CN107697944B - A kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble - Google Patents
A kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble Download PDFInfo
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- CN107697944B CN107697944B CN201710866509.8A CN201710866509A CN107697944B CN 107697944 B CN107697944 B CN 107697944B CN 201710866509 A CN201710866509 A CN 201710866509A CN 107697944 B CN107697944 B CN 107697944B
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/006—Compounds containing, besides cadmium, two or more other elements, with the exception of oxygen or hydrogen
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a kind of preparation methods of the spherical zinc cadmium sulphur solid-solution material of particles self assemble, weigh CMC wiring solution-forming, are then successively stirred and are ultrasonically treated, and form mixed solution A；Zinc diacetate dihydrate and Cadmium diacetate dihydrate are weighed, is added in mixed solution A, is then successively stirred and is ultrasonically treated, mixed solution B is formed；Thioacetamide is weighed as sulphur source, is added in mixed solution B；Then it is successively stirred and is ultrasonically treated, form mixed solution C；Mixed solution C is acidified using HCl solution, then is ultrasonically treated, mixed solution D is formed；Mixed solution D is added in the liner of polytetrafluoroethylene (PTFE) and carries out hydro-thermal reaction；To after the reaction was completed, product be distinguished centrifuge washing several times through deionized water and ethyl alcohol, then drying and grinding obtains material requested powder.
Description
Technical field
The present invention relates to Zn1-xCdxA kind of preparation method of S material, and in particular to spherical zinc cadmium sulphur solid solution of particles self assemble
Body (Zn0.2Cd0.8S) the preparation method of material.
Background technique
Nowadays, with the development of scientific and technological industry and aerospace, building and electronic field etc., the requirement to material is got over
Carrying out higher, traditional material cannot meet the requirements, and the development that more and more functional materials and composite material are leaped.
Before II-VI compound is had a wide range of applications due to them in fields such as semiconductor laser, solid luminescence and solar batteries
Scape and have been a concern, wherein Zn1-xCdxS (0≤x≤1) solid-solution material is as novel catalysis material, since it can
The forbidden bandwidth and unique catalytic activity of transformation are adjusted, and is widely studied.
Zn1-xCdxS solid solution is as a kind of semiconductor type photochemical catalyst with direct broad-band gap, with Cd usage amount
Increase, forbidden bandwidth is gradually lowered to 2.3eV from 3.6eV, just because of its appropriate forbidden bandwidth, can be good at making
With the black light of a certain amount of visible light and a part in sunlight.And it has cheap and easy to get, chemical stability
The advantages of strong and anti-light corrosion, just arouses widespread concern once coming out.Zn1-xCdxS many fields all there is
Potential application, and usually it is applied to luminescence generated by light photoconductor equipment, photocatalysis, fluorescent powder and other photoelectric fields
In.
In recent years, with for Zn1-xCdxS 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, use coprecipitation, microemulsion method and thermal decomposition method etc. normal
Zn has successfully been prepared in rule method1-xCdxS solid solution.
Currently, Zn0.2Cd0.8The synthetic method of S (x=0.2) material mainly has: coprecipitation (Xing C, Zhang Y,
Yan W,et al.Band structure-controlled solid olution of d1-xZnxS photocatalyst
for hydrogen production by water splitting[J].Int.J.Hydrogen Energ.,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 Commun., 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 is fast, and simple process is easy to operate, and product quality is excellent, but for temperature
It is more demanding, energy consumption is larger, and product is made to be easy to happen sintering or melting, reacts not easily-controllable.Microemulsion method technological operation
Relatively simple, device simple operations facilitate uniform particle, but have a large amount of organic matter and generate, and certain shadow is had to environment
It rings, causes environmental pollution, reaction rate is more difficult to control, it is also necessary to increase the processing to byproduct of reaction, so that the cost of reaction
Increase.Thermal decomposition method operation is simple, and reaction rate is fast, but product is easily caused to reunite, and reaction required temperature is higher, to production
Required energy and cost requirement are higher.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble, with gram
Take problem of the existing technology, preparation cost of the present invention is low, short preparation period, and it is new to prepare good crystallinity, pattern
The Zn of grain husk0.2Cd0.8S material.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of spherical Zn of particles self assemble0.2Cd0.8The preparation method of S material, comprising the following steps:
Step 1: it weighs CMC and H is added2In O, it is made into the solution of 1~3g/L, is then successively stirred and is ultrasonically treated,
Form mixed solution A；
Step 2: according to nZn:nCdThe ratio of=1:1 weighs Zn (Ac)2·2H2O and Zn (Cd)2·2H2It is molten that mixing is added in O
In liquid A, and CMC and Zn (Ac)2·2H2The ratio of O is (0.036~0.108g): (0.1~0.5mmol) is then successively stirred
Ultrasonic treatment is mixed and stirred, mixed solution B is formed；
Step 3: thioacetamide is weighed as sulphur source, is added in mixed solution B, wherein thioacetyl and Zn (Ac)2·
2H2The molar ratio of O is (1~3): (0.1~0.5) is then successively stirred and is ultrasonically treated, and forms mixed solution C；
Step 4: being acidified mixed solution C using HCl solution, then be ultrasonically treated, and mixed solution D is formed；
Step 5: mixed solution D is added in the liner of polytetrafluoroethylene (PTFE) and carries out hydro-thermal reaction；
Step 6: to after the reaction was completed, product be distinguished centrifuge washing several times through deionized water and ethyl alcohol, is then dried
Grinding obtains Zn0.2Cd0.8S material powder.
Further, mixing time is 1~3h in step 1, and sonication treatment time is 5~30min.
Further, mixing time is 15min in step 2, and sonication treatment time is 5~30min.
Further, mixing time is 15min in step 3, and sonication treatment time is 5~30min.
Further, the concentration of HCl solution is 0.01~0.1mol/L in step 4.
Further, the PH of mixed solution C is adjusted to 2.0~3.0 using HCl solution in step 4.
Further, the time being ultrasonically treated in step 4 is 5~20min.
Further, hydrothermal reaction condition is as follows in step 5: 30%~36%, reaction temperature is controlled for packing ratio control
At 140 DEG C~180 DEG C, the reaction time is controlled in 2h~6h.
Further, product is distinguished centrifuge washing 3~6 times through deionized water and ethyl alcohol in step 6.
Further, dry in step 6 specifically: 40~60 DEG C at a temperature of be dried in vacuo 1~3h.
Compared with prior art, the invention has the following beneficial technical effects:
Preparation process of the present invention is simple, at low cost, the period is short, while prepared Zn0.2Cd0.8S material be little particle from
The nanometer assembled is spherical, with biggish specific surface area, therefore the electron-transport Distance Shortened of semiconductor, electron hole
Separative efficiency be improved, therefore the photo-catalysis capability of material is stronger, and the size of material reaches dozens to a few hundred nanometers, and material
Purity is high, crystallinity are strong, can apply in fields such as photocatalytic degradation of organic matter, photodissociation aquatic products hydrogen or electronic light emitting devices,
Good economic benefit and social benefit are obtained, since the performance of material is more excellent, application also can preferably be developed.
Further, Zn is prepared using hydro-thermal method0.2Cd0.8S material, technological operation is simple, does not need large-scale reaction
Equipment, under hydrothermal conditions, a kind of chemical constituent of water can be used as work and participate in reaction, are both solvent and mineralizer is same
When be alternatively arranged as pressure transmission medium；By participating in dialysis reaction and control physical chemical factor etc., inorganic compound is realized
It is formed and modified.Not only one pack system tiny crystals can be prepared, but also bi-component or multi-component special compound powder can be prepared.Hydro-thermal
The characteristics of method produces is particle purity is high, good dispersion, good crystalline and can control that production cost is low, the powder prepared with hydro-thermal method
Body is generally not necessarily to be sintered, and is conducive to depollution of environment etc..This can grow up to avoid crystal grain during the sintering process and impurity holds
The disadvantages of being easily mixed into.The difference of object phase and appearance structure has large effect to the performance of material, and the method for the present invention is by zinc salt
(Zn(Ac)2·2H2) and cadmium salt (Zn (Cd) O2·2H2O) water-soluble in CMC (sodium carboxymethylcellulose) with thioacetamide (TAA)
Hydro-thermal reaction is carried out under the acid condition of liquid to obtain product.
Detailed description of the invention
Fig. 1 is example 3 of the present invention passed through technique hydro-thermal method synthesis Zn0.2Cd0.8The XRD diagram of S material；
Fig. 2 is that example 3 of the present invention synthesizes Zn by hydro-thermal method0.2Cd0.8The SEM of S material schemes.
Specific embodiment
Embodiments of the present invention are described in further detail below:
A kind of spherical Zn of particles self assemble0.2Cd0.8The preparation method of S material, comprising the following steps:
1) CMC is weighed a certain amount of, is made into the solution (36ml) of 1~3g/L, after carrying out 1~3h of magnetic agitation, is surpassed
5~30min of sound forms mixed solution A.
2) Zinc diacetate dihydrate (Zn (Ac) is used2·2H2) and Cadmium diacetate dihydrate (Zn (Cd) O2·2H2It O) is raw material
(nZn:nCd=1:1), 0.1~0.5mmol is weighed respectively, is added in mixed solution A, after carrying out magnetic agitation 15min, and into
Row 5~30min of ultrasound, forms mixed solution B.
3) 1~3mmol is weighed as sulphur source using thioacetamide, be added in mixed solution B, carry out magnetic agitation
After 15min, and 5~30min of ultrasound is carried out, forms mixed solution C.
4) concentration prepared is used to be acidified for the HCl solution of 0.01~0.1mol/L to mixed solution C, using PH
Tester is detected, and after the solution PH of whole system is adjusted to PH=2.0~3.0, then carries out 5~20min of ultrasound, is formed
Mixed solution D.
5) mixed solution D is added in the liner of polytetrafluoroethylene (PTFE), packing ratio control is 30%~36%, reaction temperature control
At 140 DEG C~180 DEG C, the reaction time controls in 2h~6h system.
6) to after the reaction was completed, distinguish centrifuge washing 3~6 times through deionized water and ethyl alcohol.Then 40~60 DEG C of vacuum are dry
It is ground that Zn can be obtained after dry 1~3h0.2Cd0.8S material powder.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
1) CMC is weighed a certain amount of, is made into the solution (36ml) of 1g/L, after carrying out magnetic agitation 1h, carries out ultrasound 5min,
Form solution A.
2) Zinc diacetate dihydrate (Zn (Ac) is used2·2H2) and Cadmium diacetate dihydrate (Zn (Cd) O2·2H2It O) is raw material
(nZn:nCd=1:1), 0.1mmol is weighed respectively, is added in solution A, after carrying out magnetic agitation 15min, and carries out ultrasound
5min forms mixed solution B.
3) 1mmol is weighed as sulphur source using thioacetamide, be added in mixed solution B, carry out magnetic agitation
After 15min, and ultrasonic 5min is carried out, forms solution C.
4) concentration prepared is used to be acidified for the HCl solution of 0.01mol/L to solution C, using PH tester into
Row detection, after the solution PH of whole system is adjusted to PH=2.0, then carries out ultrasonic 5min, forms mixed solution D.
5) solution D being added in the liner of polytetrafluoroethylene (PTFE), 30%, reaction temperature is controlled at 140 DEG C for packing ratio control,
Reaction time controls in 2h.
6) to after the reaction was completed, distinguish centrifuge washing 3 times through deionized water and ethyl alcohol.Then after 40 DEG C of vacuum drying 1h,
It is ground that Zn can be obtained0.2Cd0.8S material powder.
Embodiment 2
1) CMC is weighed a certain amount of, is made into the solution (36ml) of 2g/L, after carrying out magnetic agitation 2h, carries out ultrasound
15min forms solution A.
2) Zinc diacetate dihydrate (Zn (Ac) is used2·2H2) and Cadmium diacetate dihydrate (Zn (Cd) O2·2H2It O) is raw material
(nZn:nCd=1:1), 0.3mmol is weighed respectively, is added in solution A, after carrying out magnetic agitation 15min, and carries out ultrasound
15min forms mixed solution B.
3) 2mmol is weighed as sulphur source using thioacetamide, be added in mixed solution B, carry out magnetic agitation
After 15min, and ultrasonic 15min is carried out, forms solution C.
4) concentration prepared is used to be acidified for the HCl solution of 0.05mol/L to solution C, using PH tester into
Row detection, after the solution PH of whole system is adjusted to PH=2.5, then carries out ultrasonic 10min, forms mixed solution D.
5) solution D being added in the liner of polytetrafluoroethylene (PTFE), 33%, reaction temperature is controlled at 160 DEG C for packing ratio control,
Reaction time controls in 4h.
6) to after the reaction was completed, distinguish centrifuge washing 4 times through deionized water and ethyl alcohol.Then 40~60 DEG C of vacuum drying 2h
Afterwards, ground that Zn can be obtained0.2Cd0.8S material powder.
Embodiment 3
1) CMC is weighed a certain amount of, is made into the solution (36ml) of 3g/L, after carrying out magnetic agitation 3h, carries out ultrasound
30min forms solution A.
2) Zinc diacetate dihydrate (Zn (Ac) is used2·2H2) and Cadmium diacetate dihydrate (Zn (Cd) O2·2H2It O) is raw material
(nZn:nCd=1:1), 0.5mmol is weighed respectively, is added in solution A, after carrying out magnetic agitation 15min, and carries out ultrasound
30min forms mixed solution B.
3) 3mmol is weighed as sulphur source using thioacetamide, be added in mixed solution B, carry out magnetic agitation
After 15min, and ultrasonic 30min is carried out, forms solution C.
4) it uses the concentration prepared to be acidified for the HCl solution of 0.1mol/L to solution C, is carried out using PH tester
Detection, after the solution PH of whole system is adjusted to PH=3.0, then carries out ultrasonic 20min, forms mixed solution D.
5) solution D being added in the liner of polytetrafluoroethylene (PTFE), 36%, reaction temperature is controlled at 180 DEG C for packing ratio control,
Reaction time controls in 6h.
6) to after the reaction was completed, distinguish centrifuge washing 6 times through deionized water and ethyl alcohol.Then after 60 DEG C of vacuum drying 3h,
It is ground that Zn can be obtained0.2Cd0.8S material powder.
As can be seen from Figure 1 sample prepared by embodiment 3 respectively corresponds standard card PDF#49-1302
(Zn0.2Cd0.8S).The line of its diffraction maximum is respectively in 24.835 ° of correspondence (100) crystal faces, 26.526 ° of correspondence (002) crystal faces,
28.203 ° of correspondence (101) crystal faces.It can also be seen that the crystallinity of the material and object are mutually preferable from XRD diagram.From Fig. 2
Know the nano-particle diameter size about 500nm or so of the material.Micron ball can be formed by the assembling between little particle
Zn0.2Cd0.8S powder.
Claims (8)
1. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble, which comprises the following steps:
Step 1: it weighs sodium carboxymethylcellulose and H is added2In O, it is made into the solution of 1~3g/L, is then successively stirred and surpasses
Sonication forms mixed solution A；
Step 2: according to nZn:nCdThe ratio of=1:1 weighs Zn (Ac)2·2H2O and Cd (Ac)2·2H2Mixed solution A is added in O
In, and sodium carboxymethylcellulose and Zn (Ac)2·2H2The ratio of O be (0.036~0.108g): (0.1~0.5mmol), then according to
It is secondary to be stirred and be ultrasonically treated, form mixed solution B；
Step 3: thioacetamide is weighed as sulphur source, is added in mixed solution B, wherein thioacetamide and Zn (Ac)2·
2H2The molar ratio of O is (1~3): (0.1~0.5) is then successively stirred and is ultrasonically treated, and forms mixed solution C；
Step 4: being acidified mixed solution C using HCl solution, and the pH of mixed solution C is made to be adjusted to 2.0~3.0, then into
Row ultrasonic treatment, forms mixed solution D；
Step 5: mixed solution D is added in the liner of polytetrafluoroethylene (PTFE) and carries out hydro-thermal reaction, hydrothermal reaction condition is as follows: filling out
It fills than control 30%~36%, at 140 DEG C~180 DEG C, the reaction time is controlled in 2h~6h for reaction temperature control；
Step 6: to after the reaction was completed, product be distinguished centrifuge washing several times through deionized water and ethyl alcohol, then drying and grinding
Obtain Zn0.2Cd0.8S material powder.
2. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, feature
It is, mixing time is 1~3h in step 1, and sonication treatment time is 5~30min.
3. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, feature
It is, mixing time is 15min in step 2, and sonication treatment time is 5~30min.
4. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, feature
It is, mixing time is 15min in step 3, and sonication treatment time is 5~30min.
5. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, feature
It is, the concentration of HCl solution is 0.01~0.1mol/L in step 4.
6. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, feature
It is, the time being ultrasonically treated in step 4 is 5~20min.
7. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, feature
It is, product is distinguished centrifuge washing 3~6 times through deionized water and ethyl alcohol in step 6.
8. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, feature
Be, it is dry in step 6 specifically: 40~60 DEG C at a temperature of be dried in vacuo 1~3h.
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| CN108675339B (en) * | 2018-07-24 | 2020-02-07 | 陕西科技大学 | Preparation method of rodlike self-assembled spherical zinc-cadmium-sulfur solid solution material |
| CN109574065B (en) * | 2019-01-22 | 2020-12-08 | 陕西科技大学 | Foliaceous Zn0.2Cd0.8Preparation method of S material |
Citations (2)
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| CN101254467A (en) * | 2008-04-11 | 2008-09-03 | 浙江大学 | Precipitating-hydrothermal preparation with high visible light catalytic activity nano CdxZn1-xS photocatalyst |
| CN104941666A (en) * | 2015-06-19 | 2015-09-30 | 哈尔滨工业大学 | Method for preparing CdxZn1-xS solid solution photocatalyst provided with cubic sphalerite structure and corresponding to visible light |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254467A (en) * | 2008-04-11 | 2008-09-03 | 浙江大学 | Precipitating-hydrothermal preparation with high visible light catalytic activity nano CdxZn1-xS photocatalyst |
| CN104941666A (en) * | 2015-06-19 | 2015-09-30 | 哈尔滨工业大学 | Method for preparing CdxZn1-xS solid solution photocatalyst provided with cubic sphalerite structure and corresponding to visible light |
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| Enhanced photocatalytic activity for hydrogen evolution from water by Zn0.5Cd0.5S/WS2 heterostructure;Haitao Zhao et al.;《Materials Science in Semiconductor Processing》;20161205;第59卷;第68-75页 |
| Hong Du et al..Bare Cd1−xZnxS ZB/WZ Heterophase Nanojunctions for Visible Light Photocatalytic Hydrogen Production with High Efficiency.《ACS Appl. Mater. Interfaces》.2016,第8卷第24550-24558页. |
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