CN110127749A - A kind of preparation method of the cuprous sulfide nano flower of cupric defect - Google Patents
A kind of preparation method of the cuprous sulfide nano flower of cupric defect Download PDFInfo
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- CN110127749A CN110127749A CN201910450346.4A CN201910450346A CN110127749A CN 110127749 A CN110127749 A CN 110127749A CN 201910450346 A CN201910450346 A CN 201910450346A CN 110127749 A CN110127749 A CN 110127749A
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- nano flower
- cuprous sulfide
- sulfide nano
- water
- cupric
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- 239000002057 nanoflower Substances 0.000 title claims abstract description 69
- AQMRBJNRFUQADD-UHFFFAOYSA-N copper(I) sulfide Chemical compound [S-2].[Cu+].[Cu+] AQMRBJNRFUQADD-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 230000007547 defect Effects 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000010949 copper Substances 0.000 claims abstract description 43
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052802 copper Inorganic materials 0.000 claims abstract description 40
- 239000004094 surface-active agent Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 19
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 19
- 239000011734 sodium Substances 0.000 claims abstract description 19
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 16
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 10
- 238000010792 warming Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 75
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 67
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 30
- 239000003513 alkali Substances 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 239000000047 product Substances 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 14
- 235000013339 cereals Nutrition 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 8
- 229960000935 dehydrated alcohol Drugs 0.000 description 8
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 2
- 229910001950 potassium oxide Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The present invention relates to a kind of preparation methods of the cuprous sulfide nano flower of cupric defect, belong to technical field of nano material.Highly basic, surfactant, elemental copper, hydrazine hydrate, vulcanized sodium are uniformly mixed by the present invention with water, are warming up to temperature at the uniform velocity under air-proof condition as 180 ~ 220 DEG C and 22 ~ 24 h of isothermal reaction and are obtained reaction system；Reaction system is cooled to room temperature, centrifuge separation, remove supernatant liquor, then adopt be washed with deionized to cleaning solution for neutrality, be drying to obtain cuprous sulfide nano flower.The method of the present invention reaction condition is mild, yield is high, product morphology is relatively uniform and reproducible, and the average grain diameter of cuprous sulfide nano flower obtained is 700 nm ~ 1.9 μm, and the average grain diameter for forming the nanometer sheet of nano flower is 400 nm or so；Cuprous sulfide nano flower of the present invention has hierarchical structure and cupric defect, can be applicable to the fields such as photochemical catalyst, solar battery, electrochemical energy storing device and sensor.
Description
Technical field
The present invention relates to a kind of preparation methods of the cuprous sulfide nano flower of cupric defect, belong to nano material technology neck
Domain.
Background technique
Cuprous sulfide is cheap, is a kind of important transient metal sulfide and a kind of good more of chemical stability
Function semiconductor material.Cuprous sulfide material particle size is small for nanometer, large specific surface area, and due to quantum size effect, skin effect
And macro quanta tunnel effect, with the incomparable light of block materials, electricity and electrochemical properties, therefore cuprous sulfide nanometer
Material is widely used in the fields such as photochemical catalyst, solar battery, electrochemical energy storing device and sensor, extensive by people
Concern and research.There are many preparation method of cuprous sulfide nano material, such as chemical precipitation method, microwave irradiation, vapor deposition
Method, with phase method, colloidal sol ~ gel method, microemulsion method, hydrothermal synthesis method, spray pyrolysis and ultrasonic etc..These methods exist
Shortcomings to a certain extent, such as Product size or pattern are difficult to control, yield is not high, severe reaction conditions or preparation process ratio
It is more complex and the cost is relatively high.
Summary of the invention
In view of the problems of the existing technology the present invention, provides a kind of preparation method of cuprous sulfide nano flower, the present invention
Prepared under mild reaction conditions using highly basic, surfactant, elemental copper, salt and water as raw material it is with hierarchical structure,
The cuprous sulfide nano flower of cupric defect, the method for the present invention reaction condition is mild, easy to operate, yield is high, obtained vulcanization
Cuprous nano flower has the characteristics that size is controllable, regular appearance.
A kind of preparation method of the cuprous sulfide nano flower of cupric defect, the specific steps are as follows:
Highly basic, surfactant, elemental copper, hydrazine hydrate and vulcanized sodium are mixed with water, it is even under air-proof condition after mixing
It is 180 ~ 220 DEG C and isothermal reaction 22 ~ obtain reaction system for 24 hours that speed, which is warming up to temperature,；Reaction system is cooled to room temperature, centrifugation point
From, removal supernatant liquor, then dehydrated alcohol and deionized water is used to wash to cleaning solution as neutrality, it is drying to obtain cuprous sulfide and receives
Popped rice.
The highly basic is the compound alkali of potassium hydroxide and sodium hydroxide.
Further, it is 2:(1 ~ 2 that the mass ratio of the potassium hydroxide and sodium hydroxide, which is range).
The surfactant is trimethyl cetyl ammonium bromide.
The mass ratio of the highly basic and water is 10:(1 ~ 5), the mass ratio of surfactant and water is 0.72:(1 ~ 5), it is single
The mass ratio of matter copper and vulcanized sodium is 2:(1 ~ 15), the mass ratio of elemental copper and water is 0.4:(1 ~ 5), the volume of hydrazine hydrate and water
Than for 0.05:(1 ~ 5).
The additive amount of the deionized water by elemental copper, salt can react sufficiently on the basis of, water, which is not added, cannot get powder product,
Add the more voluminous object of water more, but water is added excessively to obtain that product morphology tends to particle or pattern is uneven；
Sealing is the evaporation of moisture in order to prevent to ensure to react more abundant, improves yield.
Preferably, drying temperature is 30 ~ 80 DEG C；It can ensure that the yield, product morphology and stability of product；
Preferably, elemental copper is copper sheet.
The average grain diameter of the cuprous sulfide nano flower is 700 nm ~ 1.9 μm, forms the average grain of the nanometer sheet of nano flower
Diameter is 350 ~ 600nm；
The molecular formula of cuprous sulfide nano flower is Cu7.2S4；
The beneficial effects of the present invention are:
(1) present invention is prepared in a mild condition using highly basic, surfactant, elemental copper, hydrazine hydrate, salt and water as raw material
Cuprous sulfide nano flower, the synthesis temperature of the technique is low, pressure is low, yield is high, product morphology is regular and reproducible；
(2) cuprous sulfide nano flower of the present invention has hierarchical structure and cupric defect, can be applicable to photochemical catalyst, solar-electricity
The fields such as pond, electrochemical energy storing device and sensor；
(3) the method for the present invention is easy to operate, and preparation process is easy to control, and is suitable for industrialized production, low production cost and ring
It protects.
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of 1 cuprous sulfide nano flower of embodiment；
Fig. 2 is the scanning electron microscope (SEM) photograph of 1 cuprous sulfide nano flower of embodiment；
Fig. 3 is the scanning electron microscope (SEM) photograph of 2 cuprous sulfide nano flower of embodiment；
Fig. 4 is the scanning electron microscope (SEM) photograph of 3 cuprous sulfide nano flower of embodiment；
Fig. 5 is the scanning electron microscope (SEM) photograph of 4 cuprous sulfide nano flower of embodiment；
Fig. 6 is the scanning electron microscope (SEM) photograph of 5 cuprous sulfide nano flower of embodiment；
Fig. 7 is the scanning electron microscope (SEM) photograph of 6 cuprous sulfide nano flower of embodiment；
Fig. 8 is the scanning electron microscope (SEM) photograph of 7 cuprous sulfide nano flower of embodiment.
Specific embodiment
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
A kind of embodiment 1: preparation method of the cuprous sulfide nano flower of cupric defect, the specific steps are as follows:
By highly basic (the compound alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl cetyl ammonium bromide CTAB),
Elemental copper (copper sheet), hydrazine hydrate, nine water vulcanized sodium are uniformly mixed with deionized water and are sealed in polytetrafluoroethylcontainer container, will gather
Tetrafluoroethene container be placed in heating equipment constant-speed heating to temperature be 200 DEG C and isothermal reaction for 24 hours, after being cooled to room temperature, from
Heart separation, removes supernatant liquor, uses dehydrated alcohol and deionized water to wash to cleaning solution as neutrality, being placed in temperature is 30 DEG C of items
Cuprous sulfide nano flower is drying to obtain under part；Wherein the mass ratio of potassium hydroxide and sodium hydroxide is 5.65:4.35, highly basic (hydrogen
The compound alkali of potassium oxide and sodium hydroxide) it with the mass ratio of water is 10:1, surfactant (trimethyl cetyl ammonium bromide
It CTAB) is 0.72:1 with the mass ratio of water, the mass ratio of elemental copper and vulcanized sodium is 2:1, and the mass ratio of elemental copper and water is
The volume ratio of 0.4:1, hydrazine hydrate and water is 0.05:1；
The X ray diffracting spectrum of the present embodiment cuprous sulfide nano flower is shown in Fig. 1, from fig. 1, it can be seen that product crystallinity is good, and it
With Cu7.2S4PDF#24-0061 card matching, illustrate that products therefrom is the cuprous sulfide Cu of cupric defect7.2S4, this outer width
The nanometer sheet thickness that half-peak breadth embodies composition nano flower is thin, this is consistent with scanning electron microscopic picture；
The scanning electron microscope (SEM) photograph of the present embodiment cuprous sulfide nano flower is shown in Fig. 2, and as can be seen from Figure 2, which is made of nanometer sheet
Nano flower, the average grain diameter of nano flower are 800 nm or so, and the average grain diameter for forming the nanometer sheet of nano flower is 400 nm or so,
Whole pattern is uniform.
A kind of embodiment 2: preparation method of the cuprous sulfide nano flower of cupric defect, the specific steps are as follows:
By highly basic (the compound alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl cetyl ammonium bromide CTAB),
Elemental copper (copper sheet), hydrazine hydrate, nine water vulcanized sodium are uniformly mixed with deionized water and are sealed in polytetrafluoroethylcontainer container, will gather
Tetrafluoroethene container be placed in heating equipment constant-speed heating to temperature be 200 DEG C and isothermal reaction for 24 hours, after being cooled to room temperature, from
Heart separation, removes supernatant liquor, uses dehydrated alcohol and deionized water to wash to cleaning solution as neutrality, being placed in temperature is 40 DEG C of items
Cuprous sulfide nano flower is drying to obtain under part；Wherein the mass ratio of potassium hydroxide and sodium hydroxide is 5.65:4.35, highly basic (hydrogen
The compound alkali of potassium oxide and sodium hydroxide) it with the mass ratio of water is 10:3, surfactant (trimethyl cetyl ammonium bromide
It CTAB) is 0.72:3 with the mass ratio of water, the mass ratio of elemental copper and vulcanized sodium is 2:1, and the mass ratio of elemental copper and water is
The volume ratio of 0.4:3, hydrazine hydrate and water is 0.05:3；
The scanning electron microscope (SEM) photograph of the present embodiment cuprous sulfide nano flower is shown in Fig. 3, and as can be seen from Figure 3, which is made of nanometer sheet
Nano flower, the average grain diameter of nano flower are 1.2 μm or so, and the average grain diameter for forming the nanometer sheet of nano flower is 600 nm or so,
Whole pattern is uniform.
A kind of embodiment 3: preparation method of the cuprous sulfide nano flower of cupric defect, the specific steps are as follows:
By highly basic (the compound alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl cetyl ammonium bromide CTAB),
Elemental copper (copper sheet), hydrazine hydrate, nine water vulcanized sodium are uniformly mixed with deionized water and are sealed in polytetrafluoroethylcontainer container, will gather
Tetrafluoroethene container be placed in heating equipment constant-speed heating to temperature be 200 DEG C and isothermal reaction for 24 hours, after being cooled to room temperature, from
Heart separation, removes supernatant liquor, uses dehydrated alcohol and deionized water to wash to cleaning solution as neutrality, being placed in temperature is 50 DEG C of items
Cuprous sulfide nano flower is drying to obtain under part；Wherein the mass ratio of potassium hydroxide and sodium hydroxide is 2:1, highly basic (potassium hydroxide
With the compound alkali of sodium hydroxide) it with the mass ratio of water is 2:1, surfactant (trimethyl cetyl ammonium bromide CTAB) and water
Mass ratio be 0.72:5, the mass ratio of elemental copper and vulcanized sodium is 2:1, and the mass ratio of elemental copper and water is 0.4:5, hydrazine hydrate
Volume ratio with water is 0.05:5；
The scanning electron microscope (SEM) photograph of the present embodiment cuprous sulfide nano flower is shown in Fig. 4, and as can be seen from Figure 4, which is made of nanometer sheet
Nano flower, the average grain diameter of nano flower are 900 nm or so, and the average grain diameter for forming the nanometer sheet of nano flower is 450 nm or so,
Whole pattern is more uniform.
A kind of embodiment 4: preparation method of the cuprous sulfide nano flower of cupric defect, the specific steps are as follows:
By highly basic (the compound alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl cetyl ammonium bromide CTAB),
Elemental copper (copper sheet), hydrazine hydrate, nine water vulcanized sodium are uniformly mixed with deionized water and are sealed in polytetrafluoroethylcontainer container, will gather
Tetrafluoroethene container be placed in heating equipment constant-speed heating to temperature be 200 DEG C and isothermal reaction for 24 hours, after being cooled to room temperature, from
Heart separation, removes supernatant liquor, uses dehydrated alcohol and deionized water to wash to cleaning solution as neutrality, being placed in temperature is 60 DEG C of items
Cuprous sulfide nano flower is drying to obtain under part；Wherein the mass ratio of potassium hydroxide and sodium hydroxide is 1:1, highly basic (potassium hydroxide
With the compound alkali of sodium hydroxide) with the mass ratio of water be 10:1, surfactant (trimethyl cetyl ammonium bromide CTAB) with
The mass ratio of water is 0.72:1, and the mass ratio of elemental copper and vulcanized sodium is 2:15, and the mass ratio of elemental copper and water is 0.4:1, water
The volume ratio for closing hydrazine and water is 0.05:1；
The scanning electron microscope (SEM) photograph of the present embodiment cuprous sulfide nano flower is shown in Fig. 5, and as can be seen from Figure 5, which is made of nanometer sheet
Nano flower, the average grain diameter of nano flower are 700 nm or so, and the average grain diameter for forming the nanometer sheet of nano flower is 350 nm or so,
Whole pattern is more uniform.
A kind of embodiment 5: preparation method of the cuprous sulfide nano flower of cupric defect, the specific steps are as follows:
By highly basic (the compound alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl cetyl ammonium bromide CTAB),
Elemental copper (copper sheet), hydrazine hydrate, nine water vulcanized sodium are uniformly mixed with deionized water and are sealed in polytetrafluoroethylcontainer container, will gather
It is 200 DEG C and isothermal reaction 20h, after being cooled to room temperature that tetrafluoroethene container, which is placed in constant-speed heating to temperature in heating equipment, from
Heart separation, removes supernatant liquor, uses dehydrated alcohol and deionized water to wash to cleaning solution as neutrality, being placed in temperature is 80 DEG C of items
Cuprous sulfide nano flower is drying to obtain under part；Wherein the mass ratio of potassium hydroxide and sodium hydroxide is 2:1.3, highly basic (hydroxide
The compound alkali of potassium and sodium hydroxide) it with the mass ratio of water is 10:1, surfactant (trimethyl cetyl ammonium bromide CTAB)
It is 0.72:1 with the mass ratio of water, the mass ratio of elemental copper and vulcanized sodium is 1:1, and the mass ratio of elemental copper and water is 0.4:1, water
The volume ratio for closing hydrazine and water is 0.05:1；
The scanning electron microscope (SEM) photograph of the present embodiment cuprous sulfide nano flower is shown in Fig. 6, as can be seen from Figure 6, the present embodiment cuprous sulfide nano flower
Average grain diameter be 1.5 μm or so, whole pattern is more uniform.
A kind of embodiment 6: preparation method of the cuprous sulfide nano flower of cupric defect, the specific steps are as follows:
By highly basic (the compound alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl cetyl ammonium bromide CTAB),
Elemental copper (copper sheet), hydrazine hydrate, nine water vulcanized sodium are uniformly mixed with deionized water and are sealed in polytetrafluoroethylcontainer container, will gather
Tetrafluoroethene container be placed in heating equipment constant-speed heating to temperature be 190 DEG C and isothermal reaction for 24 hours, after being cooled to room temperature, from
Heart separation, removes supernatant liquor, uses dehydrated alcohol and deionized water to wash to cleaning solution as neutrality, being placed in temperature is 30 DEG C of items
Cuprous sulfide nano flower is drying to obtain under part；Wherein the mass ratio of potassium hydroxide and sodium hydroxide is 2:1.6, highly basic (hydroxide
The compound alkali of potassium and sodium hydroxide) with the mass ratio of water be 5:1, surfactant (trimethyl cetyl ammonium bromide CTAB) with
The mass ratio of water is 0.72:2, and the mass ratio of elemental copper and vulcanized sodium is 2:7, and the mass ratio of elemental copper and water is 0.2:1, hydration
The volume ratio of hydrazine and water is 0.05:2；
The scanning electron microscope (SEM) photograph of the present embodiment cuprous sulfide nano flower is shown in Fig. 7, as can be seen from Figure 7, the present embodiment cuprous sulfide nano flower
Average grain diameter be 1.7 μm or so, whole pattern is more uniform.
A kind of embodiment 7: preparation method of the cuprous sulfide nano flower of cupric defect, the specific steps are as follows:
By highly basic (the compound alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl cetyl ammonium bromide CTAB),
Elemental copper (copper sheet), hydrazine hydrate, nine water vulcanized sodium are uniformly mixed with deionized water and are sealed in polytetrafluoroethylcontainer container, will gather
It is 220 DEG C and isothermal reaction 22h, after being cooled to room temperature that tetrafluoroethene container, which is placed in constant-speed heating to temperature in heating equipment, from
Heart separation, removes supernatant liquor, uses dehydrated alcohol and deionized water to wash to cleaning solution as neutrality, being placed in temperature is 50 DEG C of items
Cuprous sulfide nano flower is drying to obtain under part；Wherein the mass ratio of potassium hydroxide and sodium hydroxide is 1:1, highly basic (potassium hydroxide
With the compound alkali of sodium hydroxide) with the mass ratio of water be 10:1, surfactant (trimethyl cetyl ammonium bromide CTAB) with
The mass ratio of water is 0.72:1, and the mass ratio of elemental copper and vulcanized sodium is 2:15, and the mass ratio of elemental copper and water is 0.4:1, water
The volume ratio for closing hydrazine and water is 0.05:1；
The scanning electron microscope (SEM) photograph of the present embodiment cuprous sulfide nano flower is shown in Fig. 8, as it can be observed in the picture that the present embodiment cuprous sulfide nano flower
Average grain diameter be 1.9 μm or so, whole pattern is more uniform.
Claims (5)
1. a kind of preparation method of the cuprous sulfide nano flower of cupric defect, which is characterized in that specific step is as follows:
Highly basic, surfactant, elemental copper, hydrazine hydrate, vulcanized sodium and water are uniformly mixed, are at the uniform velocity warming up under air-proof condition
Temperature is 180 ~ 220 DEG C and 22 ~ 24 h of isothermal reaction and obtains reaction system；Reaction system is cooled to room temperature, and is centrifugated, removal
Supernatant liquor, then adopt be washed with deionized to cleaning solution for neutrality, be drying to obtain the cuprous sulfide nano flower of cupric defect.
2. the preparation method of the cuprous sulfide nano flower of cupric defect according to claim 1, it is characterised in that: highly basic is served as reasons
The compound alkali of potassium hydroxide and sodium hydroxide composition.
3. the preparation method of the cuprous sulfide nano flower of cupric defect according to claim 2, it is characterised in that: potassium hydroxide
Mass ratio with sodium hydroxide is 2:(1 ~ 2).
4. the preparation method of the cuprous sulfide nano flower of cupric defect according to claim 1, it is characterised in that: surface-active
Agent is trimethyl cetyl ammonium bromide.
5. the preparation method of the cuprous sulfide nano flower of cupric defect according to claim 1, it is characterised in that: highly basic and water
Mass ratio be 10:(1 ~ 5), the mass ratio of surfactant and water is 0.72:(1 ~ 5), the mass ratio of elemental copper and vulcanized sodium
For 2:(1 ~ 15), the mass ratio of elemental copper and water is 0.4:(1 ~ 5), the volume ratio of hydrazine hydrate and water is 0.05:(1 ~ 5).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110683571A (en) * | 2019-09-27 | 2020-01-14 | 中国科学院合肥物质科学研究院 | Preparation method of flower-shaped cuprous sulfide micron particles |
| CN112536022A (en) * | 2020-11-22 | 2021-03-23 | 重庆交通大学 | CQDS/Cu2Preparation method of S nanoflower |
| CN112978798A (en) * | 2021-02-02 | 2021-06-18 | 昆明理工大学 | Method and device for preparing molybdenum oxide nano material with adjustable phase, shape and size |
| CN113394414A (en) * | 2021-06-16 | 2021-09-14 | 福州大学 | Construction of flower-core type S-doped manganese-copper electrocatalyst based on metal polyphenol modified sodium alginate/nano-cellulose composite aerogel |
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| CN113394414A (en) * | 2021-06-16 | 2021-09-14 | 福州大学 | Construction of flower-core type S-doped manganese-copper electrocatalyst based on metal polyphenol modified sodium alginate/nano-cellulose composite aerogel |
| CN113788493A (en) * | 2021-09-18 | 2021-12-14 | 安徽师范大学 | Microcapsule composite material, preparation method thereof and application thereof in lithium ion battery |
| CN113788493B (en) * | 2021-09-18 | 2023-09-01 | 乌海瑞森新能源材料有限公司 | Microcapsule composite material, preparation method thereof and application thereof in lithium ion battery |
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