the SiO with good dispersity, good uniformity and particle size of about 300nm is prepared by using TEOS under alkaline condition and adopting a Stober method 2 Nanospheres;
s1: 30mg of SiO are weighed 2 Adding into 30mL glycerol, ultrasonic dispersing for 30min, and adding 0.2g SnCl 2 ·2H 2 O, stirring until the solution is completely dissolved to obtain a solution A;
s2: adding 0.2g of selenium powder into 5mL of triethanolamine solvent, and stirring until the selenium powder is completely dissolved to obtain a solution B; and dropwise adding the solution B into the solution A, stirring by using a magnetic device at the stirring speed of 400r/min for 30min to form a mixed solution C, wherein the molar ratio of tin ions to selenium ions in the mixed solution C is 1:2;
s3: filling the obtained mixed solution C into a high-pressure reaction kettle, ensuring the volume filling ratio to be between one third and two thirds, then putting the sealed reaction kettle into a homogeneous reaction instrument, setting the temperature parameter to be 130 ℃, reacting for 3 hours, carrying out homogeneous reaction, and cooling to room temperature after the reaction is finished to obtain a black mixed solution D; centrifuging and washing the obtained black mixed solution D for 4 times by using absolute ethyl alcohol and deionized water respectively, and then putting the centrifuged substance into a freeze drying oven for drying for 7 hours to obtain black powder D;
mixing the black powder D with 0.8mg of glucose solution, and then filling the mixture into a high-pressure reaction kettle, wherein the volume filling ratio is ensured to be between one third and two thirds. Putting the sealed reaction kettle into a homogeneous reactor, setting the temperature parameter to be 120 ℃, setting the reaction time to be 3 hours, carrying out homogeneous reaction, obtaining black powder after the reaction is finished, putting the obtained black powder after the reaction into a tubular furnace for heat treatment, wherein the temperature of the tubular furnace is 550 ℃, the heating rate is 8 ℃/min, and the calcination time is 4 hours, thus finally obtaining SiO 2 a/SnSe/C composite material.
Example 3
SiO (silicon dioxide) 2 The preparation method of the/SnSe/C composite material comprises the following steps:
the SiO with good dispersity, good uniformity and particle size of about 300nm is prepared by using TEOS under alkaline condition and adopting a Stober method 2 Nanospheres;
s1: 40mg of SiO are weighed 2 Adding into 40mL of ethylene glycol, performing ultrasonic dispersion for 80min, and adding 0.3g of SnCl 2 ·2H 2 O, stirring until the O is completely dissolved to obtain a solution A;
s2: adding 0.3g of selenium powder into 6mL of triethanolamine solvent, and stirring until the selenium powder is completely dissolved to obtain a solution B; and dropwise adding the solution B into the solution A, stirring by using a magnetic device at the stirring speed of 100r/min for 80min to form a mixed solution C, wherein the molar ratio of tin ions to selenium ions in the mixed solution C is 1:1;
s3: filling the obtained mixed solution C into a high-pressure reaction kettle, ensuring the volume filling ratio to be between one third and two thirds, then putting the sealed reaction kettle into a homogeneous reactor, setting the temperature parameter to be 120 ℃, carrying out homogeneous reaction for 4 hours, and cooling to room temperature after the reaction is finished to obtain a black mixed solution D; centrifuging and washing the obtained black mixed solution D by using absolute ethyl alcohol and deionized water respectively for 3 times, and drying the centrifuged substance in a freeze drying oven for 7 hours to obtain black powder D;
mixing the black powder D with 1mg of glucose solution, and then putting the mixture into a high-pressure reaction kettle to ensure that the volume filling ratio is between one third and two thirds. Putting the sealed reaction kettle into a homogeneous reactor, setting the temperature parameter to be 120 ℃, setting the reaction time to be 4 hours, carrying out homogeneous reaction, obtaining black powder after the reaction is finished, putting the obtained black powder after the reaction into a tubular furnace for heat treatment, wherein the temperature of the tubular furnace is 500 ℃, the heating rate is 6 ℃/min, and the calcination time is 5 hours, and finally obtaining SiO 2 a/SnSe/C composite material.
Example 4
SiO (silicon dioxide) 2 The preparation method of the/SnSe/C composite material comprises the following steps:
SiO with good dispersity, good uniformity and particle size of about 300nm is prepared by TEOS under alkaline condition by Stober method 2 Nanospheres;
s1: 80mg of SiO are weighed 2 Adding into 60mL of ethylene glycol, performing ultrasonic dispersion for 80min, and adding 1g of SnCl 2 ·2H 2 O, stirring until the O is completely dissolved to obtain a solution A;
s2: adding 0.8g of selenium powder into 8mL of triethanolamine solvent, and stirring until the selenium powder is completely dissolved to obtain a solution B; and dropwise adding the solution B into the solution A, stirring by using a magnetic device at the stirring speed of 600r/min for 80min to form a mixed solution C, wherein the molar ratio of tin ions to selenium ions in the mixed solution C is 1:2;
s3: filling the obtained mixed solution C into a high-pressure reaction kettle, ensuring the volume filling ratio to be between one third and two thirds, then putting the sealed reaction kettle into a homogeneous reaction instrument, setting the temperature parameter to be 180 ℃, reacting for 7 hours, carrying out homogeneous reaction, and cooling to room temperature after the reaction is finished to obtain a black mixed solution D; centrifuging and washing the obtained black mixed solution D for 3 times by using absolute ethyl alcohol and deionized water respectively, and drying the centrifuged substance in a freeze drying oven for 8 hours to obtain black powder D;
mixing the black powder D with 2mg of glucose solution, and then putting the mixture into a high-pressure reaction kettle to ensure that the volume filling ratio is between one third and two thirds. Putting the sealed reaction kettle into a homogeneous reactor, setting the temperature parameter to be 180 ℃, the reaction time to be 5h, carrying out homogeneous reaction, obtaining reacted black powder after the reaction is finished, putting the obtained reacted black powder into a tubular furnace for heat treatment, and finally obtaining SiO, wherein the temperature of the tubular furnace is 600 ℃, the heating rate is 5 ℃/min, and the calcination time is 4h 2 a/SnSe/C composite material.
Example 5
SiO (silicon dioxide) 2 The preparation method of the/SnSe/C composite material comprises the following steps:
the SiO with good dispersity, good uniformity and particle size of about 300nm is prepared by using TEOS under alkaline condition and adopting a Stober method 2 Nanospheres;
s1: 30mg of SiO are weighed 2 Adding into 60mL of ethylene glycol, performing ultrasonic dispersion for 50min, and adding 10g of SnCl 2 ·2H 2 O, stirring until the solution is completely dissolved to obtain a solution A;
s2: adding 2g of selenium powder into 2mL of triethanolamine solvent, and stirring until the selenium powder is completely dissolved to obtain a solution B; dropwise adding the solution B into the solution A, and stirring by using a magnetic device at the stirring speed of 100r/min for 80min to form a mixed solution C;
s3: filling the obtained mixed solution C into a high-pressure reaction kettle, ensuring the volume filling ratio to be between one third and two thirds, then putting the sealed reaction kettle into a homogeneous reaction instrument, setting the temperature parameter to be 220 ℃, and the reaction time to be 1h, carrying out homogeneous reaction, and after the reaction is finished, cooling to room temperature to obtain a black mixed solution D; centrifuging and washing the obtained black mixed solution D for 5 times by using absolute ethyl alcohol and deionized water respectively, and then putting the centrifuged substance into a freeze drying oven for drying for 8 hours to obtain black powder D;
mixing the black powder D with 2mg of glucose solution, and then filling the mixture into a high-pressure reaction kettle, wherein the volume filling ratio is ensured to be between one third and two thirds. Placing the sealed reaction kettle into a homogeneous reactor, setting the temperature parameter to be 220 ℃, the reaction time to be 7h, carrying out homogeneous reaction, obtaining black powder after the reaction is finished, placing the obtained black powder after the reaction into a tubular furnace for heat treatment, wherein the temperature of the tubular furnace is 200 ℃, the heating rate is 5 ℃/min, and the calcination time is 1h, and finally obtaining SiO 2 a/SnSe/C composite material.
FIG. 1 shows SiO prepared by the present invention 2 XRD pattern of/SnSe/C composite material, as can be seen, the peak value of XRD is exactly corresponding to standard card 48-1224 (SnSe), which shows that in SiO 2 SnSe is successfully grown on the nanospheres.
FIG. 2 shows the SiO prepared by the present invention 2 SEM picture of/SnSe/C composite material, from which SiO can be seen 2 @ SnSe is a substance having a layer of small particles and also some agglomeration, which is made of SiO 2 The result of mixing and synthesizing the @ SnSe and the glucose solution is that the substance is coated by carbon.
The above contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention should not be limited thereby, and any modification made on the basis of the technical idea proposed by the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. SiO (silicon dioxide) 2 The preparation method of the/SnSe/C composite material is characterized by comprising the following steps:
s1: mixing SiO 2 Mixing the nanosphere and the solvent, and adding SnCl 2 ·2H 2 O, obtaining a mixed solution A;
s2: mixing selenium powder and triethanolamine to obtain a mixed solution B; dropwise adding the mixed solution B into the solution A and stirring to obtain a mixed solution C;
s3: putting the mixed solution C into a reaction container for homogeneous reaction to obtain a black mixed solution D after the reaction is finished; centrifuging and washing the black mixed solution D to obtain black powder D; mixing the black powder D with glucose solution, placing the mixture into a reaction vessel for homogeneous reaction to obtain reacted black powder, and performing heat treatment on the reacted black powder to obtain SiO 2 a/SnSe/C composite material.
2. An SiO as claimed in claim 1 2 The preparation method of the/SnSe/C composite material is characterized in that in S1, the SiO 2 Nanospheres, solvents and SnCl 2 ·2H 2 The dosage ratio of O is (20-80) mg: (20-60) mL: (0.1-10) g; the solvent is ethylene glycol or glycerol.
3. An SiO as claimed in claim 1 2 The preparation method of the/SnSe/C composite material is characterized in that in S1, the SiO 2 The nanospheres and the solvent are mixed in an ultrasonic dispersion mode, and the ultrasonic dispersion time is 20-80 min.
4. SiO as claimed in claim 1 2 The preparation method of the/SnSe/C composite material is characterized in that in S2, the dosage ratio of the selenium powder to the triethanolamine is (0.1-2) g: (2-8) mL; the molar ratio of tin ions to selenium ions in the mixed solution C is 1: (1-5).
5. An SiO as claimed in claim 1 2 The preparation method of the/SnSe/C composite material is characterized in that in S2, the stirring is carried out by adopting a magnetic device, the stirring speed is 100-600 r/min, and the stirring time is 20-80 min.
6. An SiO as claimed in claim 1 2 /SnSThe preparation method of the e/C composite material is characterized in that in S3, the mixed solution C accounts for one third to two thirds of the total volume of a reaction vessel; placing the mixed solution C into a reaction kettle, sealing the reaction container, placing the reaction container into a phase reactor, carrying out homogeneous reaction, and cooling to room temperature after the reaction is finished to obtain a black mixed solution D, wherein the temperature of the homogeneous reaction is 100-220 ℃, and the reaction time is 1-7 h; the centrifugation and washing are carried out for 2-5 times by adopting ethanol and deionized water.
7. An SiO as claimed in claim 1 2 The preparation method of the/SnSe/C composite material is characterized in that in S3, the glucose solution is obtained by mixing glucose and deionized water; the dosage ratio of the glucose to the deionized water is (0.1-5) mg: (1-10) mL; the dosage ratio of the selenium powder to the glucose solution is (0.1-2) g: (1-2) mg.
8. An SiO as claimed in claim 1 2 The preparation method of the/SnSe/C composite material is characterized in that in S3, black powder D and glucose solution account for one third to two thirds of the total volume of a reaction kettle in the reaction kettle; and (3) placing the black powder D and the glucose solution into a reaction kettle, sealing the reaction kettle, placing the reaction kettle into a phase reactor, carrying out homogeneous reaction, and cooling to room temperature after the reaction is finished to obtain the reacted black powder, wherein the temperature of the homogeneous reaction is 100-220 ℃, and the reaction time is 2-7 h.
9. An SiO as claimed in claim 1 2 The preparation method of the/SnSe/C composite material is characterized in that in S3, the technological parameters of the heat treatment are as follows: the temperature rising rate is 5-10 ℃/min, the temperature is 200-600 ℃, and the calcination is carried out for 1-5 h.
10. Using a SiO as claimed in any of claims 1 to 9 2 SiO prepared by preparation method of/SnSe/C composite material 2 a/SnSe/C composite material.
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