CN106732668A - A kind of hydrothermal preparing process of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials - Google Patents
A kind of hydrothermal preparing process of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials Download PDFInfo
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- flower
- cupric oxide
- molybdenum bisuphide
- oxide composite
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 85
- 229960004643 cupric oxide Drugs 0.000 title claims abstract description 66
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000011733 molybdenum Substances 0.000 title claims abstract description 65
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 62
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000008569 process Effects 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 9
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 6
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 13
- 238000013019 agitation Methods 0.000 claims description 12
- 239000007795 chemical reaction product Substances 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 239000012085 test solution Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 10
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 4
- 239000005864 Sulphur Substances 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 229910052744 lithium Inorganic materials 0.000 abstract 1
- 150000002751 molybdenum Chemical class 0.000 abstract 1
- 238000005406 washing Methods 0.000 description 12
- 239000003643 water by type Substances 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 230000008859 change Effects 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 6
- 230000010355 oscillation Effects 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- 206010013786 Dry skin Diseases 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 5
- -1 lithium (sodium) ion Chemical class 0.000 description 5
- 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 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- VVNXEADCOVSAER-UHFFFAOYSA-N lithium sodium Chemical compound [Li].[Na] VVNXEADCOVSAER-UHFFFAOYSA-N 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 229910001948 sodium oxide Inorganic materials 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000003836 solid-state method Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 229910002064 alloy oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/39—
Abstract
The invention discloses a kind of hydrothermal preparing process of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials, using Sodium Molybdate Dihydrate as molybdenum source, used as sulphur source, in 220 degrees Celsius of reaction temperature, the reaction time is synthesis of carbon/molybdenum disulfide nano material under the hydrothermal condition of 24 hours to thiocarbamide.And with this molybdenum bisuphide as masterplate, different amounts of water copper acetate and NaOH are added by priority, and a certain amount of CTAB, in 100 degrees Celsius of reaction temperature, reaction time is that the hydrothermal condition of 10 hours goes down to synthesize flower-shaped molybdenum bisuphide/cupric oxide composite nano materials, and the structure that synthesized material is inlayed because its is flower-shaped has preferably application on the field such as photocatalysis and lithium sode cell negative material.
Description
Technical field
The present invention relates to a kind of preparation method of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials, belong to nano combined
Field of material preparation.
Background technology
Molybdenum bisuphide is a kind of typical transient metal sulfide, and body phase shows layer structure, is that indirect band gap is partly led
Body, energy gap is 1.29 electron-volts；Its two-dimentional single layer structure is direct band-gap semicondictor, and energy gap is about 1.8 electronics
Volt；The application of molybdenum bisuphide widely, is mainly used in photoelectrocatalysis, the electrode material of rechargeable battery, sensor etc.
Field, and due to its unique layer structure, industrially it is also commonly used as lubricant.Cupric oxide is a kind of semiconductor alloy
Oxide, its energy gap is about 1.7 electron-volts, and spectral absorption is concentrated mainly on visible-range, therefore can be applied to light
The application of the aspects such as electrical part, photoelectrocatalysis, energy storage and conversion, various kinds of sensors, and with low toxicity, it is stable, efficiently, into
This low advantage.
Cupric oxide nano structural load is formed into nano composite material in certain condition on flower-shaped curing molybdenum sheet surface
Under can show cooperative effect.In photocatalysis field, the photocatalytic activity of single metal oxide is relatively low, main cause be by
Cannot in time be separated in its photo-generated carrier for producing, cause the light induced electron for producing and hole to be quickly combined again in its inside,
In it is participated in catalytic reaction, and due to single metal oxide in the course of reaction of synthesis inevitably
There occurs a certain degree of reunion so that the active reaction sites quantity on surface is reduced, so as to cause the effect of its photo-generated carrier
Rate declines, and above-mentioned two reason causes catalytic rate reduction in single metal oxide (such as cupric oxide) light-catalyzed reaction.Make
The molybdenum bisuphide synthesized with hydro-thermal method has adjustable this key factor of pattern, is carried on when using cupric oxide as light absorbent
When the surface and edge of molybdenum bisuphide, the separation and migration of photo-generated carrier can not only be effectively lifted, reduce photoproduction load
The recombination rate again of son is flowed, and the scope of spectral absorption can be increased, therefore construct flower-shaped molybdenum bisuphide/cupric oxide composite Nano
Material is conducive to improving its photocatalysis performance.In energy storage device field, such as the negative material of lithium (sodium) ion battery, flower
Shape molybdenum bisuphide/cupric oxide composite nano materials are interacted and big interlamellar spacing due to its weaker Van der Waals, are increased
The storage density of lithium (sodium) ion；Simultaneously as the support effect of cupric oxide and the layer coupling formed with molybdenum bisuphide are made
With the cyclical stability in lithium (sodium) battery charge and discharge process can be improved.Further, since the cupric oxide of sheet with it is flower-shaped
There is larger interracial contact in the two-dimensional nano hetero-junctions that molybdenum bisuphide is constituted, this causes that they can have in photocatalytic process
Effect promotes separation, transmission and the raising of active reaction sites of carrier；Also so that they are in energy storage device application
The efficiency of energy storage density and lifting electric charge transmission can be improved.Therefore, flower-shaped molybdenum bisuphide/cupric oxide composite nano materials have
Relatively broad application prospect.
The method for preparing composite nano materials at present has a lot, including：High temperature solid-state method, sol-gel process, chemical precipitation
Method, hydro-thermal method etc..High temperature solid-state method refers at high temperature between solid interface by contact, reaction, nucleation, crystal growth reaction
A kind of method of product is generated, with low cost, yield is big, the features such as preparation process is simple；Its shortcoming includes that energy consumption is big, sample
Easily reunite, impurity etc. is easily mixed during the course of the reaction.The process of sol-gel process is by ester type compound or metal alkoxide
It is dissolved in organic solvent, forms uniform solution, be subsequently adding other components, reaction at a certain temperature forms gel, finally
Sample is made through dried process, its advantage is simple reactions steps, and uniformity is good, and the temperature needed for reaction is relatively low；It has the disadvantage
Expensive starting materials of reaction and part is poisonous, the time of reaction is more long.Chemical precipitation method refers to that precipitating reagent is utilized under solution state
By sample pellet, sample drying or calcination process are obtained corresponding sample again afterwards, used in the reaction of its advantage
Instrument is simple, is adapted to prepare sample on a large scale, has the disadvantage to be difficult to control to sample quality, and uniformity is more low.Hydro-thermal method refers to
Sample goes to create an environment for HTHP in closed container by heating, crystal is dissolved during the course of the reaction
This process is recrystallized, preparing sample by hydro-thermal method has good dispersion, the features such as the crystallinity of crystal is high, the method
It is middle low temperature with reaction temperature, equipment is simple, the features such as easy to operate.
The content of the invention
In order to solve above-mentioned the deficiencies in the prior art, the present invention provides a kind of flower-shaped molybdenum bisuphide/cupric oxide composite Nano
The hydrothermal preparing process of material, good crystallinity is prepared using hydro-thermal method, uniformity is high and microscopic appearance be flower-shaped molybdenum bisuphide/
Cupric oxide composite nano materials, this composite can have preferable photoelectric transformation efficiency and as lithium (sodium) electricity as photochemical catalyst
The negative material in pond possesses memory capacity and cyclical stability high.
The technical solution adopted by the present invention step is as follows：
The first step：Molybdenum disulfide nano material powder is added in deionized water, ultrasonic vibration 30 minutes is mixed
Thing A；
Second step：One water copper acetate is dissolved into mixture A, mixture B is obtained；
3rd step：NaOH is dissolved in deionized water, solution C is obtained；
4th step：By in solution C addition mixture B, stir 20 minutes, obtain mixture D；
5th step：By in CTAB powder addition mixture D, stir 10 minutes, obtain mixture E；
6th step：Mixture E is transferred in the polytetrafluoroethyllining lining of stainless steel autoclave, at 100 degrees Celsius
Reaction obtains mixed reaction product F in 10 hours, after stainless steel autoclave naturally cools to room temperature, first removes upper strata clear
, then be transferred to mixed reaction product F in beaker by liquid；
7th step：Mixed reaction product F is cleaned multiple times using deionized water, until when the pH of scrub raffinate is for neutrality, obtaining
To aqueous flower-shaped molybdenum bisuphide/cupric oxide composite nano materials；
8th step：Aqueous flower-shaped molybdenum bisuphide/cupric oxide composite nano materials are put into vacuum drying chamber, are taken the photograph 60
Dried 24 hours under family name's degree, obtain dry flower-shaped molybdenum bisuphide/cupric oxide composite nano materials.
The preparation method of above-mentioned molybdenum disulfide nano material is：
The first step：Deionized water dissolving Sodium Molybdate Dihydrate is used, solution G is obtained；
Second step：Thiocarbamide is dissolved into solution G, Solution H is obtained；
3rd step：During hydrochloric acid dropwise to instill Solution H, while magnetic agitation, using the pH value of pH meter test solution H, directly
PH value to Solution H reaches 2；
4th step：Solution H is continued into magnetic agitation 20 minutes；
5th step：Solution H is transferred in the polytetrafluoroethyllining lining of stainless steel autoclave, it is anti-at 220 degrees Celsius
Answer 24 hours and obtain mixed reaction product I, after stainless steel autoclave naturally cools to room temperature, first remove supernatant liquor,
Then mixed reaction product I is transferred in beaker；
6th step：Mixed reaction product I is respectively washed using deionized water and ethanol tri- times, staticly settle removing supernatant
The molybdenum disulfide nano material containing ethanol is obtained afterwards；
7th step：Molybdenum disulfide nano material containing ethanol is put into vacuum drying chamber, 24 are dried at 60 c
Hour, obtain dry molybdenum disulfide nano material.
Above-mentioned molybdenum disulfide nano material and the mass ratio of a water copper acetate are 0.4~4.
An above-mentioned water copper acetate is 1: 20 with the mol ratio of NaOH.
The beneficial effects of the invention are as follows：
1. the nanostructured being compounded to form using molybdenum bisuphide and cupric oxide, can avoid cupric oxide nano structure in reaction
During reunite, it is to avoid compound be subject to photoetch, be conducive to improving flower-shaped molybdenum bisuphide/cupric oxide composite nanostructure in light
Carrier separation, transmission in catalytic reaction process, reduce the stability of recombination rate again and catalyst after the separation of carrier；
At the same time as the negative material of lithium (sodium) ion battery, with energy storage density and cyclical stability higher.
2. the flower-shaped molybdenum bisuphide/cupric oxide composite nano materials sample for being prepared using hydro-thermal method has good dispersion, steady
The features such as determining, and process is simple, favorable repeatability.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of molybdenum disulfide nano material powder.
Fig. 2 is the XRD spectrum of the flower-shaped molybdenum bisuphide/cupric oxide composite nano materials of gained of embodiment 1,2,3,4,5.
Fig. 3 is the stereoscan photograph and transmission electricity of the flower-shaped molybdenum bisuphide/cupric oxide composite nano materials of gained of embodiment 1
Mirror photo.
Fig. 4 is the stereoscan photograph of the flower-shaped molybdenum bisuphide/cupric oxide composite nano materials of gained of embodiment 2.
Fig. 5 is the stereoscan photograph of the flower-shaped molybdenum bisuphide/cupric oxide composite nano materials of gained of embodiment 3.
Fig. 6 is the stereoscan photograph of the flower-shaped molybdenum bisuphide/cupric oxide composite nano materials of gained of embodiment 4.
Fig. 7 is the stereoscan photograph of the flower-shaped molybdenum bisuphide/cupric oxide composite nano materials of gained of embodiment 5.
Specific embodiment
Flower-shaped molybdenum bisuphide/cupric oxide composite nano materials are prepared, its key step is divided into two steps, including molybdenum bisuphide is received
The preparation of rice material and the preparation of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials.
The preparation method of molybdenum disulfide nano material：0.6 gram of Sodium Molybdate Dihydrate is dissolved into 60 milliliters of deionized water,
2.4 grams of thiocarbamides are dissolved into above-mentioned solution again, uniform solution is obtained using magnetic agitation, hydrochloric acid dropwise instilled solution and is protected simultaneously
Stirring is held, after solution ph reaches 2, continues magnetic agitation solution 20 minutes, resulting solution is transferred to 100 milliliters of stainless steels
The polytetrafluoroethyllining lining of autoclave, 24 hours are incubated using air dry oven at 220 degrees Celsius；Sample is naturally cooled to
Taken out after room temperature, the supernatant liquor of the product after terminating is heated in first removal, is washed respectively three times with deionized water and ethanol, is obtained
Wet solid product, dries 24 hours under finally putting it into 60 degrees Celsius, obtains the powder of molybdenum disulfide nano material.Fig. 1
It is the stereoscan photograph of synthesized molybdenum disulfide nano material powder.
The preparation method of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials：By 0.35 gram of dry molybdenum disulfide nano
Material powder is distributed in 45 ml deionized waters, sonic oscillation 30 minutes, then by a water copper acetate (molybdenum disulfide nano material
Material and the mass ratio of a water copper acetate for 0.4~4) be dissolved into the molybdenum disulfide nano material suspension of gained；By hydrogen-oxygen
Change sodium (a water copper acetate is 1: 20 with the mol ratio of NaOH) and be dissolved in 25 ml deionized waters, a water second is added into afterwards
In the mixture of sour copper and molybdenum disulfide nano material, stir 20 minutes, 0.13 gram of CTAB is added into mixture, magnetic agitation 10
Minute, mixture is then transferred to 100 milliliters of polytetrafluoroethyllining linings of stainless steel autoclave, use air dry oven
It is interior to be incubated 10 hours under 100 degrees Celsius, it is naturally cooled to room temperature afterwards, sample is taken out, use deionized water water washing
Sample is multiple, until when the pH of the waste liquid after washing is for neutrality, solid is sent into vacuum drying chamber under conditions of vacuum with 60
Degree Celsius drying 24 hours, has obtained flower-shaped molybdenum bisuphide/cupric oxide composite nano materials afterwards.
Molybdenum bisuphide and cupric oxide mass ratio in the flower-shaped molybdenum bisuphide of embodiment 1-/cupric oxide composite nano materials are 1:
1
0.35 gram of dry molybdenum disulfide nano material powder is distributed in 45 ml deionized waters, 30 points of sonic oscillation
, then be dissolved into 0.875 gram of one water copper acetate in the molybdenum disulfide nano material suspension of gained by clock；By 3.5 grams of hydroxides
Sodium is dissolved in 25 ml deionized waters, is added into afterwards in the mixture of a water copper acetate and molybdenum disulfide nano material, stirring
20 minutes, 0.13 gram of CTAB is added into mixture, then mixture is transferred to 100 milliliters of stainless steels by magnetic agitation 10 minutes
The polytetrafluoroethyllining lining of autoclave, 10 hours are incubated using in air dry oven under 100 degrees Celsius, and it is made afterwards certainly
Room temperature is so cooled to, sample is taken out, until the pH of the waste liquid after washing is neutrality using deionized water water washing sample repeatedly
When, solid is sent into vacuum drying chamber under conditions of vacuum with 60 degrees Celsius of dryings 24 hours, flower-shaped two sulphur has been obtained afterwards
Change molybdenum/cupric oxide composite nano materials.
XRD spectrum in Fig. 2 proves that the product of the synthesis of embodiment 1 is molybdenum bisuphide and the compound of cupric oxide.Fig. 3 is colored
The stereoscan photograph of shape molybdenum bisuphide/cupric oxide composite nano materials, illustration shows partial structurtes in scanning electron microscope (SEM) photograph
Transmission electron microscope photo, it can be seen that the cupric oxide of nanometer forms composite construction in being embedded in flower-shaped molybdenum disulfide nano material.
Molybdenum bisuphide and cupric oxide mass ratio in the flower-shaped molybdenum bisuphide of embodiment 2-/cupric oxide composite nano materials are 2:
1
0.35 gram of dry molybdenum disulfide nano material powder is distributed in 45 ml deionized waters, 30 points of sonic oscillation
, then be dissolved into 0.4375 gram of one water copper acetate in the molybdenum disulfide nano material suspension of gained by clock；By 1.75 grams of hydrogen-oxygens
Change sodium and be dissolved in 25 ml deionized waters, be added into afterwards in the mixture of a water copper acetate and molybdenum disulfide nano material, stir
Mix 20 minutes, 0.13 gram of CTAB added into mixture, magnetic agitation 10 minutes, then by mixture be transferred to 100 milliliters it is stainless
The polytetrafluoroethyllining lining of steel autoclave, 10 hours are incubated using in air dry oven under 100 degrees Celsius, and it is made afterwards
Room temperature is naturally cooled to, sample is taken out, until the pH of the waste liquid after washing is neutrality using deionized water water washing sample repeatedly
When, solid is sent into vacuum drying chamber under conditions of vacuum with 60 degrees Celsius of dryings 24 hours, flower-shaped two sulphur has been obtained afterwards
Change molybdenum/cupric oxide composite nano materials.
XRD spectrum in Fig. 2 prove embodiment it is 2-in-1 into product be molybdenum bisuphide and the compound of cupric oxide.Fig. 4 is colored
The stereoscan photograph of shape molybdenum bisuphide/cupric oxide composite nano materials.
Molybdenum bisuphide and cupric oxide mass ratio in the flower-shaped molybdenum bisuphide of embodiment 3-/cupric oxide composite nano materials are 3:
1
0.35 gram of dry molybdenum disulfide nano material powder is distributed in 45 ml deionized waters, 30 points of sonic oscillation
, then be dissolved into 0.2918 gram of one water copper acetate in the molybdenum disulfide nano material suspension of gained by clock；By 1.1672 grams of hydrogen
Sodium oxide molybdena is dissolved in 25 ml deionized waters, is added into afterwards in the mixture of a water copper acetate and molybdenum disulfide nano material,
Stirring 20 minutes, mixture is added by 0.13 gram of CTAB, and then mixture is transferred to 100 milliliters not by magnetic agitation 10 minutes
The polytetrafluoroethyllining lining of rust steel autoclave, 10 hours are incubated using in air dry oven under 100 degrees Celsius, are made afterwards
It naturally cools to room temperature, takes out sample, until during the pH of the waste liquid after washing is using deionized water water washing sample repeatedly
Property when, solid is sent into vacuum drying chamber under conditions of vacuum with 60 degrees Celsius of dryings 24 hours, flower-shaped two have been obtained afterwards
Molybdenum sulfide/cupric oxide composite nano materials.
XRD spectrum in Fig. 2 proves that the product of the synthesis of embodiment 3 is molybdenum bisuphide and the compound of cupric oxide.Fig. 5 is colored
The stereoscan photograph of shape molybdenum bisuphide/cupric oxide composite nano materials.
Molybdenum bisuphide and cupric oxide mass ratio in the flower-shaped molybdenum bisuphide of embodiment 4-/cupric oxide composite nano materials are 6:
1
0.35 gram of dry molybdenum disulfide nano material powder is distributed in 45 ml deionized waters, 30 points of sonic oscillation
, then be dissolved into 0.1459 gram of one water copper acetate in the molybdenum disulfide nano material suspension of gained by clock；By 0.5833 gram of hydrogen
Sodium oxide molybdena is dissolved in 25 ml deionized waters, is added into afterwards in the mixture of a water copper acetate and molybdenum disulfide nano material,
Stirring 20 minutes, mixture is added by 0.13 gram of CTAB, and then mixture is transferred to 100 milliliters not by magnetic agitation 10 minutes
The polytetrafluoroethyllining lining of rust steel autoclave, 10 hours are incubated using in air dry oven under 100 degrees Celsius, are made afterwards
It naturally cools to room temperature, takes out sample, until during the pH of the waste liquid after washing is using deionized water water washing sample repeatedly
Property when, solid is sent into vacuum drying chamber under conditions of vacuum with 60 degrees Celsius of dryings 24 hours, flower-shaped two have been obtained afterwards
Molybdenum sulfide/cupric oxide composite nano materials.
XRD spectrum in Fig. 2 proves that the product of the synthesis of embodiment 4 is molybdenum bisuphide and the compound of cupric oxide.Fig. 6 is colored
The stereoscan photograph of shape molybdenum bisuphide/cupric oxide composite nano materials.
Molybdenum bisuphide and cupric oxide mass ratio in the flower-shaped molybdenum bisuphide of embodiment 5-/cupric oxide composite nano materials are 10
∶1
0.35 gram of dry molybdenum disulfide nano material powder is distributed in 45 ml deionized waters, 30 points of sonic oscillation
, then be dissolved into 0.0875 gram of one water copper acetate in the molybdenum disulfide nano material suspension of gained by clock；By 0.35 gram of hydrogen-oxygen
Change sodium and be dissolved in 25 ml deionized waters, be added into afterwards in the mixture of a water copper acetate and molybdenum disulfide nano material, stir
Mix 20 minutes, 0.13 gram of CTAB added into mixture, magnetic agitation 10 minutes, then by mixture be transferred to 100 milliliters it is stainless
The polytetrafluoroethyllining lining of steel autoclave, 10 hours are incubated using in air dry oven under 100 degrees Celsius, and it is made afterwards
Room temperature is naturally cooled to, sample is taken out, until the pH of the waste liquid after washing is neutrality using deionized water water washing sample repeatedly
When, solid is sent into vacuum drying chamber under conditions of vacuum with 60 degrees Celsius of dryings 24 hours, flower-shaped two sulphur has been obtained afterwards
Change molybdenum/cupric oxide composite nano materials.
XRD spectrum in Fig. 2 proves that the product of the synthesis of embodiment 5 is molybdenum bisuphide and the compound of cupric oxide.Fig. 7 is colored
The stereoscan photograph of shape molybdenum bisuphide/cupric oxide composite nano materials.
Claims (4)
1. a kind of hydrothermal preparing process of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials, it is characterised in that：
The first step：Molybdenum disulfide nano material powder is added in deionized water, ultrasonic vibration 30 minutes obtains mixture A；
Second step：One water copper acetate is dissolved into mixture A, mixture B is obtained；
3rd step：NaOH is dissolved in deionized water, solution C is obtained；
4th step：By in solution C addition mixture B, stir 20 minutes, obtain mixture D；
5th step：By in CTAB powder addition mixture D, stir 10 minutes, obtain mixture E；
6th step：Mixture E is transferred in the polytetrafluoroethyllining lining of stainless steel autoclave, in 100 degrees Celsius of reactions
Obtain mixed reaction product F within 10 hours, after stainless steel autoclave naturally cools to room temperature, first remove supernatant liquor, with
Mixed reaction product F is transferred in beaker afterwards；
7th step：Mixed reaction product F is cleaned multiple times using deionized water, until when the pH of scrub raffinate is for neutrality, being contained
Flower-shaped molybdenum bisuphide/cupric oxide the composite nano materials of water；
8th step：Aqueous flower-shaped molybdenum bisuphide/cupric oxide composite nano materials are put into vacuum drying chamber, at 60 degrees Celsius
Lower drying 24 hours, obtains dry flower-shaped molybdenum bisuphide/cupric oxide composite nano materials.
2. the hydrothermal preparing process of a kind of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials according to claim 1, its
The preparation method of molybdenum disulfide nano material described in feature is：
The first step：Deionized water dissolving Sodium Molybdate Dihydrate is used, solution G is obtained；
Second step：Thiocarbamide is dissolved into solution G, Solution H is obtained；
3rd step：During hydrochloric acid dropwise to instill Solution H, while magnetic agitation, uses the pH value of pH meter test solution H, Zhi Daorong
The pH value of liquid H reaches 2；
4th step：Solution H is continued into magnetic agitation 20 minutes；
5th step：Solution H is transferred in the polytetrafluoroethyllining lining of stainless steel autoclave, 24 are reacted at 220 degrees Celsius
Hour obtains mixed reaction product I, after stainless steel autoclave naturally cools to room temperature, first removes supernatant liquor, then
Mixed reaction product I is transferred in beaker；
6th step：Mixed reaction product I is respectively washed using deionized water and ethanol tri- times, obtained after staticly settling removing supernatant
To the molybdenum disulfide nano material containing ethanol；
7th step：Molybdenum disulfide nano material containing ethanol is put into vacuum drying chamber, is dried 24 hours at 60 c,
Obtain dry molybdenum disulfide nano material.
3. the hydrothermal preparing process of a kind of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials according to claim 1, its
The mass ratio of molybdenum disulfide nano material and a water copper acetate described in being characterised by is 0.4~4.
4. the hydrothermal preparing process of a kind of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials according to claim 1, its
A water copper acetate and the mol ratio of NaOH described in being characterised by are 1: 20.
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