CN106629820A - Controllable preparation method of Cu2ZnSnS4 nano-crystalline material - Google Patents
Controllable preparation method of Cu2ZnSnS4 nano-crystalline material Download PDFInfo
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- CN106629820A CN106629820A CN201610813712.4A CN201610813712A CN106629820A CN 106629820 A CN106629820 A CN 106629820A CN 201610813712 A CN201610813712 A CN 201610813712A CN 106629820 A CN106629820 A CN 106629820A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/006—Compounds containing, besides tin, two or more other elements, with the exception of oxygen or hydrogen
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- 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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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/51—Particles with a specific particle size distribution
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention belongs to the technical field of a nano material and a nano technology, and more specifically relates to a controllable preparation method of a Cu2ZnSnS4 nano-crystalline material. The preparation method comprises the following steps: adding copper acetate, zinc acetate and stannic chloride in oleylamine, introducing argon as protection gas, stirring copper acetate, zinc acetate and stannic chloride under certain temperature for completely dissolving the materials to obtain a complexation solution of metal salt; heating the complexation solution of metal salt to set temperature, adding a diphenyl ether solution of thiocarbanilide; after the reaction is complete, cooling the material to the room temperature, cleaning the reaction products by methanol to obtain the Cu2ZnSnS4 nano-crystalline material. The method selects thiocarbanilide as a sulfur source, employs a heat injection method to prepare the Cu2ZnSnS4 nano-crystalline material, the Cu2ZnSnS4 nano-crystalline material is obtained by controlling the addition proportion of the precursor, and the Cu2ZnSnS4 nano-crystallines with different size is obtained by controlling the reaction temperature and the reaction time.
Description
Technical field
The invention belongs to nano material and field of nanometer technology, and in particular to a kind of Cu2ZnSnS4Nanocrystalline material can
Control Preparation Method.
Background technology
With the change of size, the characteristic such as its optics, electricity significantly change to semiconductor nano material can occur.When receiving
When being smaller in size than its Bohr radius of meter Jing, it may appear that unique quantum size effect.Therefore, semiconductor nano material grinds
Study carefully of great interest, and prospect is widely used in fields such as solar cell, light emitting diodes.At present,
The nanocrystalline materials such as cadmium sulfide, vulcanized lead have been obtained for extensive research, and its good physical property makes it have widely
Using.Cu2ZnSnS4As a kind of polynary semi-conducting material, with the higher absorption coefficient of light (>104cm-1) and suitable forbidden band
Width (~1.5eV), changing the ratio of different elements can obtain Cu of different nature2ZnSnS4Material so as to huge
Application potential.Meanwhile, element contained by the material is nontoxic and rich reserves elements, with cheap and eco-friendly
Characteristic, therefore, study Cu2ZnSnS4Nanocrystalline material has important academic and using value.At present, Cu2ZnSnS4It is nanocrystalline
The preparation of material is generally using elemental sulfur as sulphur source presoma so that higher temperature and longer is needed in preparation process
Reaction time.In addition, such preparation process easily generates Cu2SnS3Deng dephasign.Therefore, simple Cu is found2ZnSnS4Nanometer
The preparation method of brilliant material has great importance.
The content of the invention
The present invention is directed to the deficiencies in the prior art, it is therefore intended that provide a kind of Cu2ZnSnS4Nanocrystalline material can
Control Preparation Method.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of Cu2ZnSnS4The controllable method for preparing of nanocrystalline material, it is characterised in that comprise the steps:
(1) copper acetate, zinc acetate, butter of tin are added in oleyl amine, are passed through argon gas protective gas, at a certain temperature
Stirring is completely dissolved copper acetate, zinc acetate, butter of tin, obtains the complex solution of slaine;
(2) complex solution of above-mentioned slaine is heated to into design temperature, the diphenyl ether for being subsequently adding rhenocure CA is molten
Liquid is reacted;
(3) after reaction terminates, room temperature is cooled to, adds methyl alcohol to clean to reacting products therefrom, obtain Cu2ZnSnS4
Nanocrystalline material.
In such scheme, the mol ratio of the copper acetate, zinc acetate and butter of tin is 2:1:1.
In such scheme, on the basis of 1mol copper acetates, the volume of the oleyl amine is 20mL.
In such scheme, step (1) temperature is:50~100 DEG C, the time of the stirring is 5~30 minutes.
In such scheme, step (2) temperature is 100~300 DEG C, and the time of the reaction is 1~60min.
In such scheme, in the hexichol ethereal solution of step (2) rhenocure CA, the concentration of rhenocure CA is
1mol/L。
In such scheme, the volume of the complex solution of step (2) slaine and the hexichol ethereal solution of rhenocure CA
Than for 20:3~8.
The arbitrary preparation method of claim 1~7 prepares gained Cu2ZnSnS4Nanocrystalline material.
Beneficial effects of the present invention:It is sulphur source that the present invention chooses rhenocure CA, and using hot injection method Cu is prepared2ZnSnS4
Nanocrystalline material, the ratio added by controlling presoma obtains Cu2ZnSnS4Nanocrystalline material;By controlling reaction temperature and
Reaction time obtains various sizes of Cu2ZnSnS4It is nanocrystalline.Preparation method process is simple of the present invention, favorable reproducibility, cost
It is cheap, meet environmental requirement.
Description of the drawings
Fig. 1 is the Cu that the present invention is prepared2ZnSnS4The thing phase characterization result of nanocrystalline material, wherein a is XRD spectrum,
B is EDS collection of illustrative plates.
Fig. 2 is the Cu that embodiment 1 is prepared2ZnSnS4The TEM image of nanocrystalline material, wherein a are TEM image, and b is
Nanocrystalline size distribution plot in figure a.
Fig. 3 is the Cu that embodiment 2 is prepared2ZnSnS4The TEM image of nanocrystalline material, wherein a are TEM image, and b is
Nanocrystalline size distribution plot in figure a.
Fig. 4 is the Cu that embodiment 3 is prepared2ZnSnS4The TEM image of nanocrystalline material, wherein a are TEM image, and b is
Nanocrystalline size distribution plot in figure a.
Fig. 5 is the Cu that embodiment 4 is prepared2ZnSnS4The TEM image of nanocrystalline material, wherein a are TEM image, and b is
Nanocrystalline size distribution plot in figure a.
Fig. 6 is the Cu that embodiment 5 is prepared2ZnSnS4The TEM image of nanocrystalline material, wherein a are TEM image, and b is
Nanocrystalline size distribution plot in figure a.
Fig. 7 is the Cu that embodiment 6 is prepared2ZnSnS4The TEM image of nanocrystalline material, wherein a are TEM image, and b is
Nanocrystalline size distribution plot in figure a.
Specific embodiment
For a better understanding of the present invention, below in conjunction with the accompanying drawings, embodiment further elucidates present disclosure, but this
Bright content is not limited solely to the following examples.
Embodiment 1
Cu2ZnSnS4The controllable method for preparing of nanocrystalline material, comprises the steps:
(1) 2mmol copper acetates, 1mmol zinc acetates, 1mmol butters of tin are added in 20mL oleyl amines, are passed through argon gas guarantor
Shield gas, control temperature is completely dissolved copper acetate, zinc acetate, butter of tin at 50 DEG C, and with quick stirring 5 minutes, obtains
To the complex solution of slaine;
(2) 3mL, concentration are added in above-mentioned metal salt solution for the hexichol ethereal solution of 1mol/L rhenocure CAs, heating
React 1 minute to 100 DEG C of design temperature;
(3) after reaction terminates, room temperature is cooled to, the Cu for adding substantial amounts of methyl alcohol to obtain reaction2ZnSnS4It is nanocrystalline to carry out
Cleaning, obtains Cu2ZnSnS4Nanocrystalline material.
The present embodiment prepares Cu2ZnSnS4The particle size of nanocrystalline material is 1.9nm, and its TEM image is shown in Fig. 2
(a)。
Embodiment 2
Cu2ZnSnS4The controllable method for preparing of nanocrystalline material, comprises the steps:
(1) 2mmol copper acetates, 1mmol zinc acetates, 1mmol butters of tin are added in 20mL oleyl amines, are passed through argon gas guarantor
Shield gas, control temperature is completely dissolved copper acetate, zinc acetate, butter of tin at 60 DEG C, and with quick stirring 10 minutes,
Obtain the complex solution of slaine;
(2) 4mL, concentration are added in above-mentioned metal salt solution for the hexichol ethereal solution of 1mol/L rhenocure CAs, heating
React 5 minutes to 140 DEG C of design temperature;
(3) after reaction terminates, room temperature is cooled to, the Cu for adding substantial amounts of methyl alcohol to obtain reaction2ZnSnS4It is nanocrystalline to carry out
Cleaning, obtains Cu2ZnSnS4Nanocrystalline material.
The present embodiment prepares Cu2ZnSnS4The particle size of nanocrystalline material is 3.9nm, and its TEM image is shown in Fig. 3
(a)。
Embodiment 3
Cu2ZnSnS4The controllable method for preparing of nanocrystalline material, comprises the steps:
(1) 2mmol copper acetates, 1mmol zinc acetates, 1mmol butters of tin are added in 20mL oleyl amines, are passed through argon gas guarantor
Shield gas, control temperature is completely dissolved copper acetate, zinc acetate, butter of tin at 70 DEG C, and with quick stirring 15 minutes,
Obtain the complex solution of slaine;
(2) 5mL, concentration are added in above-mentioned metal salt solution for the hexichol ethereal solution of 1mol/L rhenocure CAs, heating
React 10 minutes to 180 DEG C of design temperature;
(3) after reaction terminates, room temperature is cooled to, the Cu for adding substantial amounts of methyl alcohol to obtain reaction2ZnSnS4It is nanocrystalline to carry out
Cleaning, obtains Cu2ZnSnS4Nanocrystalline material.
The present embodiment prepares Cu2ZnSnS4The particle size of nanocrystalline material is 5.5nm, and its TEM image is shown in Fig. 4
(a)。
Embodiment 4
Cu2ZnSnS4The controllable method for preparing of nanocrystalline material, comprises the steps:
(1) 2mmol copper acetates, 1mmol zinc acetates, 1mmol butters of tin are added in 20mL oleyl amines, are passed through argon gas guarantor
Shield gas, control temperature is completely dissolved copper acetate, zinc acetate, butter of tin at 80 DEG C, and with quick stirring 20 minutes,
Obtain the complex solution of slaine;
(2) 6mL, concentration are added in above-mentioned metal salt solution for the hexichol ethereal solution of 1mol/L rhenocure CAs, heating
React 20 minutes to 220 DEG C of design temperature;
(3) after reaction terminates, room temperature is cooled to, the Cu for adding substantial amounts of methyl alcohol to obtain reaction2ZnSnS4It is nanocrystalline to carry out
Cleaning, obtains Cu2ZnSnS4Nanocrystalline material.
The present embodiment prepares Cu2ZnSnS4The particle size of nanocrystalline material is 6.6nm, and its TEM image is shown in Fig. 5
(a)。
Embodiment 5
Cu2ZnSnS4The controllable method for preparing of nanocrystalline material, comprises the steps:
(1) 2mmol copper acetates, 1mmol zinc acetates, 1mmol butters of tin are added in 20mL oleyl amines, are passed through argon gas guarantor
Shield gas, control temperature is completely dissolved copper acetate, zinc acetate, butter of tin at 90 DEG C, and with quick stirring 25 minutes,
Obtain the complex solution of slaine;
(2) 7mL, concentration are added in above-mentioned metal salt solution for the hexichol ethereal solution of 1mol/L rhenocure CAs, heating
React 30 minutes to 260 DEG C of design temperature;
(3) after reaction terminates, room temperature is cooled to, the Cu for adding substantial amounts of methyl alcohol to obtain reaction2ZnSnS4It is nanocrystalline to carry out
Cleaning, obtains Cu2ZnSnS4Nanocrystalline material.
The present embodiment prepares Cu2ZnSnS4The particle size of nanocrystalline material is 7.9nm, and its TEM image is shown in Fig. 6
(a)。
Embodiment 6
Cu2ZnSnS4The controllable method for preparing of nanocrystalline material, comprises the steps:
(1) 2mmol copper acetates, 1mmol zinc acetates, 1mmol butters of tin are added in 20mL oleyl amines, are passed through argon gas guarantor
Shield gas, control temperature is completely dissolved copper acetate, zinc acetate, butter of tin at 100 DEG C, and with quick stirring 30 minutes,
Obtain the complex solution of slaine;
(2) 8mL, concentration are added in above-mentioned metal salt solution for the hexichol ethereal solution of 1mol/L rhenocure CAs, heating
React 60 minutes to 300 DEG C of design temperature;
(3) after reaction terminates, room temperature is cooled to, the Cu for adding substantial amounts of methyl alcohol to obtain reaction2ZnSnS4It is nanocrystalline to carry out
Cleaning, obtains Cu2ZnSnS4Nanocrystalline material.
The present embodiment prepares Cu2ZnSnS4The particle size of nanocrystalline material is 8.7nm, and its TEM image is shown in Fig. 7
(a)。
Cu prepared by the present invention2ZnSnS4The XRD spectrum of nanocrystalline material, EDS collection of illustrative plates are shown in Fig. 1.XRD spectrum in Fig. 1 (a)
The position of shown each diffraction maximum and relative intensity are and Cu2ZnSnS4XRD spectrum match, EDS collection of illustrative plates shows it in Fig. 1 (b)
Element ratio and Cu2ZnSnS4Stoichiometric proportion can preferably coincide, illustrate synthesize product be Cu2ZnSnS4Material.
The Cu that the embodiment of the present invention 1~6 is prepared2ZnSnS4The appearance structure of nanocrystalline material is characterized, and characterizes knot
Fruit sees Fig. 2~7.Fig. 2~7 show by controlling different reaction conditions, can obtain various sizes of Cu2ZnSnS4It is nanocrystalline
Material;Under the conditions of single, nanocrystalline size is more uniform, shows nanocrystalline with preferable monodispersity.
Obviously, above-described embodiment is only intended to clearly illustrate made example, and not to the restriction of embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need to be exhaustive to all of embodiment.And therefore the obvious change amplified or change
Move within still in the protection domain of the invention.
Claims (8)
1. a kind of Cu2ZnSnS4The controllable method for preparing of nanocrystalline material, it is characterised in that comprise the steps:
(1) copper acetate, zinc acetate, butter of tin are added in oleyl amine, are passed through argon gas protective gas, stirred at a certain temperature
Copper acetate, zinc acetate, butter of tin are completely dissolved, the complex solution of slaine is obtained;
(2) complex solution of above-mentioned slaine is heated to into design temperature, adding the hexichol ethereal solution of rhenocure CA is carried out
Reaction;
(3) after reaction terminates, room temperature is cooled to, after adding methyl alcohol to clean reaction products therefrom, obtains Cu2ZnSnS4Receive
The brilliant material of rice.
2. Cu according to claim 12ZnSnS4The controllable method for preparing of nanocrystalline material, it is characterised in that the acetic acid
The mol ratio of copper, zinc acetate and butter of tin is 2:1:1.
3. Cu according to claim 12ZnSnS4The controllable method for preparing of nanocrystalline material, it is characterised in that with 1mol vinegar
On the basis of sour copper, the volume of the oleyl amine is 20mL.
4. Cu according to claim 12ZnSnS4The controllable method for preparing of nanocrystalline material, it is characterised in that step (1)
The temperature is 50~100 DEG C, and the time of the stirring is 5~30 minutes.
5. Cu according to claim 12ZnSnS4The controllable method for preparing of nanocrystalline material, it is characterised in that step (2)
The temperature is 100~300 DEG C, and the time of the reaction is 1~60min.
6. Cu according to claim 12ZnSnS4The controllable method for preparing of nanocrystalline material, it is characterised in that step (2)
In the hexichol ethereal solution of the rhenocure CA, the concentration of rhenocure CA is 1mol/L.
7. Cu according to claim 12ZnSnS4The controllable method for preparing of nanocrystalline material, it is characterised in that step (2)
The complex solution of the slaine is 20 with the volume ratio of the hexichol ethereal solution of rhenocure CA:3~8.
8. the arbitrary preparation method of claim 1~7 prepares gained Cu2ZnSnS4Nanocrystalline material.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109761266A (en) * | 2018-12-27 | 2019-05-17 | 西安交通大学 | A kind of preparation method of auto-dope copper-zinc-tin-sulfur nano-crystalline photoelectric material |
CN111019149A (en) * | 2019-12-12 | 2020-04-17 | 武汉理工大学 | COF-5 one-dimensional rod-like crystal material and preparation method thereof |
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CN103058267A (en) * | 2013-02-03 | 2013-04-24 | 南京邮电大学 | Method for synthesizing copper-zinc-tin-sulfur nano material through hot injection |
CN105164047A (en) * | 2013-03-15 | 2015-12-16 | 纳米技术有限公司 | Cu2ZnSnS4 nanoparticles |
CN105565379A (en) * | 2015-12-07 | 2016-05-11 | 武汉理工大学 | Controllable preparation method of Cu3SbS4 nanocrystalline material |
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2016
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109761266A (en) * | 2018-12-27 | 2019-05-17 | 西安交通大学 | A kind of preparation method of auto-dope copper-zinc-tin-sulfur nano-crystalline photoelectric material |
CN111019149A (en) * | 2019-12-12 | 2020-04-17 | 武汉理工大学 | COF-5 one-dimensional rod-like crystal material and preparation method thereof |
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