CN109731583A - A kind of two-step method preparation Zn0.2Cd0.8The method of S/rGO composite material - Google Patents
A kind of two-step method preparation Zn0.2Cd0.8The method of S/rGO composite material Download PDFInfo
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- CN109731583A CN109731583A CN201910057777.4A CN201910057777A CN109731583A CN 109731583 A CN109731583 A CN 109731583A CN 201910057777 A CN201910057777 A CN 201910057777A CN 109731583 A CN109731583 A CN 109731583A
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Abstract
A kind of two-step method preparation Zn0.2Cd0.8Ethylenediamine wiring solution-forming A is added into deionization for the method for S/rGO composite material；Zinc diacetate dihydrate and four nitric hydrate cadmiums are added in solution A and form solution B；L-cysteine is added in solution B and forms solution C；Solution C is added in the liner of polytetrafluoroethylene (PTFE), carries out hydro-thermal reaction；To after the reaction was completed, distinguish centrifuge washing several times through deionized water and ethyl alcohol, obtain Zn through drying and grinding0.2Cd0.8S powder；RGO wiring solution-forming D is added into deionized water；Take Zn0.2Cd0.8S powder is added in solution D and forms solution E；After solution E is carried out hydro-thermal reaction, centrifuge washing is distinguished through deionized water and ethyl alcohol, obtains Zn through drying and grinding0.2Cd0.8S/rGO material powder.Preparation process of the present invention is simple, at low cost, using the distinctive band structure of graphene, makes Zn0.2Cd0.8The light induced electron of S solid-solution material enters in graphene, and electronics is limited in different object phases respectively from hole, reaches the inhibiting effect compound to photo-generate electron-hole.
Description
Technical field
Zn is prepared the present invention relates to a kind of0.2Cd0.8A kind of method of S/rGO composite material, and in particular to two-step method preparation
Zn0.2Cd0.8The method of S/rGO composite material.
Background technique
Today's society, with social progress and development, the degree of industrialization and manual intelligent is higher and higher, for institute
Also higher and higher using the requirement of material, traditional material is not able to satisfy the demand used, therefore more and more functional materials
And composite material is rapidly progressed.And II-VI compound is the emphasis and hot spot studied instantly, since they are partly leading
The fields such as body laser, sensor, solid luminescence and solar battery have a wide range of applications, therefore have attracted much attention always.
Wherein ZnxCd1-xS (0≤x≤1) solid-solution material is as a kind of novel material with good photocatalysis performance, due to it
The forbidden bandwidth and unique catalytic activity of adjustable transformation, and widely studied.
ZnxCd1-xS solid-solution material is used as a kind of semiconductor type photochemical catalyst with direct broad-band gap with Cd
The increase of amount, forbidden bandwidth are gradually lowered to 2.3eV from 3.6eV, due to its appropriate forbidden bandwidth, can make it very well
Utilization and absorb sunlight in a certain amount of visible light and a part black light.And its with it is cheap,
Chemical stability is stronger, anti-light corrosion and the advantages that be easy recycling, just arouses widespread concern once coming out.
ZnxCd1-xAll there is potential applications in many industrial circles by S, and are usually applied to luminescence generated by light and photoconductor is set
Standby, photocatalytic degradation produces hydrogen, in fluorescent powder and other photoelectric fields.Graphene belongs to zero gap semiconductor, electron mobility
Higher, theoretical specific surface area is up to 2630m2/ g is the good carrier of photochemical catalyst.Utilize this distinctive energy band knot of graphene
Structure and ZnxCd1-xS (0≤x≤1) solid-solution material is compound, can make ZnxCd1-xThe light induced electron of S (0≤x≤1) solid-solution material
Into in graphene, electronics is limited in different object phases respectively from hole, reaches the inhibition compound to photo-generate electron-hole
Effect, while expanding ZnxCd1-xThe optical response range of S (0≤x≤1) solid-solution material, makes it have more stable photocatalysis
Performance.
In recent years, with for ZnxCd1-xS research is goed deep into, and researcher learns that its structure and performance are made with it
Standby method has close connection.According to the exploration of people, hydro-thermal method, coprecipitation, microemulsion method and heat point have been used
Zn has successfully been prepared in the conventional methods such as solutionxCd1-xS solid-solution material.Currently, Zn0.2Cd0.8The conjunction of S (x=0.2) material
Mainly have at method: coprecipitation (Xing C, Zhang Y, Yan W, et al.Band structure-controlled
solid solution of Cd1-xZnxS photocatalyst for hydrogen production by water
Splitting [J] .Int.J.Hydrogen Energy, 2006,31 (14): 2018-2024), microemulsion method (Chen D, Gao
L.Microemulsion-mediated synthesis of cadmium zinc sulfide nanocrystals with
composition-modulated optical properties[J].Solid State Communications,2005,
133 (3): 145-150.), thermal decomposition method (Yu J, Yang B, Cheng B.Noble-metal-free carbon
nanotube-Cd0.1Zn0.9S composites for high visible-light photocatalytic H2-
production performance[J].Nanoscale,2012,4(8):2670-2677.).Wherein, coprecipitation reaction speed
Degree is fast, and simple process is easy to operate, and product quality is excellent, but for the more demanding of temperature, energy consumption is larger, and product is easy hair
Raw burn knot or melting are reacted not easily-controllable.Microemulsion method technological operation is relatively simple, and device is simple, easy to operate, and particle is equal
It is even, but have a large amount of organic matter and generate, it can have a certain impact to environment, cause environmental pollution, reaction rate is more difficult to control,
It also needs to increase the processing to byproduct of reaction, so that the increased costs of reaction.Thermal decomposition method operation is simple, reaction rate
Fastly, but product is easily caused to reunite, and reaction required temperature is higher, it is higher to energy and cost requirement needed for producing.
Summary of the invention
Low, simple process that the purpose of the present invention is to provide a kind of preparation costs, and good crystallinity, pattern can be prepared
Novel two-step method prepares Zn0.2Cd0.8The method of S/rGO composite material.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
Step 1: it takes the ethylenediamine of 5~10mL to be added in the deionized water of 20~40mL and forms mixed solution A；
Step 2: take respectively 0.2~0.4mmol Zinc diacetate dihydrate and 0.8~1.6mmol four nitric hydrate cadmiums with
nZn: nCdThe molar ratio of=1:4 is added in mixed solution A and mixed solution B is made；
Step 3: it takes the L-cysteine of 2~4mmol as sulphur source, is added in mixed solution B and forms mixed solution C；
Step 4: mixed solution C is added in the liner of polytetrafluoroethylene (PTFE), in 160~200 DEG C of 8~12h of reaction；
Step 5: to after the reaction was completed, through grinding after deionized water and ethyl alcohol distinguish centrifuge washing, vacuum drying
Zn0.2Cd0.8S material powder；
Step 6: take the redox graphene that 1~2mL concentration is 1mg/mL that the deionized water magnetic force of 29~48mL is added
Stirring forms mixed solution D；
Step 7: the Zn of 0.1~0.5mmol is taken0.2Cd0.8S powder is added in mixed solution D, and magnetic agitation forms mixing
Solution E；
Step 8: will mixed solution E be added polytetrafluoroethylene (PTFE) liner in, 160~200 DEG C react 18~for 24 hours；
Step 9: to after the reaction was completed, through grinding after deionized water and ethyl alcohol distinguish centrifuge washing, vacuum drying to obtain the final product
Zn0.2Cd0.8S/rGO material powder.
It is described Step 1: step 2 and step 3 be 20~40min of magnetic agitation, 15~30min of ultrasonic disperse prepare
Mixed solution A, mixed solution B and mixed solution C.
The step 4 packing ratio is 25%~50%.
The step 5 deionized water and ethyl alcohol are distinguished centrifuge washing 3~5 times.
The step 5 vacuum drying temperature is 60~80 DEG C, and drying time is 6~10h.
The step 8 packing ratio is 30%~50%.
The deionized water and ethyl alcohol of the step 9 are distinguished centrifuge washing 3~5 times.
The vacuum drying temperature of the step 9 is 60~80 DEG C, and drying time is 6~10h.
Compared with prior art, the invention has the following beneficial technical effects:
Preparation process of the present invention is simple, at low cost, while by rGO and the rodlike Zn being assembled into0.2Cd0.8S nanosphere is multiple
It closes, Zn can be made using the distinctive band structure of graphene with biggish specific surface area0.2Cd0.8The light of S solid-solution material
Raw electronics enters in graphene, and electronics is limited in different object phases respectively from hole, reaches compound to photo-generate electron-hole
Inhibiting effect, while expanding Zn0.2Cd0.8The optical response range of S solid-solution material makes it have more stable photocatalytic
Energy.Therefore the photo-catalysis capability of material is stronger, the size of material reaches dozens to a few hundred nanometers, and material purity is high, crystallinity is strong,
It can apply in fields such as photocatalytic degradation of organic matter, photodissociation aquatic products hydrogen or electronic light emitting devices, obtain economic effect well
Benefit and social benefit, since the performance of material is more excellent, application also can preferably be developed.
Detailed description of the invention
Fig. 1 is Zn prepared by the embodiment of the present invention 20.2Cd0.8The XRD diagram of S/rGO material；
Fig. 2 is Zn prepared by the embodiment of the present invention 20.2Cd0.8The SEM of S/rGO material schemes；
Fig. 3 is Zn prepared by the embodiment of the present invention 20.2Cd0.8The hydrogen manufacturing Time-orientation figure of S/rGO material；
Fig. 4 is Zn prepared by the embodiment of the present invention 20.2Cd0.8The hydrogen manufacturing loop test figure of S/rGO material.
Specific embodiment
The invention will be described in further detail with reference to the accompanying drawings and embodiments.
Embodiment 1:
Step 1: take the ethylenediamine (EN) of 5mL that magnetic agitation 20min, ultrasonic disperse in the deionized water of 20mL is added
15min forms mixed solution A；
Step 2: the Zinc diacetate dihydrate (Zn (Ac) of 0.2mmol is taken respectively2·2H2) and four nitric hydrates of 0.8mmol O
Cadmium (Zn (NO3)2·4H2O magnetic agitation 20min, ultrasonic disperse 15min in mixed solution A) is added, mixed solution B is made；
Step 3: it takes the L-cysteine of 2mmol as sulphur source, magnetic agitation 20min, ultrasound in mixed solution B is added
Disperse 15min and forms mixed solution C；
Step 4: mixed solution C being added in the liner of polytetrafluoroethylene (PTFE), and control packing ratio is 25%, is reacted at 160 DEG C
8h；
Step 5: to after the reaction was completed, distinguish centrifuge washing 3 times through deionized water and ethyl alcohol, in 60 DEG C of vacuum drying 6h
By grinding to obtain Zn0.2Cd0.8S material powder；
Step 6: take the redox graphene that 1mL concentration is 1mg/mL that the deionized water magnetic agitation shape of 29mL is added
At mixed solution D；
Step 7: the Zn of 0.1mmol is taken0.2Cd0.8S powder is added in mixed solution D, and magnetic agitation forms mixed solution E；
Step 8: mixed solution E being added in the liner of polytetrafluoroethylene (PTFE), and control packing ratio is 30%, is reacted at 160 DEG C
18h；
Step 9: to after the reaction was completed, distinguish centrifuge washing 3 times through deionized water and ethyl alcohol, in 60 DEG C of vacuum drying 6h
By grinding up to Zn0.2Cd0.8S/rGO material powder.
Embodiment 2:
Step 1: take the ethylenediamine (EN) of 10mL that magnetic agitation 30min, ultrasonic disperse in the deionized water of 40mL is added
30min forms mixed solution A；
Step 2: the Zinc diacetate dihydrate (Zn (Ac) of 0.3mmol is taken respectively2·2H2) and four nitric hydrates of 1.2mmol O
Cadmium (Zn (NO3)2·4H2O magnetic agitation 30min, ultrasonic disperse 30min in mixed solution A) is added, mixed solution B is made；
Step 3: it takes the L-cysteine of 3mmol as sulphur source, magnetic agitation 30min, ultrasound in mixed solution B is added
Disperse 30min and forms mixed solution C；
Step 4: mixed solution C being added in the liner of polytetrafluoroethylene (PTFE), and control packing ratio is 50%, is reacted at 200 DEG C
12h；
Step 5: to after the reaction was completed, distinguish centrifuge washing 4 times through deionized water and ethyl alcohol, in 80 DEG C of vacuum drying 8h
By grinding to obtain Zn0.2Cd0.8S material powder；
Step 6: take the redox graphene that 2mL concentration is 1mg/mL that the deionized water magnetic agitation shape of 48mL is added
At mixed solution D；
Step 7: the Zn of 0.5mmol is taken0.2Cd0.8S powder is added in mixed solution D, and magnetic agitation forms mixed solution E；
Step 8: mixed solution E being added in the liner of polytetrafluoroethylene (PTFE), and control packing ratio is 50%, is reacted at 200 DEG C
24h；
Step 9: to after the reaction was completed, distinguish centrifuge washing 4 times through deionized water and ethyl alcohol, in 80 DEG C of vacuum drying 8h
By grinding up to Zn0.2Cd0.8S/rGO material powder.
As can be seen from Figure 1 sample prepared by embodiment 2 corresponds to standard card PDF#40-0835 (Zn0.2Cd0.8S).From
It can be seen that the crystallinity of the material is preferable in XRD diagram.The microsphere diameter that the material can have been found out from Fig. 2 is about 600nm
Left and right.As can be seen from Figure 3 sample prepared by embodiment 2 is 1117.3 μ in the hydrogen manufacturing amount of a reaction time (4h)
mol.It can be seen that sample prepared by embodiment 2 passes through the loop test of three periods (12h) in Fig. 4, hydrogen manufacturing performance does not have substantially
There is decline, illustrates that its photocatalysis performance is stablized.
Embodiment 3:
Step 1: take the ethylenediamine (EN) of 8mL that magnetic agitation 40min, ultrasonic disperse in the deionized water of 30mL is added
20min forms mixed solution A；
Step 2: the Zinc diacetate dihydrate (Zn (Ac) of 0.4mmol is taken respectively2·2H2) and four nitric hydrates of 1.6mmol O
Cadmium (Zn (NO3)2·4H2O magnetic agitation 40min, ultrasonic disperse 20min in mixed solution A) is added, mixed solution B is made；
Step 3: it takes the L-cysteine of 4mmol as sulphur source, magnetic agitation 40min, ultrasound in mixed solution B is added
Disperse 20min and forms mixed solution C；
Step 4: mixed solution C being added in the liner of polytetrafluoroethylene (PTFE), and control packing ratio is 38%, is reacted at 180 DEG C
10h；
Step 5: to after the reaction was completed, distinguish centrifuge washing 5 times through deionized water and ethyl alcohol, in 70 DEG C of vacuum drying 10h
By grinding to obtain Zn0.2Cd0.8S material powder；
Step 6: the deionized water magnetic force for taking the redox graphene that 1.5mL concentration is 1mg/mL that 38.5mL is added stirs
It mixes to form mixed solution D；
Step 7: the Zn of 0.3mmol is taken0.2Cd0.8S powder is added in mixed solution D, and magnetic agitation forms mixed solution E；
Step 8: mixed solution E being added in the liner of polytetrafluoroethylene (PTFE), and control packing ratio is 40%, is reacted at 180 DEG C
20h；
Step 9: to after the reaction was completed, distinguish centrifuge washing 5 times through deionized water and ethyl alcohol, in 70 DEG C of vacuum drying 10h
By grinding up to Zn0.2Cd0.8S/rGO material powder.
Claims (8)
1. a kind of two-step method prepares Zn0.2Cd0.8The method of S/rGO composite material, it is characterised in that the following steps are included:
Step 1: it takes the ethylenediamine of 5~10mL to be added in the deionized water of 20~40mL and forms mixed solution A；
Step 2: four nitric hydrate cadmiums of the Zinc diacetate dihydrate and 0.8~1.6mmol that take 0.2~0.4mmol respectively are with nZn:
nCdThe molar ratio of=1:4 is added in mixed solution A and mixed solution B is made；
Step 3: it takes the L-cysteine of 2~4mmol as sulphur source, is added in mixed solution B and forms mixed solution C；
Step 4: mixed solution C is added in the liner of polytetrafluoroethylene (PTFE), in 160~200 DEG C of 8~12h of reaction；
Step 5: to after the reaction was completed, through grinding after deionized water and ethyl alcohol distinguish centrifuge washing, vacuum drying
Zn0.2Cd0.8S material powder；
Step 6: take the redox graphene that 1~2mL concentration is 1mg/mL that the deionized water magnetic agitation of 29~48mL is added
Form mixed solution D；
Step 7: the Zn of 0.1~0.5mmol is taken0.2Cd0.8S powder is added in mixed solution D, and magnetic agitation forms mixed solution
E；
Step 8: will mixed solution E be added polytetrafluoroethylene (PTFE) liner in, 160~200 DEG C react 18~for 24 hours；
Step 9: to after the reaction was completed, through grinding after deionized water and ethyl alcohol distinguish centrifuge washing, vacuum drying to obtain the final product
Zn0.2Cd0.8S/rGO material powder.
2. two-step method according to claim 1 prepares Zn0.2Cd0.8The method of S/rGO composite material, it is characterised in that: institute
State Step 1: step 2 and step 3 be 20~40min of magnetic agitation, 15~30min of ultrasonic disperse prepare mixed solution A,
Mixed solution B and mixed solution C.
3. two-step method according to claim 1 prepares Zn0.2Cd0.8The method of S/rGO composite material, it is characterised in that: institute
Stating step 4 packing ratio is 25%~50%.
4. two-step method according to claim 1 prepares Zn0.2Cd0.8The method of S/rGO composite material, it is characterised in that: institute
It states step 5 deionized water and ethyl alcohol is distinguished centrifuge washing 3~5 times.
5. two-step method according to claim 1 prepares Zn0.2Cd0.8The method of S/rGO composite material, it is characterised in that: institute
Stating step 5 vacuum drying temperature is 60~80 DEG C, and drying time is 6~10h.
6. two-step method according to claim 1 prepares Zn0.2Cd0.8The method of S/rGO composite material, it is characterised in that: institute
Stating step 8 packing ratio is 30%~50%.
7. two-step method according to claim 1 prepares Zn0.2Cd0.8The method of S/rGO composite material, it is characterised in that: institute
The deionized water and ethyl alcohol for stating step 9 are distinguished centrifuge washing 3~5 times.
8. two-step method according to claim 1 prepares Zn0.2Cd0.8The method of S/rGO composite material, it is characterised in that: institute
The vacuum drying temperature for stating step 9 is 60~80 DEG C, and drying time is 6~10h.
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| CN111129494A (en) * | 2019-12-28 | 2020-05-08 | 常州大学 | Preparation method of sulfo-spinel/graphene electrode material and electrode material thereof |
| CN112939062A (en) * | 2021-04-19 | 2021-06-11 | 陕西科技大学 | Rodlike Zn0.7Cd0.3Preparation method of S material |
| CN113044876A (en) * | 2021-04-14 | 2021-06-29 | 陕西科技大学 | Preparation method of sea urchin-shaped zinc-cadmium-sulfur material |
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| CN110354867A (en) * | 2019-07-18 | 2019-10-22 | 陕西科技大学 | A kind of Zn0.2Cd0.8The preparation method of S/rGO catalysis material |
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| CN113044876A (en) * | 2021-04-14 | 2021-06-29 | 陕西科技大学 | Preparation method of sea urchin-shaped zinc-cadmium-sulfur material |
| CN113044876B (en) * | 2021-04-14 | 2022-08-05 | 陕西科技大学 | Preparation method of sea urchin-shaped zinc-cadmium-sulfur material |
| CN112939062A (en) * | 2021-04-19 | 2021-06-11 | 陕西科技大学 | Rodlike Zn0.7Cd0.3Preparation method of S material |
| CN112939062B (en) * | 2021-04-19 | 2022-08-05 | 陕西科技大学 | Rodlike Zn 0.7 Cd 0.3 Preparation method of S material |
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