CN116574483A - Preparation method of tellurium nanowire multi-component composite material - Google Patents
Preparation method of tellurium nanowire multi-component composite material Download PDFInfo
- Publication number
- CN116574483A CN116574483A CN202310534446.1A CN202310534446A CN116574483A CN 116574483 A CN116574483 A CN 116574483A CN 202310534446 A CN202310534446 A CN 202310534446A CN 116574483 A CN116574483 A CN 116574483A
- Authority
- CN
- China
- Prior art keywords
- heating
- stirring
- tellurium
- composite material
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 107
- 239000002070 nanowire Substances 0.000 title claims abstract description 98
- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 164
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 97
- 238000003756 stirring Methods 0.000 claims abstract description 89
- 239000002904 solvent Substances 0.000 claims abstract description 57
- 239000000243 solution Substances 0.000 claims abstract description 42
- 239000011259 mixed solution Substances 0.000 claims abstract description 29
- 239000012046 mixed solvent Substances 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 24
- 150000001875 compounds Chemical class 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 239000004094 surface-active agent Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 13
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 13
- 239000012467 final product Substances 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 29
- 229910021389 graphene Inorganic materials 0.000 claims description 28
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 27
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 16
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 16
- 238000003760 magnetic stirring Methods 0.000 claims description 16
- 238000010907 mechanical stirring Methods 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 235000006708 antioxidants Nutrition 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- 235000010323 ascorbic acid Nutrition 0.000 claims description 7
- 229960005070 ascorbic acid Drugs 0.000 claims description 7
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 7
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 7
- 229960001763 zinc sulfate Drugs 0.000 claims description 7
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 6
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 235000011150 stannous chloride Nutrition 0.000 claims description 6
- 239000001119 stannous chloride Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 4
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 4
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 235000007686 potassium Nutrition 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 4
- VOADVZVYWFSHSM-UHFFFAOYSA-L sodium tellurite Chemical compound [Na+].[Na+].[O-][Te]([O-])=O VOADVZVYWFSHSM-UHFFFAOYSA-L 0.000 claims description 4
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 4
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 4
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- XQSBLCWFZRTIEO-UHFFFAOYSA-N hexadecan-1-amine;hydrobromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[NH3+] XQSBLCWFZRTIEO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- IIXQANVWKBCLEB-UHFFFAOYSA-N tellurium trioxide Chemical compound O=[Te](=O)=O IIXQANVWKBCLEB-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 2
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 claims description 2
- 229940083575 sodium dodecyl sulfate Drugs 0.000 claims description 2
- 229940082004 sodium laurate Drugs 0.000 claims description 2
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 2
- 229940080350 sodium stearate Drugs 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 12
- 239000013078 crystal Substances 0.000 description 8
- 238000002310 reflectometry Methods 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- QOYRNHQSZSCVOW-UHFFFAOYSA-N cadmium nitrate tetrahydrate Chemical compound O.O.O.O.[Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QOYRNHQSZSCVOW-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
A preparation method of tellurium nanowire multi-element composite material, belonging to the technical field of composite material preparation. The method comprises the following steps: mixing a tellurium source with a volatilizable alcohol solvent, heating and stirring uniformly to obtain a solution I; mixing, heating and uniformly stirring a surfactant and a volatilizable alcohol solvent to obtain a solution II; mixing an alkaline compound with an alcohol solvent, heating and stirring uniformly to obtain a solution III; heating and uniformly stirring the solution I, the solution II and the solution III to obtain a mixed solution; introducing inert gas into the mixed solution, adding a reducing agent, heating and stirring uniformly to obtain a precursor, and adding a material to be compounded and an antioxidant into the precursor to obtain a tellurium nanowire composite material mixed solution; and (3) washing the final product with the mixed solvent for multiple times, and centrifugally drying to obtain the tellurium nanowire multi-element composite material. The invention has the advantages of short preparation period, simple and controllable process, safety, no pollution, low energy consumption, excellent product performance, suitability for laboratory preparation, large-scale production in factories and the like.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a preparation method of a tellurium nanowire multi-element composite material.
Background
Tellurium is a metalloid element, and is now gradually developed into a material supporting the development of high-precision technology, and can be used as a novel infrared detection material, a glass colorant, a power generation component, a novel thin film solar cell key material and the like in the metallurgical industry, the petrochemical industry, the electronic industry and new energy technology. Tellurium is made into nano wires, and excellent photoelectric properties are obtained by utilizing the anisotropy of the nano wires, and binary combination of the tellurium nano wires and noble metals or compounds can further enhance the photoelectric properties of the nano wires. However, few reports on the electromagnetic wave absorption performance of tellurium nanowires and composites thereof are reported. The graphene, mxene and other 2D structural materials have the advantages of light specific gravity, high absorption value and the like when applied to the field of electromagnetic wave absorption, and if tellurium nanowires are compounded with the 2D structural graphene and Mxene, the electromagnetic wave absorption performance of the tellurium nanowires is expected to be further improved. However, few reports are about the preparation of tellurium nanowires/graphene/Mxene and other multicomponent composite materials and the analysis of electromagnetic absorption performance. Therefore, if the method for preparing the tellurium nanowire/graphene/Mxene composite material in a large scale and at low cost is invented, the high-performance electromagnetic wave absorbing material is expected to be obtained to meet the application requirements of the field.
In the synthesis of telluride nanowire based on hydrothermal method (2018, 04 period of material science), vitamin C, CTAB, sodium tellurite and cadmium nitrate tetrahydrate are used as raw materials, and the telluride nanowire is prepared by hydrothermal method. The method has the advantages of easy preparation environment and the like. However, the risk is high in the experimental process, and the prepared nanowires are easy to agglomerate, so that the performance of the nanowires is influenced.
Method for preparing metal tellurium nanowires by thermal evaporation(rare Metal materials and engineering. 2021,50 (10)) to be high-purity Bi 2 Te 3 As an evaporation source, one-dimensional tellurium nanowires were successfully prepared on Au-coated quartz plates, and the experimental depth analyzed the growth mechanism of the high-purity one-dimensional Te nanowires. The experiment requires high temperature conditions to obtain the final product, and has the advantages of low yield, relatively high preparation cost and no market competitiveness.
In Environmentally Benign Synthesis ofUltrathin Metal Telluride Nanowires (journal of American society of chemistry, 2014, 7, 8) as TeO 2 Preparing a precursor by taking KOH and ascorbic acid as raw materials, and compounding noble metals such as Cu, ag and the like with the precursor by utilizing a hydrothermal method to prepare the ultrathin tellurium nanowire composite material. The experimental preparation process is environment-friendly, and the diameter of the nanowire of the final experimental product is short.
In the preparation method of the flexible reduced graphene and tellurium nanowire composite thermoelectric film (application number 201511023207.1), graphene oxide powder and sodium styrenesulfonate are used as raw materials, a tellurium nanowire/glass fiber film initial sample is obtained through the steps of a hydrothermal method, vacuum filtration and the like, and a final product is obtained through reaction under the protection of high temperature and inert gas. The product has higher Seebeck coefficient and good thermoelectric conversion performance. However, the preparation process of the method is too complex, so that the experimental environment is harsh, and the popularization and application are seriously affected.
In view of the above, tellurium nanowires have been widely studied as important functional materials, and particularly can exhibit more excellent properties after being compounded with other materials. However, few reports on the compounding of the layered 2d structure such as tellurium nanowires/graphene/Mxene are available.
Disclosure of Invention
The invention solves the problem that no tellurium nanowire multi-element composite material exists in China at present, and provides a preparation method of the tellurium nanowire multi-element composite material.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a tellurium nanowire multi-element composite material, which comprises the following steps:
step one: mixing tellurium source and volatilizable alcohol solvent in a certain proportion, heating and stirring uniformly to obtain solution I;
step two: mixing, heating and uniformly stirring a surfactant and a volatilizable alcohol solvent according to a certain proportion to obtain a solution II;
step three: mixing an alkaline compound with an alcohol solvent according to a certain proportion, heating and uniformly stirring to obtain a solution III;
step four: placing the solution I, the solution II and the solution III in a three-neck flask, heating and uniformly stirring to obtain a mixed solution;
step five: introducing inert gas into the mixed solution, adding a reducing agent at a certain temperature, heating and uniformly stirring to obtain a precursor, and adding a material to be compounded and an antioxidant into the precursor to obtain a tellurium nanowire composite material mixed solution;
step six: and (3) washing the final product with a mixed solvent with a certain volume ratio for multiple times, and centrifugally drying to obtain the tellurium nanowire multi-element composite material.
Further, in the first step, the tellurium source is one or more of tellurium dioxide, tellurium trioxide or sodium tellurite; the volatilizable alcohol solvent is one or more of glycol, ethanol, glycerol, isobutanol or methanol; the mass ratio of the tellurium source to the volatilizable alcohol solvent is 1:1 to 10; the heating is direct heating or magnetic heating, and the used heater is one of a controllable electromagnetic heating furnace, a heating rod or an infrared heater; the stirring is magnetic stirring or mechanical stirring, and the stirring rotating speed is 50-500 r/min; the heating temperature is 25-100 ℃; the heating and stirring time is 10 min-100 min.
Further, in the second step, the surfactant is one or more of polyvinylpyrrolidone, cetyl ammonium bromide, sodium oleate, octadecyl amine, sodium laurate, sodium stearate, sodium dodecyl sulfate or sodium dodecyl benzene sulfonate; the volatilizable alcohol solvent is one or more of glycol, ethanol, glycerol, isobutanol or methanol; the mass ratio of the surfactant to the alcohol solvent is 1:1 to 8; the heating is direct heating or magnetic heating; the heating temperature is 30-90 ℃; the rotating speed of the stirrer is 30 r/min-600 r/min; the heating and stirring time is 20-80 min.
Further, in the third step, the alkaline compound is one or more of potassium hydroxide, sodium hydroxide, triethanolamine, methylamine, urea, ethylamine, ethanolamine, ethylenediamine, dimethylamine, trimethylamine, triethylamine, propylamine or isopropylamine; the alcohol solvent is one or more of glycol, ethanol, glycerol, isobutanol or methanol; the stirring is magnetic stirring or mechanical stirring; the mass ratio of the alkaline compound to the alcohol solvent is 1:1 to 8; the heating is direct heating or magnetic heating; the heating temperature is 20-90 ℃; the rotating speed of the stirrer is 30 r/min-500 r/min; the heating and stirring time is 20-90 min.
Further, in the fourth step, the heating is direct heating or magnetic heating; the stirring is magnetic stirring or mechanical stirring; the heating temperature is 10-90 ℃; the rotating speed of the stirrer is 20 r/min-400 r/min; the heating and stirring time is 10 min-90 min.
In the fifth step, the inert gas is one or more of nitrogen and argon, and the gas flow rate is 0.1L/min-5L/min; the temperature is 40-200 ℃; the reducing agent is one or more of ascorbic acid, sodium borohydride, stannous chloride, oxalic acid or potassium borohydride; the heating is direct heating or magnetic heating; the heating time is 1-60 h; the stirring is magnetic stirring or mechanical stirring, and the rotating speed is 50-800 r/min; the stirring time is 1-60 h; the material to be compounded is one or more of Mxene, graphene, copper sulfate, nickel nitrate or zinc sulfate; the antioxidant is one or more of ascorbic acid, sodium borohydride, stannous chloride, oxalic acid or potassium borohydride.
In the sixth step, the mixed solvent is a mixed solution of ethanol and water, and the volume ratio of the ethanol to the water is 2:1 to 10; the volume ratio of the mixed solvent to the tellurium nanowire composite material mixed solution is 1:2 to 10; the washing times are 5-10 times; the centrifugal mode is a high-speed centrifugal machine; the speed of the centrifugation is 3000 r/min-5000 r/min, and the time is 2 min-20 min; the drying temperature is 100-200 ℃ and the drying time is 1-2 h; the diameter of tellurium nanowires in the tellurium nanowire composite material is 50-500 nm, and the length of tellurium nanowires in the tellurium nanowire composite material is 10-50 mm; the reflectivity of the tellurium nanowire composite material is-10 dB to-60 dB.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the tellurium nanowire/graphene/Mxene composite material, the one-dimensional tellurium nanowire, the two-dimensional graphene, the Mxene and the like are compounded to form the three-dimensional structure composite material, and electromagnetic waves reach higher loss through multiple refraction in the three-dimensional structure material.
2. The polarity of the polar solvent and the polarity of the surfactant are utilized to tightly combine three materials of tellurium nanowires, graphene and Mxene, and when electromagnetic wave radiation is received, various interface polarizations are generated so as to consume the electromagnetic wave.
3. The method can regulate the reaction time and temperature of each step and the change of the functional group of the surfactant to control the radius and the length of the tellurium nanowire.
4. The invention has the advantages of short preparation period, simple and controllable process, safety, no pollution, low energy consumption, excellent product performance, suitability for laboratory preparation, large-scale production in factories and the like.
5. The tellurium nanowire/graphene/Mxene three-dimensional structure composite material with various polarization effect interfaces is prepared by utilizing a thermal decomposition method in a regulatable manner.
6. In the invention, other composite materials can be directly added into the tellurium nanowires in the reaction process, and a plurality of tightly combined composite materials can be obtained.
7. The three-dimensional structure material is applied to the electromagnetic wave absorption field, the reflectivity of the three-dimensional structure material is-26 dB when the optimal content is 20 percent (80 percent of paraffin), and the high absorption value under the condition of very low content is obtained.
Drawings
FIG. 1 is an XRD pattern of a tellurium nanowire/graphene/Mxene composite.
Fig. 2 is a transmission electron microscope image of tellurium nanowires.
FIG. 3 is a transmission electron microscopy image of tellurium nanowires/graphene/Mxene composites.
Fig. 4 is an electromagnetic wave absorption diagram of a tellurium nanowire/graphene/Mxene composite.
Detailed Description
The following description of the present invention refers to the accompanying drawings and examples, but is not limited to the same, and modifications and equivalents of the present invention can be made without departing from the spirit and scope of the present invention.
Example 1:
the preparation method of the tellurium nanowire/graphene/Mxene composite material comprises the following steps:
step one: mixing tellurium source and volatilizable alcohol solvent in a certain proportion, heating and stirring uniformly to obtain solution I;
the tellurium source is tellurium dioxide; the volatilizable alcohol solvent is ethylene glycol; the mass ratio of the tellurium source to the volatilizable alcohol solvent is 1:2; the heating mode is direct heating; the heater is a controllable electromagnetic heating furnace; the stirring is magnetic stirring; the heating temperature is 30 ℃ and the time is 10min; the rotating speed of the stirrer is 100r/min;
step two: mixing, heating and uniformly stirring a surfactant and a volatilizable alcohol solvent according to a certain proportion to obtain a solution II;
the surfactant is polyvinylpyrrolidone; the volatilizable alcohol solvent is ethylene glycol; the mass ratio of the surfactant to the alcohol solvent is 1:2; the heating mode is direct heating; the heating temperature is 40 ℃ and the time is 30min; the rotating speed of the stirrer is 100r/min;
step three: mixing, heating and stirring the alkaline compound and the alcohol solvent according to a certain proportion uniformly to obtain a solution III.
The alkaline compound is potassium hydroxide; the alcohol solvent is ethylene glycol; the stirring is magnetic stirring; the mass ratio of the alkaline compound to the alcohol solvent is 1:2; the heating mode is direct heating; the heating temperature is 30 ℃; the rotating speed of the stirrer is 100r/min; the heating and stirring time is 30min;
step four: and (3) placing the solution I, the solution II and the solution III in a three-necked flask, heating and uniformly stirring to obtain a mixed solution.
The heating mode is direct heating; the stirring is magnetic stirring; the heating temperature is 20 ℃; the rotating speed of the stirrer is 100r/min; the heating and stirring time is 20min;
step five: and (3) introducing inert gas into the mixed solution, adding a reducing agent at a certain temperature, heating and uniformly stirring to obtain a precursor, and adding a material to be compounded and an antioxidant into the precursor to obtain the tellurium nanowire composite mixed solution.
The inert gas is argon; the gas flow rate is 1L/min; the temperature is 50 ℃; the reducing agent is ascorbic acid; the heating mode is direct heating; the heating time is 20 hours; the stirring mode is magnetic stirring; the rotating speed of the stirrer is 100r/min; the stirring time is 2 hours; the material to be compounded is Mxene and graphene; the antioxidant is ascorbic acid;
step six: and (3) washing the final product with a mixed solvent with a certain volume ratio for multiple times, and centrifugally drying to obtain tellurium nanowire composite material solid.
The mixed solvent is a mixed solvent of ethanol and water; the volume ratio of the mixed solvent is 2:3, a step of; the volume ratio of the mixed solvent to the tellurium nanowire composite material mixed solution is 1:3, a step of; the washing times are 6 times; the centrifugal mode is a high-speed centrifugal machine; the centrifugal speed is 3500r/min; centrifuging for 3min; the drying temperature is 100 ℃; drying time is 1h; the length of the tellurium nanowire in the tellurium nanowire/graphene/Mxene composite material is 16mm, and the diameter is 206nm; the reflectivity of the tellurium nanowire/graphene/Mxene composite material is-26 dB.
As can be seen from the XRD pattern (fig. 1), the sample was found to be 2θ=23.544 DEG, 27.563 DEG, 38.261 DEG, 43.332 DEG, 51.941 DEG, 61.585 DEG diffraction peaks correspond to (100), (101), (102), (111), (103), (211) structural crystal planes of Te crystals, respectively, which are consistent with diffraction peak positions of standard PDF cards PDF#36-1452, indicating successful preparation of Te. Diffraction peaks at 2θ= 25.721 °,28.263 °,29.873 °,48.163 °,50.983 ° correspond to C respectively 70 The (003), (101), (012), (211), (214) structural crystal planes of the crystals are consistent with the positions of diffraction peaks of the standard PDF card PDF#48-1449, and correspond to the SEM results of FIG. 2, indicating successful coating of graphene. Diffraction peaks at 2θ= 27.858 °,29.733 ° 47.535 °,57.168 °,60.599 ° correspond to C respectively 3 N 4 The (110), (200), (111), (220), (310) structural crystal planes of the crystals are consistent with the diffraction peak positions of the standard PDF card PDF#50-1512, which indicates that Te compound nanowires prepared by a Te/graphene/Mxene system are successfully prepared. By the thank you le formulaThe diameter of the Te compound nanowire crystal particle prepared by the Te/graphene/Mxene system can be calculated from the half-width of the characteristic peak of the crystal face (101) of Te to be about 206nm.
The linear structure is evident from fig. 2, which illustrates the successful fabrication of tellurium nanowires.
As can be seen from fig. 3, tellurium nanowires are distributed on the surface or inside of graphene and Mxene, and the size distribution is 200nm to 250nm, and the prepared nanowires have smaller size due to the addition of graphene and Mxene, so that the composite material has a multilayer structure.
FIG. 4 is reflectance data for a sample at 20% (80% paraffin wax). As can be seen from the graph, the absorption peaks of different frequency bands are different in thickness, the reflectance (more than 90% absorption rate) of less than-10 is shown at the thickness of 1-5.5mm, and the optimal reflectance is-26 dB at the thickness of 3 mm. Therefore, the absorption frequency band can be changed by adjusting the thickness of the tellurium nanowires, which shows that the tellurium nanowires can achieve good electromagnetic wave absorption effect under the condition of low content.
Example 2:
the preparation method of the tellurium nanowire/copper sulfate/Mxene composite material comprises the following steps:
step one: and mixing the tellurium source with the volatilizable alcohol solvent according to a certain proportion, heating and stirring uniformly to obtain a solution I.
The tellurium source is tellurium trioxide; the volatilizable alcohol solvent is ethanol; the mass ratio of the tellurium source to the volatilizable alcohol solvent is 1:3, a step of; the heating is magnetic heating; the heater is a heating rod; the stirring is mechanical stirring; the heating temperature is 40 ℃; the rotating speed of the stirrer is 200r/min; the heating and stirring time is 20min;
step two: mixing, heating and stirring the surfactant and the volatilizable alcohol solvent according to a certain proportion to obtain a solution II.
The surfactant is cetyl ammonium bromide; the volatilizable alcohol solvent is ethanol; the mass ratio of the surfactant to the alcohol solvent is 1:3, a step of; the heating is magnetic heating; the heating temperature is 50 ℃; the rotating speed of the stirrer is 200r/min; the heating and stirring time is 40min;
step three: mixing, heating and stirring the alkaline compound and the alcohol solvent according to a certain proportion uniformly to obtain a solution III.
The alkaline compound is sodium hydroxide; the alcohol solvent is ethanol; the stirring is mechanical stirring; the mass ratio of the alkaline compound to the alcohol solvent is 1:3, a step of; the heating is magnetic heating; the heating temperature is 40 ℃; the rotating speed of the stirrer is 200r/min; the heating and stirring time is 30min;
step four: and (3) placing the solution I, the solution II and the solution III in a three-necked flask, heating and uniformly stirring to obtain a mixed solution.
The heating is magnetic heating; the stirring is mechanical stirring; the heating temperature is 30 ℃; the rotating speed of the stirrer is 200r/min; the heating and stirring time is 40min;
step five: and (3) introducing inert gas into the mixed solution, adding a reducing agent at a certain temperature, heating and uniformly stirring to obtain a precursor, and adding a material to be compounded and an antioxidant into the precursor to obtain the tellurium nanowire composite mixed solution.
The inert gas is helium; the gas flow rate is 2L/min; the temperature is as follows: 60 ℃; the reducing agent is sodium borohydride; the heating is magnetic heating; the heating time is 40h; the stirring mode is mechanical stirring; the rotating speed of the stirrer is 200r/min; the stirring time is 3 hours; the materials to be compounded are Mxene and copper sulfate; the antioxidant is sodium borohydride;
step six: and (3) washing the final product with a mixed solvent with a certain volume ratio for multiple times, and centrifugally drying to obtain tellurium nanowire composite material solid.
The mixed solvent is a mixed solvent of ethanol and water; the volume ratio of the mixed solvent is 2:3, a step of; the mass ratio of the mixed solvent to the tellurium nanowire composite material mixed solution is 1:3, a step of; the washing times are 7 times; the centrifugal mode is a high-speed centrifugal machine; the centrifugal speed is 4000r/min; the centrifugation time is 4min; the drying temperature is 150 ℃; drying time is 2h; the length of the tellurium nanowire in the tellurium nanowire/copper sulfate/Mxene composite material is 18mm, and the diameter is 203nm; the reflectivity of the tellurium nanowire/copper sulfate/Mxene composite material is-25 dB.
Example 3:
the preparation method of the tellurium nanowire/nickel nitrate/Mxene composite material comprises the following steps:
step one: and mixing the tellurium source with the volatilizable alcohol solvent according to a certain proportion, heating and stirring uniformly to obtain a solution I.
The tellurium source is sodium tellurite; the volatilizable alcohol solvent is glycerol; the mass ratio of the tellurium source to the volatilizable alcohol solvent is 1:4, a step of; the heating is direct heating; the heater is an infrared heater; the stirring is magnetic stirring; the heating temperature is 50 ℃; the rotating speed of the stirrer is 400r/min; the heating and stirring time is 40min;
step two: mixing, heating and stirring the surfactant and the volatilizable alcohol solvent according to a certain proportion to obtain a solution II.
The surfactant is sodium oleate; the volatilizable alcohol solvent is glycerol; the mass ratio of the surfactant to the alcohol solvent is 1:4, a step of; the heating is direct heating; the heating temperature is 60 ℃; the rotating speed of the stirrer is 400r/min; the heating and stirring time is 40min;
step three: mixing, heating and stirring the alkaline compound and the alcohol solvent according to a certain proportion uniformly to obtain a solution III.
The alkaline compound is triethanolamine; the alcohol solvent is glycerol; the stirring is magnetic stirring; the mass ratio of the alkaline compound to the alcohol solvent is 1:4, a step of; the heating is direct heating; the heating temperature is 50 ℃; the rotating speed of the stirrer is 400r/min; the heating and stirring time is 50min;
step four: and (3) placing the solution I, the solution II and the solution III in a three-necked flask, heating and uniformly stirring to obtain a mixed solution.
The heating is direct heating; the stirring is magnetic stirring; the heating temperature is 40 ℃; the rotating speed of the stirrer is 300r/min; the heating and stirring time is 40min;
step five: and (3) introducing inert gas into the mixed solution, adding a reducing agent at a certain temperature, heating and uniformly stirring to obtain a precursor, and adding a material to be compounded and an antioxidant into the precursor to obtain the tellurium nanowire composite mixed solution.
The inert gas is nitrogen; the gas flow rate is 3L/min; the temperature is 70 ℃; the reducing agent is stannous chloride; the heating mode is direct heating; the heating time is 4 hours; the stirring mode is magnetic stirring; the rotating speed of the stirrer is 400r/min; the stirring time is 4 hours; the material to be compounded is Mxene and nickel nitrate; the antioxidant is stannous chloride;
step six: and (3) washing the final product with a mixed solvent with a certain volume ratio for multiple times, and centrifugally drying to obtain tellurium nanowire composite material solid.
The mixed solvent is a mixed solvent of ethanol and water; the volume ratio of the mixed solvent is 2:5, a step of; the mass ratio of the mixed solvent to the tellurium nanowire composite material mixed solution is 1:4, a step of; the washing times are 8 times; the centrifugal mode is a high-speed centrifugal machine; the centrifugal speed is 4000r/min; the centrifugation time is 6min; the drying temperature is 100 ℃; drying time is 1h; the length of tellurium nanowires in the tellurium nanowire composite material is 20mm; the diameter of the tellurium nanowire in the tellurium nanowire/nickel nitrate/Mxene composite material is 210nm; the reflectivity of the tellurium nanowire/nickel nitrate/Mxene composite material is-23 dB.
Example 4:
the preparation method of the tellurium nanowire/graphene/zinc sulfate composite material is specifically completed according to the following steps.
Step one: and mixing the tellurium source with the volatilizable alcohol solvent according to a certain proportion, heating and stirring uniformly to obtain a solution I.
The tellurium source is tellurium dioxide; the volatilizable alcohol solvent is isobutanol; the mass ratio of the tellurium source to the volatilizable alcohol solvent is 1:10; the heating is magnetic heating; the heater is a controllable electromagnetic heating furnace; the stirring is mechanical stirring; the heating temperature is 100 ℃; the rotating speed of the stirrer is 500r/min; the heating and stirring time is 100min;
step two: mixing, heating and stirring the surfactant and the volatilizable alcohol solvent according to a certain proportion to obtain a solution II.
The surfactant is sodium dodecyl benzene sulfonate; the volatilizable alcohol solvent is isobutanol; the mass ratio of the surfactant to the alcohol solvent is 1:8, 8; the heating is magnetic heating; the heating temperature is 90 ℃; the rotating speed of the stirrer is 600r/min; the heating and stirring time is 80min;
step three: mixing, heating and stirring the alkaline compound and the alcohol solvent according to a certain proportion uniformly to obtain a solution III.
The alkaline compound is methylamine; the alcohol solvent is methanol; the stirring is mechanical stirring; the mass ratio of the alkaline compound to the alcohol solvent is 1:8, 8; the heating is magnetic heating; the heating temperature is 90 ℃; the rotating speed of the stirrer is 500r/min; the heating and stirring time is 90min;
step four: and (3) placing the solution I, the solution II and the solution III in a three-necked flask, heating and uniformly stirring to obtain a mixed solution.
The heating is magnetic heating; the stirring is mechanical stirring; the heating temperature is 90 ℃; the rotating speed of the stirrer is 400r/min; the heating and stirring time is 90min;
step five: and (3) introducing inert gas into the mixed solution, adding a reducing agent at a certain temperature, heating and uniformly stirring to obtain a precursor, and adding a material to be compounded and an antioxidant into the precursor to obtain the tellurium nanowire composite mixed solution.
The inert gas is argon; the gas flow rate is 5L/min; the temperature is 100 ℃; the reducing agent is oxalic acid; the heating is magnetic heating and the like; the heating time is 5 hours; the stirring mode is mechanical stirring; the rotating speed of the stirrer is 600r/min; the stirring time is 5 hours; the material to be compounded is graphene or zinc sulfate; the antioxidant is oxalic acid;
step six: and (3) washing the final product with a mixed solvent with a certain volume ratio for multiple times, and centrifugally drying to obtain tellurium nanowire composite material solid.
The mixed solvent is a mixed solvent of ethanol and water; the volume ratio of the mixed solvent is 2:7, preparing a base material; the mass ratio of the mixed solvent to the tellurium nanowire composite material mixed solution is 1:5, a step of; the washing times are 9 times; the centrifugal mode is a high-speed centrifugal machine; the centrifugal speed is 4000r/min; the centrifugation time is 6min; the drying temperature is 150 ℃; drying time is 2h; the length of the tellurium nanowire in the tellurium nanowire/graphene/zinc sulfate composite material is 18mm; the diameter of tellurium nanowires in the tellurium nanowire/graphene/zinc sulfate composite material is 200nm; the reflectivity of the tellurium nanowire/graphene/zinc sulfate composite material is-24 dB.
Claims (7)
1. A preparation method of a tellurium nanowire multi-element composite material is characterized by comprising the following steps of: the method comprises the following steps:
step one: mixing a tellurium source with a volatilizable alcohol solvent, heating and stirring uniformly to obtain a solution I;
step two: mixing, heating and uniformly stirring a surfactant and a volatilizable alcohol solvent to obtain a solution II;
step three: mixing an alkaline compound with an alcohol solvent, heating and stirring uniformly to obtain a solution III;
step four: heating and uniformly stirring the solution I, the solution II and the solution III to obtain a mixed solution;
step five: introducing inert gas into the mixed solution, adding a reducing agent, heating and stirring uniformly to obtain a precursor, and adding a material to be compounded and an antioxidant into the precursor to obtain a tellurium nanowire composite material mixed solution;
step six: and (3) washing the final product with the mixed solvent for multiple times, and centrifugally drying to obtain the tellurium nanowire multi-element composite material.
2. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the first step, the tellurium source is one or more of tellurium dioxide, tellurium trioxide or sodium tellurite; the volatilizable alcohol solvent is one or more of glycol, ethanol, glycerol, isobutanol or methanol; the mass ratio of the tellurium source to the volatilizable alcohol solvent is 1:1 to 10; the heating is direct heating or magnetic heating, and the used heater is one of a controllable electromagnetic heating furnace, a heating rod or an infrared heater; the stirring is magnetic stirring or mechanical stirring, and the stirring rotating speed is 50-500 r/min; the heating temperature is 25-100 ℃; the heating and stirring time is 10 min-100 min.
3. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the second step, the surfactant is one or more of polyvinylpyrrolidone, cetyl ammonium bromide, sodium oleate, octadecylamine, sodium laurate, sodium stearate, sodium dodecyl sulfate or sodium dodecyl benzene sulfonate; the volatilizable alcohol solvent is one or more of glycol, ethanol, glycerol, isobutanol or methanol; the mass ratio of the surfactant to the alcohol solvent is 1:1 to 8; the heating is direct heating or magnetic heating; the heating temperature is 30-90 ℃; the rotating speed of the stirrer is 30 r/min-600 r/min; the heating and stirring time is 20-80 min.
4. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the third step, the alkaline compound is one or more of potassium hydroxide, sodium hydroxide, triethanolamine, methylamine, urea, ethylamine, ethanolamine, ethylenediamine, dimethylamine, trimethylamine, triethylamine, propylamine or isopropylamine; the alcohol solvent is one or more of glycol, ethanol, glycerol, isobutanol or methanol; the stirring is magnetic stirring or mechanical stirring; the mass ratio of the alkaline compound to the alcohol solvent is 1:1 to 8; the heating is direct heating or magnetic heating; the heating temperature is 20-90 ℃; the rotating speed of the stirrer is 30 r/min-500 r/min; the heating and stirring time is 20-90 min.
5. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the fourth step, the heating is direct heating or magnetic heating; the stirring is magnetic stirring or mechanical stirring; the heating temperature is 10-90 ℃; the rotating speed of the stirrer is 20 r/min-400 r/min; the heating and stirring time is 10 min-90 min.
6. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the fifth step, the inert gas is one or more of nitrogen and argon, and the gas flow rate is 0.1L/min-5L/min; the temperature is 40-200 ℃; the reducing agent is one or more of ascorbic acid, sodium borohydride, stannous chloride, oxalic acid or potassium borohydride; the heating is direct heating or magnetic heating; the heating time is 1-60 h; the stirring is magnetic stirring or mechanical stirring, and the rotating speed is 50-800 r/min; the stirring time is 1-60 h; the material to be compounded is one or more of Mxene, graphene, copper sulfate, nickel nitrate or zinc sulfate; the antioxidant is one or more of ascorbic acid, sodium borohydride, stannous chloride, oxalic acid or potassium borohydride.
7. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the sixth step, the mixed solvent is a mixed solution of ethanol and water, and the volume ratio of the ethanol to the water is 2:1 to 10; the volume ratio of the mixed solvent to the tellurium nanowire composite material mixed solution is 1:2 to 10; the washing times are 5-10 times; the centrifugal mode is a high-speed centrifugal machine; the speed of the centrifugation is 3000 r/min-5000 r/min, and the time is 2 min-20 min; the drying temperature is 100-200 ℃ and the drying time is 1-2 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310534446.1A CN116574483A (en) | 2023-05-12 | 2023-05-12 | Preparation method of tellurium nanowire multi-component composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310534446.1A CN116574483A (en) | 2023-05-12 | 2023-05-12 | Preparation method of tellurium nanowire multi-component composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116574483A true CN116574483A (en) | 2023-08-11 |
Family
ID=87537159
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310534446.1A Pending CN116574483A (en) | 2023-05-12 | 2023-05-12 | Preparation method of tellurium nanowire multi-component composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116574483A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103219066A (en) * | 2012-01-19 | 2013-07-24 | 中国科学院上海硅酸盐研究所 | Flexible conductive thin film compositing two-dimensional graphene and one-dimensional nanowire and preparation method thereof |
| CN103794265A (en) * | 2014-02-26 | 2014-05-14 | 无锡格菲电子薄膜科技有限公司 | Composite material of graphene and nanowires and preparation method thereof |
| CN110449169A (en) * | 2019-07-04 | 2019-11-15 | 中山大学 | A kind of semi-metallic Te nano wire/graphene hydrogel composite material and its preparation method and application |
| CN112680778A (en) * | 2020-11-09 | 2021-04-20 | 青海大学 | Preparation method of single crystal silver telluride nanotubes with uniform size |
| CN112954991A (en) * | 2021-01-27 | 2021-06-11 | 武汉工程大学 | MXene/metal nanowire composite material and freeze-thaw assembly method and application thereof |
| CN115807240A (en) * | 2022-12-26 | 2023-03-17 | 青岛科技大学 | Preparation method of carbon-supported tellurium nanowire nano material |
-
2023
- 2023-05-12 CN CN202310534446.1A patent/CN116574483A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103219066A (en) * | 2012-01-19 | 2013-07-24 | 中国科学院上海硅酸盐研究所 | Flexible conductive thin film compositing two-dimensional graphene and one-dimensional nanowire and preparation method thereof |
| CN103794265A (en) * | 2014-02-26 | 2014-05-14 | 无锡格菲电子薄膜科技有限公司 | Composite material of graphene and nanowires and preparation method thereof |
| CN110449169A (en) * | 2019-07-04 | 2019-11-15 | 中山大学 | A kind of semi-metallic Te nano wire/graphene hydrogel composite material and its preparation method and application |
| CN112680778A (en) * | 2020-11-09 | 2021-04-20 | 青海大学 | Preparation method of single crystal silver telluride nanotubes with uniform size |
| CN112954991A (en) * | 2021-01-27 | 2021-06-11 | 武汉工程大学 | MXene/metal nanowire composite material and freeze-thaw assembly method and application thereof |
| CN115807240A (en) * | 2022-12-26 | 2023-03-17 | 青岛科技大学 | Preparation method of carbon-supported tellurium nanowire nano material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105110318A (en) | Graphene aqueous slurry, and preparation method thereof | |
| CN109273702A (en) | The all solid state preparation method of irregular micro-nano particle coated with uniform graphene | |
| CN105200520B (en) | One kind prepares Bi2(SexTe1‑x)3The method of single crystal nanoplate | |
| CN112093801B (en) | Rice hull-based nano silicon carbide/carbon composite wave-absorbing material and preparation method thereof | |
| CN114871444B (en) | Preparation method of silver powder with high tap density and narrow particle size distribution | |
| CN102219523B (en) | Low-temperature co-firing ceramic wave-absorbing material and preparation method thereof | |
| CN112225186A (en) | Preparation method of spherical boron nitride | |
| US20220306540A1 (en) | Method for preparing infrared radiation ceramic material | |
| CN116574483A (en) | Preparation method of tellurium nanowire multi-component composite material | |
| CN109713115B (en) | Cu-Se-S system thermoelectric material and preparation method thereof | |
| CN105921742B (en) | A method of preparing hexagonal boron nitride package nano nickle granules | |
| CN107960050A (en) | A kind of preparation method of graphene/three-dimensional flower-shaped bismuth ferrite composite wave-suction material | |
| CN105290414A (en) | Method for synthesizing nano copper particles | |
| CN115318210B (en) | Preparation method and application of cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding | |
| CN101165001B (en) | Method for preparing silicon carbide ceramic plasticized by sheet aluminum oxide particle and carbon fibre combination | |
| Li et al. | Preparation of micro-size flake silver powder by planetary ball mill | |
| CN112980389A (en) | Preparation method of functionalized graphene wave-absorbing material | |
| CN114604858B (en) | Three-dimensional reduction graphene oxide rGO/ScFeO 3 Preparation method of composite wave-absorbing material | |
| CN110695372A (en) | Preparation method for improving copper-graphene interface by using rare earth elements | |
| CN102502835A (en) | Method for preparing silver molybdate nano square crystal | |
| CN111943254B (en) | Uniformly dispersed zinc oxide-multilayer graphene composite material and preparation method thereof | |
| CN102585588B (en) | Preparation method of copper-zinc-tin-sulfur ink | |
| CN110213954B (en) | Halloysite/boron-nitrogen co-doped carbon/cobalt composite material and preparation method and application thereof | |
| CN112279223A (en) | Preparation process of refined h-BN powder | |
| CN102009185A (en) | Preparation method of silver nanobelts |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |