CN107876068A - A kind of preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable - Google Patents
A kind of preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable Download PDFInfo
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- CN107876068A CN107876068A CN201710971830.2A CN201710971830A CN107876068A CN 107876068 A CN107876068 A CN 107876068A CN 201710971830 A CN201710971830 A CN 201710971830A CN 107876068 A CN107876068 A CN 107876068A
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- molybdenum disulfide
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 135
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 59
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 52
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000000463 material Substances 0.000 title claims abstract description 47
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 46
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000007306 functionalization reaction Methods 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 239000008187 granular material Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 57
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 26
- 229910052700 potassium Inorganic materials 0.000 claims description 26
- 239000011591 potassium Substances 0.000 claims description 26
- 238000003760 magnetic stirring Methods 0.000 claims description 16
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 16
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 16
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 16
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 13
- 239000012498 ultrapure water Substances 0.000 claims description 13
- 238000005119 centrifugation Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000010348 incorporation Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000000877 morphologic effect Effects 0.000 claims description 4
- 229910001868 water Inorganic materials 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 45
- 230000003197 catalytic effect Effects 0.000 abstract description 18
- 238000007254 oxidation reaction Methods 0.000 abstract description 13
- 230000003647 oxidation Effects 0.000 abstract description 12
- 239000003054 catalyst Substances 0.000 abstract description 9
- 239000002131 composite material Substances 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 238000001308 synthesis method Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 19
- 239000002086 nanomaterial Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- JRTYPQGPARWINR-UHFFFAOYSA-N palladium platinum Chemical compound [Pd].[Pt] JRTYPQGPARWINR-UHFFFAOYSA-N 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002840 Pt-MoS2 Inorganic materials 0.000 description 1
- CLBRCZAHAHECKY-UHFFFAOYSA-N [Co].[Pt] Chemical compound [Co].[Pt] CLBRCZAHAHECKY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000411 inducer Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002063 nanoring Substances 0.000 description 1
- PCLURTMBFDTLSK-UHFFFAOYSA-N nickel platinum Chemical compound [Ni].[Pt] PCLURTMBFDTLSK-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000001126 phototherapy Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000000015 thermotherapy Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
- 239000002023 wood Substances 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
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
- B01J35/19—Catalysts containing parts with different compositions
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation method of the platinum of morphology controllable palladium/molybdenum disulfide nano-composite material.In building-up process, change the ratio of platinum palladium presoma, one-step synthesis method has obtained the bimetallic functionalization molybdenum disulfide nano-composite material of different-shape, is changing ratio Pd:Pt=10:1、1:1、1:Synthesize to have obtained spherical, concave surface cubic block and flower-shaped platinum palladium duplex metal nano granule functionalization molybdenum disulfide nano-composite material when 5, three has catalytic activity as catalyst to the catalysis oxidation of methanol, and compared for activity of three kinds of catalyst to methanol catalytic oxidation.A kind of platinum palladium/molybdenum disulfide nano-composite material for morphology controllable that the present invention obtains successfully has prepared morphology controllable using simple, efficient one-step synthesis method, size is controllable, the controllable platinum palladium duplex metal nano granule functionalization molybdenum disulfide nano-composite material of component, the composite can be applied to the catalysis oxidation of methanol as catalyst.
Description
Technical field
The invention belongs to technical field of nano material and its application, is related to noble metal functionalization molybdenum disulfide nano composite wood
The preparation and application of material, more particularly to a kind of preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable and its
Using.
Background technology
Platinum is for being catalyzed various dye molecules (such as：Methanol, ethanol, formic acid) for be maximally effective electrochemical catalyst.
However, for pure platinum, however it remains some problems, as price is higher, cathode reaction dynamics is slow, is easy to CO poison
Property etc., these problems hinder the development of commercializing fuel cells.There is an urgent need to design preferably according to urging on the basis of platinum
Agent and the nano material for improving overall catalytic performance.At present, can be by controlling atomic level component, pattern and surface texture come
Strengthen the performance of its platinum.In addition, also part platinum component can be replaced by increasing low-cost metal, to strengthen platinum surface atom
Electronic structure, here it is the bimetallic composition described in us.So far, the bimetallic synthesized on the basis of platinum has：Platinum
Palladium, platinum nickel, platinum cobalt, platinum and platinoid.Wherein palladium and platinum due to identical face-centered cubic lattice, good compatibility and compared with
Small lattice mismatch rate (only 0.77%), so they are easy to the nano material for preparing single crystal structure.With this
Meanwhile palladium also has good catalytic performance, and price only accounts for the 40% of platinum.Therefore, the condition of catalytic performance is not being reduced
Under, palladium is as the best candidate for reducing material cost.
At present, the synthetic method of palladium platinum nano composite material has a lot, such as：The seed law, solvent-thermal method, electrochemical displacement
Method, co-reducing process etc., however, these method synthesis steps are more, it is necessary to which special synthetic technology, this causes synthesis to become one
Individual larger challenge.Although relevant one-step synthesis method, which prepares palladium platinum bimetal nano material, before document report.Example
Such as, Jiang et al. is prepared for many mesoporous palladium platinum duplex metal nano granules that have of different component by one-step method, this to urge
Agent goes out good electro catalytic activity to the oxidation performance of methanol.Li et al. has synthesized palladium platinum using quick step wet chemistry method
The nano-rings functionalization graphene composite of core and platinum shell, and it is anti-to have probed into its oxidation to oxygen reduction (ORR) and methanol
The electrocatalysis characteristic answered, the results showed that the composite all shows excellent electro-catalysis to the oxidation reaction of ORR and methanol
Strengthen performance and good stability.Equally, Zhang et al. is prepared for difference using different halogens come the pattern of controlled material
The platinum palladium bimetal nano material of pattern, and confirm that this several catalyst has good catalytic performance to methanol.
But the palladium platinum duplex metal nano granule of different-shape is prepared still by the mol ratio of single change palladium and platinum
It is also fewer.In addition, preparing morphology controllable using the method, size is controllable and the controllable different-shape platinum palladium bimetallic of component is received
Rice grain functionalization molybdenum disulfide nano-composite material does not simultaneously have document report also for probing into its electrocatalysis characteristic.Therefore this hair
Bright preparation method has potential application prospect for preparing different-shape, size, the nano composite material of component.
In recent years, graphene received significant attention as a typical two-dimensional catalysts carrier, and molybdenum disulfide conduct
A kind of inorganic graphite alkene, there are the physical and chemical properties similar to graphene.These unique physical and chemical properties are for example big
Specific surface area, good chemical stability, there is direct band gap, there are enough active sites etc., these features
So that when as support material nano material catalysis area can not only maximize molybdenum disulfide, and electronics can be strengthened
Transport.Therefore, molybdenum disulfide has had many applications as support material.For example, Sreeprasad et al., which is reported, passes through
Chemistry and microwave assisting method are prepared for nanometer gold bar functionalization molybdenum disulfide composite and have phototherapy and thermotherapy performance.
Yuwen et al. reports is prepared for Pd-MoS by microwave assisting method2Nano composite material and have to methanol catalytic oxidation
Stronger electrocatalysis characteristic.Huang et al. is prepared for Pd, Pt, the MoS of Au and Ag nano particle functionalized single layers2Nanometer sheet is answered
Condensation material, and in this several composite, Pt-MoS2Have for Pt catalyst of the evolving hydrogen reaction relative to business higher
Catalytic activity.In summary, the duplex metal nano granule functionalization MoS of Pt bases2Nano composite material has in terms of electro-catalysis
There is more excellent catalytic performance.
The content of the invention
A kind of the defects of it is an object of the invention to for above-mentioned prior art, there is provided platinum palladium/curing of morphology controllable
The preparation method of molybdenum nano composite material.
To achieve the above object, the technical scheme that preparation method of the invention uses specifically comprises the steps of：
1) platinum palladium presoma, the secondary potassium chloroplatinate and time potassium chloropalladate that concentration is 10mM~200mM are prepared first；
2) solution one is prepared：Dimethylformamide (DMF) is mixed with ultra-pure water first, ensure DMF and H2O volume ratio
For 1:5~1:1, molybdenum disulfide is added afterwards so that the concentration of molybdenum disulfide is 10~50 μ g/mL in whole solution, and mixing is equal
20~40min is stirred with 800~900r/min rotating speed on magnetic stirring apparatus after even；
3) solution two is prepared：0.01~0.4g PVP, 0.01~0.3g KI are weighed in ready six ampoules,
Label 1,2,3,4,5,6, platinum palladium presoma is added into six bottles, it is determined that the volume for adding time potassium chloropalladate is 60~90 μ
L, time potassium chloroplatinate is then added, the mol ratio for making time potassium chloropalladate and time potassium chloroplatinate is respectively：10:1、5:1、3:1、1:1、
1:5、1:10, finally keep bottle in liquor capacity it is identical, it is insufficient to be supplied with water, be well mixed after on magnetic stirring apparatus with
800~900r/min rotating speed stirs 20~40min；
4) take in six bottles that 3~5mL solution one in step 2 is added sequentially in step 3, in magnetic after being well mixed
10~30min is stirred with 800~900r/min rotating speed on power agitator；
5) finally heated, then to natural cooling, centrifugation, cleaning under room temperature condition, centrifugation product is redispersed in
In a certain amount of ultra-pure water, platinum palladium duplex metal nano granule functionalization molybdenum disulfide nano-composite material is obtained.
Further, molybdenum disulfide can be selected in above-mentioned preparation process as support material.
Further, time presoma of the potassium chloroplatinate as platinum can be selected in preparation process, selects time potassium chloropalladate conduct
The presoma of palladium.
Further, can the use of KI (KI) be main Morphological control agent in preparation process.
Further, Morphological control agent of the dimethylformamide (DMF) for auxiliary can be used in preparation process.
Further, can the use of polyvinylpyrrolidone (PVP) be dispersant in preparation process.
Further, single solution incorporation time is 20~40min in preparation process, the incorporation times of double solution for 10~
20min。
Further, the rotating speed of the magnetic stirring apparatus controlled needed for whipping process maintains 800~900r/min.
Further, the mode of heating described in step 5 is microwave heating, and temperature control is at 100~140 DEG C, and
The time of microwave is 20~40min.
Compared with prior art, the present invention has technique effect beneficial below：
1, there is provided the adjustable morphology controllable of platinum palladium ratio bimetallic functionalization molybdenum disulfide nano-composite material the characteristics of
It is that morphology controllable is successfully prepared using simple, efficient one-step synthesis method, size is controllable, and the controllable platinum palladium bimetallic of component is received
Rice grain functionalization molybdenum disulfide nano-composite material.
2, the nano composite material pattern that the present invention obtains is various, and preparation method is simple, prepared platinum palladium bimetallic work(
Molybdenum disulfide nano-composite material can be changed good application in terms of the catalysis oxidation of methanol.
Brief description of the drawings
Fig. 1 is that the CV of the composition principle figure and its contrast methanol catalytic oxidation by changing platinum palladium presoma ratio schemes.
Fig. 2 is the bimetallic functionalization curing of the morphology controllable obtained under the ratio of change platinum palladium prepared by embodiment 1
The TEM figures of molybdenum nano composite material.It is Pd wherein to scheme A:Pt=10:TEM figures when 1, figure B is Pd:Pt=5:TEM figures when 1,
Figure C is Pd:Pt=3:TEM figures when 1, figure D is Pd:Pt=1:TEM figures when 1, figure E is Pd:Pt=1:TEM figures when 5, figure
F is Pd:Pt=1：TEM figures when 10.
Fig. 3 is the preparation of embodiment 2 in Pd:Pt=1:The double gold of platinum palladium are obtained under the species of lower change halogen of 5 ratio
The TEM figures of metal nano-particle functionalized nano composite.It is TEM figures when adding KCl wherein to scheme A, when figure B is adds KBr
TEM figure, figure C be add KI when TEM figure.
Fig. 4 is the preparation of embodiment 3 in Pd:Pt=1:The double gold of platinum palladium that temperature when changing microwave under 5 ratio obtains
The TEM figures of metal nano-particle functionalized nano composite.Wherein figure A is the TEM figures that microwave temperature is 100 DEG C, wherein figure B is
The TEM that microwave temperature is 110 DEG C schemes, wherein figure C is the TEM figures that microwave temperature is 120 DEG C, wherein figure D is that microwave temperature is 130
DEG C TEM figures, wherein figure E is TEM that microwave temperature is 150 DEG C figure, wherein figure F is the TEM figures that microwave temperature is 160 DEG C.
Fig. 5 is the preparation of embodiment 4 in Pd:Pt=1:Contrast obtains in the case of whetheing there is PVP and DMF under 5 ratio
Platinum palladium duplex metal nano granule functionalized nano composite TEM figure.Wherein figure A is obtained compound for the situation without PVP
The TEM figures of material, figure B are the TEM figures of the composite obtained in the case of having PVP, are obtained in the case of scheming C without DMF
The TEM figures of composite, figure D are the TEM figures obtained in the case of having DMF.
Fig. 6 is different proportion Pd:In the case of Pt, the platinum palladium bimetallic functionalized nano composite of different-shape, which is used as, urges
To the CV comparison diagrams of the catalytic performance of methanol catalytic oxidation during agent.
Embodiment
In conjunction with accompanying drawing, the present invention will be further described in detail.
The present invention successfully prepares morphology controllable using simple, efficient one-step synthesis method, and size is controllable, the controllable palladium of component
Platinum duplex metal nano granule functionalization molybdenum disulfide nano-composite material.It is 10 particularly in palladium and platinum presoma mol ratio:1、
1:1 and 1:5, reaction temperature is at 100~140 DEG C, and KI is main shape inducer, and PVP is as dispersant and DMF as auxiliary shape
Looks instruct to be respectively synthesized the platinum palladium duplex metal nano granule work(of spherical, concave surface cubic block and flower-shaped three kinds of patterns under conditions of agent
Molybdenum disulfide nano-composite material can be changed.Meanwhile these three catalyst all have higher catalytic activity to methanol catalytic oxidation.
Fig. 1 show Pd:Pt=10:1、1:1、1:The CV figures of composition principle figure and its contrast methanol catalytic oxidation when 5.
It can implement the present invention for ease of one of ordinary skill in the art, following specific embodiment is now provided.
Embodiment 1：
1) 100mM secondary potassium chloroplatinate and time potassium chloropalladate is prepared first, the body according to concentration according to required preparation solution
The quality of precursor needed for product weighing.
2) solution one is secondly prepared：The ultra-pure water for being firstly added 9mL DMF and 21mL mixes, and adds our support material
Expect molybdenum disulfide so that the concentration of last molybdenum disulfide remains 25 μ g/mL, with 800- on magnetic stirring apparatus after being well mixed
900r/min rotating speed stirring 30min；
3) solution two：Weigh 0.25g PVP, 0.1g KI in ready six ampoules, marked as 1,2,3,4,5,
6, the 100mM μ L of secondary potassium chloropalladate 80 are all added in six bottles, then sequentially add 8 μ L, 16 μ L, 24 μ L, 80 μ L,
400 μ L, 800 μ L 100mM potassium chloroplatinate, finally it is separately added into 792 μ L, 784 μ L, 776 μ L, 720 μ L, 400 μ L, 0 μ L
Ultra-pure water, 30min is stirred with 800-900r/min rotating speed on magnetic stirring apparatus after being well mixed.
4) take in six bottles that the 4mL solution one in step 2 is added in step 3, in magnetic agitation after being well mixed
15min is stirred with 800-900r/min rotating speed on device.
5) microwave 30min at being finally 130 DEG C in temperature, will then to natural cooling, centrifugation, cleaning under room temperature condition
Centrifugation product is redispersed in a certain amount of ultra-pure water, has just obtained platinum palladium duplex metal nano granule functionalization molybdenum disulfide nano
Composite.Fig. 2 is the TEM figures corresponding to this example, in figure A, B, C, D, E, F correspond respectively to this example marked as 1,2,3,
4th, 5,6 each group example.
Embodiment 2：
It is experiment with No. 5 in embodiment 1, only changes the species of halogen.
1) solution one is prepared：The ultra-pure water for being firstly added 6mL DMF and 14mL mixes, and adds our support material two
Molybdenum sulfide so that the concentration of last molybdenum disulfide remains 25 μ g/mL, with 800- on magnetic stirring apparatus after being well mixed
900r/min rotating speed stirring 30min；
2) tri- bottles of label a, b, c, 0.25g PVP is added, 0.1g KCl, KBr, KI is separately added into, all adds
100mM secondary potassium chloropalladate 80 μ L, the 100mM μ L of potassium chloroplatinate 400 is as solution two, after being well mixed on magnetic stirring apparatus
30min is stirred with 800-900r/min rotating speed.
3) take in three bottles that the 4mL solution one in step 1 is added in step 2, in magnetic agitation after being well mixed
15min is stirred with 800-900r/min rotating speed on device.
4) microwave 30min at being finally 130 DEG C in temperature, will then to natural cooling, centrifugation, cleaning under room temperature condition
Centrifugation product is redispersed in a certain amount of ultra-pure water, has just obtained platinum palladium duplex metal nano granule functionalization molybdenum disulfide nano
Composite.Fig. 3 is that the TEM corresponding to this example schemes, and A, B, C correspond respectively to each group of this example marked as a, b, c in figure
Experiment.
Embodiment 3：
It is experiment with No. 5 in embodiment 1, only changes temperature during microwave.
1) solution one is prepared：The ultra-pure water for being firstly added 9mL DMF and 21mL mixes, and adds our support material two
Molybdenum sulfide so that the concentration of last molybdenum disulfide remains 25 μ g/mL, with 800- on magnetic stirring apparatus after being well mixed
900r/min rotating speed stirring 30min；
2) tri- bottles of label A, B, C, D, E, F, 0.25g PVP, 0.1g KI is added and adds 100mM secondary chlorine
Palladium acid potassium 80 μ L, the 100mM μ L of potassium chloroplatinate 400 is as solution two, with 800-900r/ on magnetic stirring apparatus after being well mixed
Min rotating speed stirring 30min.
3) the 4mL solution one in step 2 is taken to be added in six bottles of step 3, in magnetic stirring apparatus after being well mixed
On 15min stirred with 800-900r/min rotating speed.
4) last microwave at 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C, 150 DEG C, 160 DEG C at different temperature respectively
30min, then to natural cooling, centrifugation, cleaning under room temperature condition, centrifugation product is redispersed in a certain amount of ultra-pure water,
Just platinum palladium duplex metal nano granule functionalization molybdenum disulfide nano-composite material has been obtained.Fig. 4 is the TEM corresponding to this example
Scheme, A, B, C, D, E, F correspond respectively to each group experiment of this example marked as A, B, C, E, D, F in figure.
Embodiment 4：
It is experiment with No. 5 in embodiment 1, only changes addition is to whether there is PVP or DMF.
1) solution one is prepared：The ultra-pure water for being firstly added 6mL DMF and 14mL mixes, and adds our support material two
Molybdenum sulfide so that the concentration of last molybdenum disulfide remains 25 μ g/mL, is well mixed on magnetic stirring apparatus with 800-900r/
Min rotating speed stirring 30min；
2) tetra- bottles of label W, X, Y, Z, the KI for weighing 0.25g PVP, 0.1g are added thereto, and a W bottle is added without
PVP, add 100mM secondary potassium chloropalladate 80 μ L, the 100mM μ L of potassium chloroplatinate 400 afterwards as solution two, it is well mixed after
30min is stirred with 800-900r/min rotating speed on magnetic stirring apparatus.
3) the 4mL solution one in step 1 is added in the bottle in step 2 marked as W, X, Z, and Y bottles only add
The 4mL 25 μ g/mL molybdenum disulfide aqueous solution, stirred after being well mixed on magnetic stirring apparatus with 800-900r/min rotating speed
15min。
4) microwave 30min at being finally 130 DEG C in temperature, will then to natural cooling, centrifugation, cleaning under room temperature condition
Centrifugation product is redispersed in a certain amount of ultra-pure water, has just obtained platinum palladium duplex metal nano granule functionalization molybdenum disulfide nano
Composite.Fig. 5 is that the TEM corresponding to this example schemes, and it is real to correspond to each group of this example marked as W, X, Y, Z by A, B, C, D in figure
Test.
Fig. 6 is that compared for working as Pd:Pt=10:1、1:1、1:In the case of 5 three kinds, the platinum palladium bimetallic functionalization of different-shape
To the CV comparison diagrams of the catalytic performance of methanol catalytic oxidation when nano composite material is as catalyst.Wherein a is Pd:Pt=10:
1, b Pd:Pt=1:1, c Pd:Pt=1:5.
Claims (9)
1. the preparation method of platinum palladium/molybdenum disulfide nano-composite material of a kind of morphology controllable, it is characterised in that include following step
Suddenly：
1) platinum palladium presoma, the secondary potassium chloroplatinate and time potassium chloropalladate that concentration is 10mM~200mM are prepared first；
2) solution one is prepared：Dimethylformamide (DMF) is mixed with ultra-pure water first, ensure DMF and H2O volume ratio is 1:5
~1:1, add molybdenum disulfide afterwards so that the concentration of molybdenum disulfide be 10~50 μ g/mL in whole solution, it is well mixed after
20~40min is stirred with 800~900r/min rotating speed on magnetic stirring apparatus；
3) solution two is prepared：0.01~0.4g PVP, 0.01~0.3g KI are weighed in ready six ampoules, label
1st, 2,3,4,5,6, platinum palladium presoma is added into six bottles, it is determined that the volume for adding time potassium chloropalladate is 60~90 μ L, so
Time potassium chloroplatinate is added afterwards, and the mol ratio for making time potassium chloropalladate and time potassium chloroplatinate is respectively：10:1、5:1、3:1、1:1、1:5、
1:10, finally keep liquor capacity in bottle identical, it is insufficient to be supplied with water, with 800 on magnetic stirring apparatus after being well mixed
~900r/min rotating speed stirs 20~40min；
4) take in six bottles that 3~5mL solution one in step 2 is added sequentially in step 3, stirred after well mixed in magnetic force
Mix and 10~30min is stirred with 800~900r/min rotating speed on device；
5) finally heated, then to natural cooling, centrifugation, cleaning under room temperature condition, centrifugation product is redispersed in necessarily
In the ultra-pure water of amount, platinum palladium duplex metal nano granule functionalization molybdenum disulfide nano-composite material is obtained.
2. the preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable according to claim 1, its feature
Molybdenum disulfide can be being selected in preparation process as support material.
3. the preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable according to claim 1, its feature
It is to select time presoma of the potassium chloroplatinate as platinum, selects time presoma of the potassium chloropalladate as palladium.
4. the preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable according to claim 1, its feature
Can the use of KI (KI) be main Morphological control agent in preparation process.
5. the preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable according to claim 1, its feature
Morphological control agent of the dimethylformamide (DMF) for auxiliary can be being used in preparation process.
6. the preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable according to claim 1, its feature
Can the use of polyvinylpyrrolidone (PVP) be dispersant in preparation process.
7. the preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable according to claim 1, its feature
In preparation process single solution incorporation time be 20~40min, the incorporation time of double solution is 10~20min.
8. the preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable according to claim 1, its feature
The rotating speed for the magnetic stirring apparatus for being to control needed for whipping process maintains 800~900r/min.
9. the preparation method of platinum palladium/molybdenum disulfide nano-composite material of morphology controllable according to claim 1, its feature
It is that mode of heating described in step 5 is microwave heating, and temperature control is at 100~140 DEG C, and the time of microwave is
20~40min.
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