CN107697944A - 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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- CN107697944A CN107697944A CN201710866509.8A CN201710866509A CN107697944A CN 107697944 A CN107697944 A CN 107697944A CN 201710866509 A CN201710866509 A CN 201710866509A CN 107697944 A CN107697944 A CN 107697944A
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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 method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble, CMC wiring solution-formings are weighed, is then stirred and is ultrasonically treated successively, form mixed solution A；Zinc diacetate dihydrate and Cadmium diacetate dihydrate are weighed, is added in mixed solution A, is then stirred and is ultrasonically treated successively, forms mixed solution B；Thioacetamide is weighed as sulphur source, is added in mixed solution B；Then it is stirred and is ultrasonically treated successively, forms mixed solution C；Mixed solution C is acidified using HCl solution, then is ultrasonically treated, forms mixed solution D；Mixed solution D is added in the liner of polytetrafluoroethylene (PTFE) and carries out hydro-thermal reaction；After the completion of question response, product is distinguished into centrifuge washing several times through deionized water and ethanol, 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 technology
Nowadays, with the development of scientific and technological industry and Aero-Space, building and electronic applications etc., the requirement to material is got over
Carrying out higher, traditional material can not meet to require, and the development that increasing functional material and composite 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 cells
Scape and receive much concern always, wherein Zn1-xCdxCatalysis material of S (0≤x≤1) solid-solution materials as novelty, because it can
The energy gap of conversion and the catalytic activity of uniqueness 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 amounts
Increase, its energy gap are gradually lowered to 2.3eV from 3.6eV, just because of its appropriate energy gap, can be good at making
With a certain amount of visible ray in sunshine and the black light of a part.And it has cheap and easy to get, chemical stability
The advantages of strong and anti-light corrosion, just aroused 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 material and other photoelectric fields
In.
In recent years, with for Zn1-xCdxS researchs are goed deep into, and researcher learns that its structure and performance are made with it
Standby method has close contact.It is normal with coprecipitation, microemulsion method and thermal decomposition method etc. according to the exploration of people
Zn has successfully been prepared in rule method1-xCdxS solid solution.
At present, 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 technique is simple to operation, and product quality is excellent, but for temperature
Requirement it is higher, energy consumption is larger, and product is easily sintered or is melted, reaction it is not easily-controllable.Microemulsion method technological operation
Relatively simple, device simple operations facilitate uniform particle, but have substantial amounts of organic matter and produce, and certain shadow is had to environment
Ring, cause environmental pollution, the more difficult control of reaction rate, it is also necessary to processing of the increase to byproduct of reaction so that the cost of reaction
Increase.Thermal decomposition method operation is simple, and reaction rate is fast, but easily causes product reunion, and temperature needed for reaction is higher, to production
Required energy and cost requirement are higher.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble, with gram
The problem of prior art is present is taken, present invention preparation cost is low, short preparation period, and it is new to prepare good crystallinity, pattern
The Zn of grain husk0.2Cd0.8S material.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of spherical Zn of particles self assemble0.2Cd0.8The preparation method of S material, comprises the following steps：
Step 1：Weigh CMC and add H2In O, 1~3g/L solution is made into, is then stirred and is ultrasonically treated successively,
Form mixed solution A；
Step 2：According to nZn:nCd=1：1 ratio weighs Zn (Ac)2·2H2O and Zn (Cd)2·2H2O, it is molten to add mixing
In liquid A, and CMC and Zn (Ac)2·2H2O ratio is (0.036~0.108g)：(0.1~0.5mmol), is then stirred successively
Supersound process is mixed and stirred, forms mixed solution B；
Step 3：Thioacetamide is weighed as sulphur source, is added in mixed solution B, wherein thioacetyl and Zn (Ac)2·
2H2O mol ratio is (1~3)：(0.1~0.5), then it is stirred and is ultrasonically treated successively, forms mixed solution C；
Step 4：Mixed solution C is acidified using HCl solution, then is ultrasonically treated, forms mixed solution D；
Step 5：Mixed solution D is added in the liner of polytetrafluoroethylene (PTFE) and carries out hydro-thermal reaction；
Step 6：After the completion of question response, product is distinguished into centrifuge washing several times through deionized water and ethanol, 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：Packing ratio control is 30%~36%, reaction temperature control
At 140 DEG C~180 DEG C, the reaction time is controlled in 2h~6h.
Further, product distinguishes centrifuge washing 3~6 times through deionized water and ethanol in step 6.
Further, drying is specially in step 6：1~3h is dried in vacuo at a temperature of 40~60 DEG C.
Compared with prior art, the present invention has technique effect beneficial below：
The Zn that preparation technology of the present invention is simple, cost is low, the cycle is short while prepared0.2Cd0.8S material be little particle from
The nanometer assembled is spherical, and it has larger specific surface area, therefore the electric transmission 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 tens to hundreds of nanometers, and material
Purity is high, crystallinity is strong, can apply in fields such as photocatalytic degradation organic matter, photodissociation aquatic products hydrogen or electronic light emitting devices,
Good economic benefit and social benefit are obtained, because the performance comparision of material is excellent, its application also can preferably be developed.
Further, Zn is prepared using hydro-thermal method0.2Cd0.8S material, technological operation are simple, it is not necessary to large-scale reaction
Equipment, under hydrothermal conditions, water can work as a kind of chemical constituent and participate in reaction, be 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
Formed and modified.Both one pack system tiny crystals can be prepared, bi-component or multi-component special compound powder can be prepared again.Hydro-thermal
The characteristics of method produces is particle purity height, good dispersion, good crystalline and can control that production cost is low, the powder prepared with hydro-thermal method
Body typically without sintering, is advantageous to depollution of environment etc..This can avoids in sintering process that crystal grain can grow up and impurity holds
The shortcomings of being easily mixed into.The different performances to material of thing phase and appearance structure have large effect, and the inventive method is by zinc salt
(Zn(Ac)2·2H2) and cadmium salt (Zn (Cd) O2·2H2O it is) water-soluble in CMC (sodium carboxymethylcellulose) with thioacetamide (TAA)
Hydro-thermal reaction is carried out under the acid condition of liquid to obtain product.
Brief description of the drawings
Fig. 1 be example 3 of the present invention by technique hydro-thermal method synthesize Zn0.2Cd0.8The XRD of S material；
Fig. 2 is that example 3 of the present invention synthesizes Zn by hydro-thermal method0.2Cd0.8The SEM figures of S material.
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, comprises the following steps：
1) CMC is weighed a certain amount of, is made into 1~3g/L solution (36ml), after carrying out 1~3h of magnetic agitation, is surpassed
5~30min of sound, form mixed solution A.
2) Zinc diacetate dihydrate (Zn (Ac) is used2·2H2) and Cadmium diacetate dihydrate (Zn (Cd) O2·2H2O) it 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 is entered
Row 5~30min of ultrasound, forms mixed solution B.
3) 1~3mmol is weighed, is added among mixed solution B, carries out magnetic agitation as sulphur source using thioacetamide
After 15min, and 5~30min of ultrasound is carried out, form mixed solution C.
4) concentration prepared is used to be acidified for 0.01~0.1mol/L HCl solution to mixed solution C, using PH
Tester is detected, and is adjusted after the solution PH of whole system 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) after the completion of question response, centrifuge washing is distinguished 3~6 times through deionized water and ethanol.Then 40~60 DEG C of vacuum are done
It is ground to can obtain Zn after dry 1~3h0.2Cd0.8S material powder.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
1) CMC is weighed a certain amount of, is made into 1g/L solution (36ml), after carrying out magnetic agitation 1h, carries out ultrasonic 5min,
Form solution A.
2) Zinc diacetate dihydrate (Zn (Ac) is used2·2H2) and Cadmium diacetate dihydrate (Zn (Cd) O2·2H2O) it 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, form mixed solution B.
3) 1mmol is weighed, is added among mixed solution B, carries out magnetic agitation as sulphur source using thioacetamide
After 15min, and ultrasonic 5min is carried out, form solution C.
4) use the concentration prepared to be acidified for 0.01mol/L HCl solution to solution C, entered using PH testers
Row detection, is adjusted to PH=2.0 after the solution PH of whole system, 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 is controlled in 2h.
6) after the completion of question response, centrifuge washing is distinguished 3 times through deionized water and ethanol.Then after 40 DEG C of vacuum drying 1h,
It is ground to can obtain Zn0.2Cd0.8S material powder.
Embodiment 2
1) CMC is weighed a certain amount of, is made into 2g/L solution (36ml), after carrying out magnetic agitation 2h, carries out ultrasound
15min, form solution A.
2) Zinc diacetate dihydrate (Zn (Ac) is used2·2H2) and Cadmium diacetate dihydrate (Zn (Cd) O2·2H2O) it 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, form mixed solution B.
3) 2mmol is weighed, is added among mixed solution B, carries out magnetic agitation as sulphur source using thioacetamide
After 15min, and ultrasonic 15min is carried out, form solution C.
4) use the concentration prepared to be acidified for 0.05mol/L HCl solution to solution C, entered using PH testers
Row detection, is adjusted to PH=2.5 after the solution PH of whole system, 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 is controlled in 4h.
6) after the completion of question response, centrifuge washing is distinguished 4 times through deionized water and ethanol.Then 40~60 DEG C of vacuum drying 2h
Afterwards, it is ground to can obtain Zn0.2Cd0.8S material powder.
Embodiment 3
1) CMC is weighed a certain amount of, is made into 3g/L solution (36ml), after carrying out magnetic agitation 3h, carries out ultrasound
30min, form solution A.
2) Zinc diacetate dihydrate (Zn (Ac) is used2·2H2) and Cadmium diacetate dihydrate (Zn (Cd) O2·2H2O) it 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, form mixed solution B.
3) 3mmol is weighed, is added among mixed solution B, carries out magnetic agitation as sulphur source using thioacetamide
After 15min, and ultrasonic 30min is carried out, form solution C.
4) use the concentration prepared to be acidified for 0.1mol/L HCl solution to solution C, carried out using PH testers
Detection, is adjusted to PH=3.0 after the solution PH of whole system, 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 is controlled in 6h.
6) after the completion of question response, centrifuge washing is distinguished 6 times through deionized water and ethanol.Then after 60 DEG C of vacuum drying 3h,
It is ground to can obtain Zn0.2Cd0.8S material powder.
As can be seen from Figure 1 sample corresponds to standard card PDF#49-1302 respectively prepared by embodiment 3
(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 thing are mutually preferable from XRD.From Fig. 2
Understand 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 powders.
Claims (10)
1. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble, it is characterised in that comprise the following steps：
Step 1：Weigh CMC and add H2In O, 1~3g/L solution is made into, is then stirred and is ultrasonically treated successively, is formed
Mixed solution A；
Step 2：According to nZn:nCd=1：1 ratio weighs Zn (Ac)2·2H2O and Zn (Cd)2·2H2O, add mixed solution A
In, and CMC and Zn (Ac)2·2H2O ratio is (0.036~0.108g)：(0.1~0.5mmol), be then stirred successively and
It is ultrasonically treated, forms mixed solution B；
Step 3：Thioacetamide is weighed as sulphur source, is added in mixed solution B, wherein thioacetyl and Zn (Ac)2·2H2O
Mol ratio be (1~3)：(0.1~0.5), then it is stirred and is ultrasonically treated successively, forms mixed solution C；
Step 4：Mixed solution C is acidified using HCl solution, then is ultrasonically treated, forms mixed solution D；
Step 5：Mixed solution D is added in the liner of polytetrafluoroethylene (PTFE) and carries out hydro-thermal reaction；
Step 6：After the completion of question response, product is distinguished into centrifuge washing several times through deionized water and ethanol, 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, its 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, its 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, its 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, its 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, its feature
It is, is adjusted the PH of mixed solution C to 2.0~3.0 using HCl solution in step 4.
7. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, its feature
It is, the time being ultrasonically treated in step 4 is 5~20min.
8. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, its feature
It is, hydrothermal reaction condition is as follows in step 5：30%~36%, reaction temperature is controlled 140 DEG C~180 for packing ratio control
DEG C, the reaction time is controlled in 2h~6h.
9. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, its feature
It is, product distinguishes centrifuge washing 3~6 times through deionized water and ethanol in step 6.
10. a kind of preparation method of the spherical zinc cadmium sulphur solid-solution material of particles self assemble according to claim 1, its feature
Be, in step 6 drying be specially：1~3h is dried in vacuo at a temperature of 40~60 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108675339A (en) * | 2018-07-24 | 2018-10-19 | 陕西科技大学 | A kind of preparation method of the glomerate zinc cadmium sulphur solid-solution material of rodlike self assembly |
| CN109574065A (en) * | 2019-01-22 | 2019-04-05 | 陕西科技大学 | The foliated Zn of one type0.2Cd0.8The preparation method of S material |
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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 |
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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 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675339A (en) * | 2018-07-24 | 2018-10-19 | 陕西科技大学 | A kind of preparation method of the glomerate zinc cadmium sulphur solid-solution material of rodlike self assembly |
| CN109574065A (en) * | 2019-01-22 | 2019-04-05 | 陕西科技大学 | The foliated Zn of one type0.2Cd0.8The preparation method of S material |
| CN109574065B (en) * | 2019-01-22 | 2020-12-08 | 陕西科技大学 | Foliaceous Zn0.2Cd0.8Preparation method of S material |
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