CN113101949A - Transition metal selenide heterostructure material and preparation method thereof - Google Patents
Transition metal selenide heterostructure material and preparation method thereof Download PDFInfo
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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 58
- -1 Transition metal selenide Chemical class 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000002243 precursor Substances 0.000 claims abstract description 72
- 150000001768 cations Chemical class 0.000 claims abstract description 44
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 31
- 239000011669 selenium Substances 0.000 claims abstract description 31
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 28
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 238000004321 preservation Methods 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 22
- 229910052786 argon Inorganic materials 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 8
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 4
- DMEGYFMYUHOHGS-UHFFFAOYSA-N cycloheptane Chemical compound C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 4
- YWWZCHLUQSHMCL-UHFFFAOYSA-N diphenyl diselenide Chemical compound C=1C=CC=CC=1[Se][Se]C1=CC=CC=C1 YWWZCHLUQSHMCL-UHFFFAOYSA-N 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 3
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- RJFAYQIBOAGBLC-BYPYZUCNSA-N Selenium-L-methionine Chemical compound C[Se]CC[C@H](N)C(O)=O RJFAYQIBOAGBLC-BYPYZUCNSA-N 0.000 claims description 3
- RJFAYQIBOAGBLC-UHFFFAOYSA-N Selenomethionine Natural products C[Se]CCC(N)C(O)=O RJFAYQIBOAGBLC-UHFFFAOYSA-N 0.000 claims description 3
- 239000012682 cationic precursor Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 3
- ZKXWKVVCCTZOLD-UHFFFAOYSA-N copper;4-hydroxypent-3-en-2-one Chemical compound [Cu].CC(O)=CC(C)=O.CC(O)=CC(C)=O ZKXWKVVCCTZOLD-UHFFFAOYSA-N 0.000 claims description 3
- 229940045803 cuprous chloride Drugs 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 3
- 229960002718 selenomethionine Drugs 0.000 claims description 3
- IYKVLICPFCEZOF-UHFFFAOYSA-N selenourea Chemical compound NC(N)=[Se] IYKVLICPFCEZOF-UHFFFAOYSA-N 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 239000002134 carbon nanofiber Substances 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 229960003280 cupric chloride Drugs 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 239000011858 nanopowder Substances 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- YOUIDGQAIILFBW-UHFFFAOYSA-J tetrachlorotungsten Chemical compound Cl[W](Cl)(Cl)Cl YOUIDGQAIILFBW-UHFFFAOYSA-J 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 6
- 239000002159 nanocrystal Substances 0.000 description 16
- 230000005540 biological transmission Effects 0.000 description 11
- 238000005406 washing Methods 0.000 description 10
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 description 8
- 238000012512 characterization method Methods 0.000 description 6
- 239000002048 multi walled nanotube Substances 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 150000003346 selenoethers Chemical class 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- QVYIMIJFGKEJDW-UHFFFAOYSA-N cobalt(ii) selenide Chemical compound [Se]=[Co] QVYIMIJFGKEJDW-UHFFFAOYSA-N 0.000 description 3
- 238000006053 organic reaction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- IRPLSAGFWHCJIQ-UHFFFAOYSA-N selanylidenecopper Chemical compound [Se]=[Cu] IRPLSAGFWHCJIQ-UHFFFAOYSA-N 0.000 description 3
- KTLOQXXVQYUCJU-UHFFFAOYSA-N [Cu].[Cu].[Se] Chemical compound [Cu].[Cu].[Se] KTLOQXXVQYUCJU-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 208000012868 Overgrowth Diseases 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- MHWZQNGIEIYAQJ-UHFFFAOYSA-N molybdenum diselenide Chemical compound [Se]=[Mo]=[Se] MHWZQNGIEIYAQJ-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a transition metal selenide heterostructure material and a preparation method thereof, wherein the preparation method of the transition metal selenide heterostructure material comprises the following steps: preparing a selenium-containing precursor solution: dissolving a precursor containing selenium element in an organic solution to obtain a selenium-containing precursor solution; preparing a cation precursor solution, wherein the cation precursor solution comprises at least two transition metal elements or simultaneously comprises the transition metal elements and the nano carbon material; and (3) heterostructure preparation: heating the cation precursor solution to 190-280 ℃, stirring and injecting the selenium-containing precursor solution under the protection of inert gas, and carrying out heat preservation and stirring reaction for 5-25min at the temperature of 180-260 ℃. The preparation method has the advantages of simplicity, convenience, practicability, short preparation time, low cost, good repeatability and the like, and the prepared finished product has the advantages of small particle size, excellent dispersibility and the like.
Description
Technical Field
The invention relates to the field of preparation of electric/photocatalyst, in particular to a transition metal selenide heterostructure material and a preparation method thereof.
Background
The global mineral energy is becoming more and more exhausted and the environmental problem is severe, which has become a known major challenge in the world today. By means of the electrocatalysis/photocatalysis technology, water can be decomposed to generate clean energy, namely hydrogen, so that the problems of environment and energy can be solved ideally, and the method is one of the new technologies which are acknowledged in the world at present and have the most application prospect. In the technical field of electro-catalysis/photocatalysis, the type, structure, morphology and surface physicochemical properties of a key material of the catalyst have important influence on the catalytic activity of the catalyst. The development of low-cost and high-efficiency non-noble metal catalysts is an important way for solving the problem of large-scale commercial clean energy preparation.
In recent years, reports of transition metal selenide heterostructure nanomaterials as electro/photocatalysts are emerging. The transition metal selenide semiconductor material has a narrow forbidden band width, and can directly absorb visible light to realize the excitation and transition of valence band electrons. Selenides are more metallic and have lower resistivity than oxides and sulfides. Moreover, a heterostructure is constructed between the selenide and the nano carbon material or a heterostructure is formed between two or more transition metal selenides, so that the adjustment of forbidden bandwidth can be realized, a directional electron rapid transmission channel is formed at a heterogeneous interface, abundant surface lattice defects and catalytic active sites can be formed in the heterogeneous process, and the improvement of electrocatalysis/photocatalysis performance are promoted. Therefore, the transition metal selenide heterostructure nano material is expected to replace high-cost noble metal-based catalysts (such as platinum, iridium, ruthenium and the like) and is applied to the light/electric catalysis field of energy and environment on a large scale.
However, there are many technical problems in the field of research on transition metal selenide heterojunction materials, and a solution is urgently needed. The most critical problem is that the particle size of the transition metal selenide heterojunction material is too large, and the dispersibility is poor. In the process of forming the heterostructure, experimental conditions are difficult to control, overgrowth of heterojunction particles is easy to form, and the problem of overlarge size is caused, so that the specific surface area of the transition metal selenide heterojunction material is seriously reduced, and the quantity of effective catalytic active sites on the surface is greatly improved. In addition, a plurality of different transition metal selenides are easy to cause serious agglomeration in the process of heterogenization or the process of heterogenization of the transition metal selenides and the nano carbon material, so that originally exposed surface catalytic active sites are covered in agglomerated particles, and the great improvement of the optical/electric catalytic activity of the transition metal selenide heterojunction material is limited.
Disclosure of Invention
Therefore, the technical problem to be solved by the present invention is to overcome the defect that serious agglomeration is easily caused in the process of heterogenizing a plurality of different transition metal selenides or the process of heterogenizing a transition metal selenide and a nanocarbon material in the prior art, so as to provide a preparation method of a transition metal selenide heterostructure material with small particle size and excellent dispersibility.
A method of preparing a transition metal selenide heterostructure material, comprising:
preparing a selenium-containing precursor solution: dissolving a precursor containing selenium element in an organic solution to obtain a selenium-containing precursor solution;
preparing a cation precursor solution, wherein the cation precursor solution comprises at least two transition metal elements or simultaneously comprises the transition metal elements and the nano carbon material;
and (3) heterostructure preparation: heating the cation precursor solution to 190-280 ℃, stirring and injecting the selenium-containing precursor solution under the protection of inert gas, and carrying out heat preservation and stirring reaction for 5-25min at the temperature of 180-260 ℃. The rotation speed of the stirring is 300-900 r/min.
Furthermore, the molar ratio of the precursor containing selenium element to the cation precursor is (0.4-2.5): 1.
during the preparation of the cationic precursor solution,
when the cation precursor solution does not contain the nano carbon material, the specific preparation process comprises the following steps: mixing a cation precursor with an organic solution, stirring at a temperature not higher than 120 ℃ under the protection of inert gas, and further preparing a cation precursor solution;
when the cation precursor solution comprises the nano carbon material, the specific preparation process comprises the following steps: mixing an organic solution with a nano carbon material, carrying out ultrasonic treatment at the temperature of not more than 80 ℃ under the protection of inert gas to prepare a nano carbon material suspension, then mixing a cation precursor with the nano carbon material suspension, and stirring at the temperature of not more than 120 ℃ under the protection of inert gas to prepare a cation precursor solution.
Further, the ultrasonic treatment power of the nano carbon material suspension is more than 180w, the treatment temperature is 50-80 ℃, and the treatment time is 1-5 h. The treatment temperature of the added cation precursor is 70-120 ℃.
The nano carbon material is at least one of carbon black nano powder, graphene nano powder, carbon nano fiber and carbon nano tube.
The cation precursor in the cation precursor solution is chloride containing transition metal elements or/and organic metal salt containing transition metal elements;
preferably, the transition metal element is selected from copper, cobalt, nickel, molybdenum, tungsten and zinc;
more preferably, the chloride containing the transition metal element is at least one of cuprous chloride, cupric chloride, cobalt chloride, nickel chloride and tungsten chloride; the transition metal element-containing organic metal salt is at least one of copper acetate, cobalt acetate, nickel acetate, copper acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, molybdenum acetylacetonate, and zinc acetate.
The organic solution is an organic matter with a melting point lower than 40 ℃ and a derivative thereof;
preferably, the carbon chain length of the organic solution is twelve to twenty-four carbons;
more preferably, the organic solution is at least one of octadecene, oleic acid, oleylamine and trioctylphosphine.
The inert gas is argon or nitrogen.
The precursor containing selenium element is at least one of elemental selenium powder, selenourea, selenomethionine and diphenyl diselenide.
After the preparation process of the heterostructure is finished, cooling to be below 80 ℃, and cleaning at least once to prepare a finished product; the cleaning process comprises the following steps: ultrasonic cleaning with organic solvent and centrifuging.
The organic solvent is at least two of n-hexane, cyclohexane, methylcyclohexane, toluene, xylene, tetrahydrofuran, cycloheptane, isopropanol, n-propanol, ethanol and methanol.
A transition metal selenide heterostructure material is prepared by the preparation method of the transition metal selenide heterostructure material.
The technical scheme of the invention has the following advantages:
1. the preparation method provided by the invention comprises the steps of heating a cation precursor solution to 190-; by the treatment of the process step, even under the condition of multiple transition metal elements, the metal selenide heterostructure with uniform size and high crystallinity can be obtained, and the particle size of the heterostructure is less than 30 nanometers and is monodisperse; meanwhile, when the raw materials simultaneously contain the transition metal element and the nano carbon material, the method can also be adopted to effectively prevent the nano carbon material and the transition metal element from agglomerating in the heterogenization process, so as to obtain the high-dispersion nano material with the heterogenization of the metal selenide and the carbon substrate, wherein the size of the heterostructure of the metal selenide is less than 35 nanometers, the heterostructure is highly dispersed on the carbon substrate, the heterostructure is not agglomerated, and the dispersion effect is excellent.
2. The preparation method provided by the invention is simple and easy to implement, short in preparation time, low in cost and good in repeatability.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a representation result related to the heterostructure nanomaterial containing the combination of nickel selenide nanocrystals and multi-walled carbon nanotubes prepared in example 1 of the present invention. Wherein (a) is a low power transmission electron microscope picture; (b) is a high power transmission electron microscope picture; (c) a dark field picture of the transmission electron microscope; (d) is a magnified transmission electron microscope dark field picture.
Fig. 2 is a representation result related to the heterostructure nano-material containing the combination of copper selenide and cobalt selenide, which is prepared in example 2 of the present invention. Wherein, (a) is a scanning electron microscope picture; (b) a low power transmission electron microscope picture; (c) is a high power transmission electron microscope picture; (d) the two-dimensional scanning imaging is performed on a dark-field picture and element distribution of the transmission electron microscope.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
A preparation method of a transition metal selenide heterostructure material comprises the following steps:
adding 0.069g of multi-walled carbon nano-tube with the diameter of 10-15 nanometers and 20 ml of oleylamine into a three-neck flask, sealing, vacuumizing, introducing argon, performing ultrasonic treatment at the temperature of 60 ℃ under the protection of argon for 2 hours, and dispersing the nano-carbon material in an organic reaction solution to form a nano-carbon material suspension. Then 0.257g of nickel acetylacetonate was charged into the three-necked flask, and vacuum was applied under a seal, followed by introducing argon again. Stirring and processing at the temperature of 80 ℃ under the protection of argon, and dissolving the cation precursor into the suspension to form a cation precursor solution. At the same time, 0.312g of diphenyl diselenide was added to 4 ml of oleylamine and dissolved at a temperature of 100 ℃ to form a selenium-containing precursor solution. Heating the cation precursor solution to 210 ℃, and injecting the selenium-containing precursor solution under the protection of argon and under the condition of rapid stirring. Then incubated at 200 ℃ for 10 minutes.
After the reaction was completed, the heating apparatus was quickly removed, and the reaction apparatus was naturally cooled to below 80 ℃ at room temperature. Adding a proper amount of toluene into the reaction solution, washing the sample by adopting ultrasonic waves, and separating the solid sample by centrifugation. And washing the product twice by adopting methylbenzene and isopropanol respectively, and then drying to obtain the product, namely the transition metal selenide heterostructure material.
The product characterization result (transmission electron microscope) is shown in fig. 1, and the product is a nickel selenide hollow nanocrystal/multi-walled carbon nanotube heterostructure nanomaterial. The external diameter of the nickel selenide nanocrystal is about 30 nanometers, the wall thickness is about 5 nanometers, and the interior of the nickel selenide nanocrystal is of a hollow structure. The nickel selenide hollow nano-crystal grows on the surface of the multi-wall carbon nano-tube in a heterogeneous mode to form a highly dispersed heterogeneous structure.
Example 2
A preparation method of a transition metal selenide heterostructure material comprises the following steps:
0.182g of anhydrous copper acetate, 0.129g of cobalt acetylacetonate, 2 ml of trioctylphosphine and 20 ml of oleylamine are added into a three-neck flask, vacuum pumping is carried out under sealing, then argon is introduced, and stirring and dissolving are carried out at the temperature of 100 ℃ under the protection of argon, so as to form a cation precursor solution. Meanwhile, 0.079g of elemental selenium powder is added into 2 ml of trioctylphosphine and dissolved at 80 ℃ to form a selenium-containing precursor solution. Heating the cation precursor solution to 240 ℃, and injecting the selenium-containing precursor solution under the protection of argon and under the condition of rapid stirring. Then incubated at 230 ℃ for 10 minutes.
After the reaction was completed, the heating apparatus was quickly removed, and the reaction apparatus was naturally cooled to below 80 ℃ at room temperature. Adding a proper amount of toluene into the reaction solution, washing the sample by adopting ultrasonic waves, and separating the solid sample by centrifugation. The product is washed by toluene and isopropanol for three times respectively, and then is dried to obtain the transition metal selenide heterojunction material.
The characterization results (transmission electron microscope) of the product shown in fig. 2 show that the size of the heterojunction nanocrystal composed of copper, cobalt and selenium elements is about 20 nanometers, and the heterojunction nanocrystal is monodisperse. Two-dimensional scanning imaging of element distribution under a transmission electron microscope and a dark field shows that cobalt selenide nano-particles with the size of 2-4 nanometers are heterogeneously grown on copper selenide nano-crystals with the size of 15-20 nanometers, and a heterostructure is formed.
Example 3
A preparation method of a transition metal selenide heterostructure material comprises the following steps:
adding 0.023g of multi-walled carbon nanotubes with the diameter of 8-12 nanometers and 20 ml of oleylamine into a three-neck flask, sealing, vacuumizing, introducing argon, performing ultrasonic treatment at 70 ℃ for 1.5 hours under the protection of argon, and dispersing the nano-carbon material in an organic reaction solution to form a nano-carbon material suspension. Then 0.072g of anhydrous copper acetate and 0.154g of nickel acetylacetonate were introduced into the three-necked flask, and vacuum was applied under a seal, followed by introducing argon again. Stirring the mixture at the temperature of 90 ℃ under the protection of argon, and dissolving a cation precursor into the suspension to form a cation precursor solution. At the same time, 0.125g of diphenyl diselenide was added to 2 ml of oleylamine and dissolved at a temperature of 90 ℃ to form a selenium-containing precursor solution. Heating the cation precursor solution to 225 ℃, and injecting the selenium-containing precursor solution under the protection of argon and under the condition of rapid stirring. Then incubated at 215 ℃ for 15 minutes.
After the reaction was completed, the heating apparatus was quickly removed, and the reaction apparatus was naturally cooled to below 80 ℃ at room temperature. Adding a proper amount of n-hexane into the reaction solution, washing the sample by adopting ultrasonic waves, and separating the solid sample by centrifugation. And washing the product once by adopting methylbenzene, isopropanol and methanol respectively, and then drying to obtain the transition metal selenide heterojunction material.
The product characterization result shows that copper selenide and nickel selenide nanocrystals grow heterogeneously to obtain heterojunction nanocrystals with grain size of about 15 nanometers, and the heterostructure is highly dispersed on the multi-walled carbon nanotube.
Example 4
A preparation method of a transition metal selenide heterostructure material comprises the following steps:
adding 0.024g of single-layer redox graphene powder and 20 ml of oleic acid into a three-neck flask, sealing, vacuumizing, introducing argon, performing ultrasonic treatment at the temperature of 60 ℃ under the protection of argon for 4 hours, and dispersing the nano carbon material in an organic reaction solution to form a nano carbon material suspension. Then 0.163g of molybdenum (VI) acetylacetonate and 0.128g of nickel acetylacetonate were charged into the three-necked flask, and vacuum was applied under a seal, followed by introducing argon again. Stirring the mixture at the temperature of 110 ℃ under the protection of argon, and dissolving a cation precursor into the suspension to form a cation precursor solution. Meanwhile, 0.079g of elemental selenium powder is added into 2 ml of trioctylphosphine and dissolved at 85 ℃ to form a selenium-containing precursor solution. Heating the cation precursor solution to 280 ℃, and injecting the selenium-containing precursor solution under the protection of argon and under the condition of rapid stirring. Then incubated at 260 ℃ for 20 minutes.
After the reaction was completed, the heating apparatus was quickly removed, and the reaction apparatus was naturally cooled to below 80 ℃ at room temperature. Adding a proper amount of toluene into the reaction solution, washing the sample by adopting ultrasonic waves, and separating the solid sample by centrifugation. And washing the product twice by adopting cyclohexane and isopropanol respectively, and then drying to obtain the transition metal selenide heterojunction material.
The product characterization result shows that the molybdenum selenide and the nickel selenide nanocrystals grow in a heterogeneous manner to obtain heterojunction nanocrystals with the grain size of about 25 nanometers, and the heterostructure is highly dispersed on the surface of the single-layer redox graphene.
Example 5
A preparation method of a transition metal selenide heterostructure material comprises the following steps:
0.314g of copper acetylacetonate, 0.257g of cobalt acetylacetonate and 25 ml of oleic acid are added into a three-neck flask, vacuum pumping is carried out under sealing, then nitrogen is introduced, and stirring and dissolving are carried out at the temperature of 120 ℃ under the protection of nitrogen, so as to form a cation precursor solution. At the same time, 0.123g of selenourea was added to 4 ml of oleic acid and dissolved at 100 ℃ to form a selenium-containing precursor solution. Heating the cation precursor solution to 230 ℃, and injecting the selenium-containing precursor solution under the protection of nitrogen and under the rapid stirring. Then incubated at 220 ℃ for 10 minutes.
After the reaction was completed, the heating apparatus was quickly removed, and the three-necked flask was naturally cooled to below 80 ℃ at room temperature. Adding a proper amount of cyclohexane into the reaction solution, washing the sample by adopting ultrasonic waves, and separating the solid sample by centrifugation. The product is washed twice by cyclohexane and methanol respectively, and then dried to obtain the transition metal selenide heterojunction material.
The product characterization result shows that the cuprous selenide and the cobalt selenide nanocrystal generate heterogenous growth, the size of the heterojunction nanocrystal consisting of copper, cobalt and selenium elements is about 25 nanometers, and the dispersibility is excellent.
Example 6
A preparation method of a transition metal selenide heterostructure material comprises the following steps:
0.198g of cuprous chloride, 0.257g of nickel acetylacetonate, 10 ml of octadecene and 15 ml of oleylamine are added into a three-neck flask, vacuum pumping is carried out under sealing, then nitrogen is introduced, and stirring and dissolving are carried out at the temperature of 110 ℃ under the protection of nitrogen, so as to form a cation precursor solution. At the same time, 0.200g selenomethionine was added to 4 ml oleic acid and dissolved at 80 ℃ to form a selenium containing precursor solution. Heating the cation precursor solution to 220 ℃, and injecting the selenium-containing precursor solution under the protection of nitrogen and under the rapid stirring. Then incubated at 210 ℃ for 10 minutes.
After the reaction was completed, the heating apparatus was quickly removed, and the three-necked flask was naturally cooled to below 80 ℃ at room temperature. Adding a proper amount of methylcyclohexane into the reaction solution, washing the sample by using ultrasonic waves, and separating the solid sample by centrifugation. Washing the product with methyl cyclohexane, xylene and ethanol once respectively, and then drying to obtain the transition metal selenide heterojunction material.
The product characterization result shows that cuprous selenide and nickel selenide nanocrystals grow in a heterogeneous manner, the size of a heterojunction nanocrystal consisting of copper, nickel and selenium elements is about 15-20 nanometers, and the dispersibility is excellent.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A method for preparing a transition metal selenide heterostructure material, comprising:
preparing a selenium-containing precursor solution: dissolving a precursor containing selenium element in an organic solution to obtain a selenium-containing precursor solution;
preparing a cation precursor solution, wherein the cation precursor solution comprises at least two transition metal elements or simultaneously comprises the transition metal elements and the nano carbon material;
and (3) heterostructure preparation: heating the cation precursor solution to 190-280 ℃, stirring and injecting the selenium-containing precursor solution under the protection of inert gas, and carrying out heat preservation and stirring reaction for 5-25min at the temperature of 180-260 ℃.
2. The method of claim 1, wherein during the preparation of the cationic precursor solution,
when the cation precursor solution does not contain the nano carbon material, the specific preparation process comprises the following steps: mixing a cation precursor with an organic solution, stirring at a temperature not higher than 120 ℃ under the protection of inert gas, and further preparing a cation precursor solution;
when the cation precursor solution comprises the nano carbon material, the specific preparation process comprises the following steps: mixing an organic solution with a nano carbon material, carrying out ultrasonic treatment at the temperature of not more than 80 ℃ under the protection of inert gas to prepare a nano carbon material suspension, then mixing a cation precursor with the nano carbon material suspension, and stirring at the temperature of not more than 120 ℃ under the protection of inert gas to prepare a cation precursor solution.
3. The method of claim 1 or 2, wherein the nanocarbon material is at least one of carbon black nanopowder, graphene nanopowder, carbon nanofibers and carbon nanotubes.
4. The method for preparing a transition metal selenide heterostructure material according to any of claims 1 to 3, wherein the cation precursor in the cation precursor solution is a chloride containing a transition metal element or/and an organic metal salt containing a transition metal element;
preferably, the transition metal element is selected from copper, cobalt, nickel, molybdenum, tungsten and zinc;
more preferably, the chloride containing the transition metal element is at least one of cuprous chloride, cupric chloride, cobalt chloride, nickel chloride and tungsten chloride; the transition metal element-containing organic metal salt is at least one of copper acetate, cobalt acetate, nickel acetate, copper acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, molybdenum acetylacetonate, and zinc acetate.
5. The method for preparing a transition metal selenide heterostructure material according to any one of claims 1 to 4, wherein the organic solution is an organic substance having a melting point lower than 40 ℃ and a derivative thereof;
preferably, the carbon chain length of the organic solution is twelve to twenty-four carbons;
more preferably, the organic solution is at least one of octadecene, oleic acid, oleylamine and trioctylphosphine.
6. The method of any one of claims 1-5, wherein the inert gas is argon or nitrogen.
7. The method for preparing a transition metal selenide heterostructure material according to any one of claims 1 to 6, wherein the selenium-containing precursor is at least one of elemental selenium powder, selenourea, selenomethionine and diphenyl diselenide.
8. The method of any one of claims 1-7, wherein the heterostructure material is cooled to a temperature below 80 ℃ after the heterostructure fabrication process is completed, and then cleaned at least once to form a finished product; the cleaning process comprises the following steps: carrying out ultrasonic cleaning and centrifugation by adopting an organic solvent;
preferably, the organic solvent is at least two of n-hexane, cyclohexane, methylcyclohexane, toluene, xylene, tetrahydrofuran, cycloheptane, isopropanol, n-propanol, ethanol, and methanol.
9. The method of claim 2, wherein the molar ratio of the selenium-containing precursor to the cationic precursor is (0.4-2.5): 1;
preferably, the ultrasonic treatment temperature of the nano carbon material suspension is 50-80 ℃, and the treatment time is 1-5 h; the treatment temperature of the added cation precursor is 70-120 ℃.
10. A transition metal selenide heterostructure material, characterized in that it is prepared by a method of preparation of a transition metal selenide heterostructure material according to any of claims 1 to 9.
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