CN110482594A - Cu2CdSnS4Micro-nano material and preparation method - Google Patents
Cu2CdSnS4Micro-nano material and preparation method Download PDFInfo
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- CN110482594A CN110482594A CN201910861516.8A CN201910861516A CN110482594A CN 110482594 A CN110482594 A CN 110482594A CN 201910861516 A CN201910861516 A CN 201910861516A CN 110482594 A CN110482594 A CN 110482594A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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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- C01P2004/51—Particles with a specific particle size distribution
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The invention discloses a kind of Cu2CdSnS4Micro-nano material and preparation method, are synthesized using two-step method, the Cd being first coordinated using sodium citrate2+、Sn4+The white intermediate of generation is reacted with aqueous slkali；Thiocarbamide is added into the white intermediate again as sulphur source, polyvinylpyrrolidone adds copper source as surfactant, using microwave irradiation synthesis it is micro-/receive Cu2CdSnS4, it is the flower-shaped Cu that the size that is assembled by the nanometer sheet of 20-30nm is 500-600nm2CdSnS43D hierarchical structure, Cu obtained2CdSnS4There is dispersibility well in organic solvent, will there is important application value in fields such as solar cell optics.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, are related to a kind of Cu2CdSnS4Micro-nano material and preparation method, tool
Body is related to a kind of 3D-Cu2CdSnS4It is micro-/to receive material and preparation method.
Background technique
Cu2CdSnS4With biggish absorption coefficient (104cm-1), band gap 1.4eV, according to unijunction solar cell
Shockleye-Queisser limiting efficiency, Cu2CdSnS4Band gap ratio Cu2ZnSnS41.5eV band gap closer to sunlight
The ideal bandgap 1.34eV of absorption.And Cu2CdSnS4Hole mobility, electric conductivity and stability with higher, it is intrinsic
P-type semiconductor, p-type electric conductivity belongs to the position receptor defects of the vacancy Cu and copper in cadmium, thus can be used as hole transport
Material.Compared to hole mobile material spiro-OMeTAD and PEDOT:PSS expensive in current perovskite solar cell,
It has synthesis conveniently, the advantages such as cheap.Currently, synthesis Cu2CdSnS4The method of use is mostly conventional solution preparation side
Method generally comprises solvent heat/hydrothermal synthesis and hot injection method etc., and solvent heat/hydrothermal synthesis method needs the longer reaction time, heat
Injection method reaction process is more complicated, and Cu synthesized by these methods2CdSnS4It is mostly spherical.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of Cu2CdSnS4Micro-nano material and preparation method, using two
Footwork synthesis, the Cd being first coordinated using sodium citrate2+、Sn4+The white intermediate for generating hydroxyl is reacted with aqueous slkali；Again to
Thiocarbamide is added in the white intermediate as sulphur source, polyvinylpyrrolidone adds copper source as surfactant, and utilization is micro-
Wave radiation method synthesis it is micro-/receive classification Cu2CdSnS4, it is the 3D hierarchical structure for being assembled by 2D nanometer sheet and being formed, due to its uniqueness
Design feature, make it that there is special advantage in solar cell application, as 3D it is micro-/the big cavity of material center received can mention
The utilization efficiency of bloom；Also, 2D nanometer sheet can also provide direct electron propagation ducts, reduce the compound phenomenon of electronics.
Technical solution provided by the invention are as follows:
A kind of 3D-Cu2CdSnS4Micro-/to receive the preparation method of material, the preparation method comprises the following steps:
(1) cadmium salt, sodium citrate are dissolved in deionized water, obtain solution A, pink salt is dissolved in ethyl alcohol and obtains solution B；
(2) solution A is mixed with solution B, aqueous slkali is added dropwise until precipitating generation, then through centrifugation, washing, drying, obtains
To white intermediate；
(3) white intermediate, thiocarbamide, mantoquita and polyvinylpyrrolidone are dissolved in ethylene glycol, carry out microwave reaction, instead
After answering, through centrifugation, washing, drying, the 3D-Cu is obtained2CdSnS4It is micro-/to receive material.
Further, in step (3), the condition of the microwave reaction is to react 5- at 600-800W, 170-180 DEG C
20min, preferably 800W, 5min is reacted at 180 DEG C.Microwave radiation causes the linear distribution of dipole or ion in the electric field,
Conducive to kinetics and promote homogeneous formation, than traditional reactive mode, it is easier to reach in a short time more preferably
Temperature.
In step (1), the cadmium salt is four nitric hydrate cadmiums；The pink salt is Tin tetrachloride pentahydrate；The aqueous slkali
For sodium hydroxide solution or potassium hydroxide solution.
In step (1), the ratio between the cadmium salt, amount of substance of sodium citrate are 1:1.
In step (1), the concentration of the cadmium salt in deionized water is 0.05-0.1mol/L, preferably 0.1mol/L.
The concentration of the pink salt in ethanol is 0.1-0.2mol/L, preferably 0.2mol/L；The solution A, solution B
Concentration ratio is 1:2.
In step (2), the concentration of the aqueous slkali is 0.5-2mol/L, preferably 2mol/L.
In step (3), the mantoquita is Copper dichloride dihydrate.
In step (3), the ratio between the white intermediate, amount of substance of thiocarbamide, mantoquita are 1:10:2~1:25:2, preferably
For 1:25:2；
In step (3), concentration of the mantoquita in ethylene glycol is 0.05-0.1mol/L, preferably 0.05mol/L；Institute
Stating concentration of the polyvinylpyrrolidone in ethylene glycol is 0.005mg/mL.
The present invention also provides the 3D-Cu that the preparation method is prepared2CdSnS4It is micro-/to receive material, it is described
Cu2CdSnS4Micro-/material of receiving is that the size being assembled by the nanometer sheet of 20-30nm is the flower-shaped Cu of 500-600nm2CdSnS4Point
Level structure, crystal phase are stannite Cu2CdSnS4Structure, wherein the atomic ratio of Cu:Cd:Sn:S is 2.7:1:0.9:4.6.
In preparation method disclosed by the invention, sodium citrate and Cd are utilized2+Coordination, under the action of highly basic with Sn4+Jointly
Sedimentation, raw glomerate white intermediate.Then, in the solvent of ethylene glycol, the white intermediate and thiocarbamide hydrolyze generation
H2S reaction generates CdS, SnS2, meanwhile, the H that thiocarbamide hydrolysis generates2S is again by the Cu of rear addition2+It is reduced to Cu+Afterwards it is in connection at
Cu2S, these binary sulfides, which combine, generates Cu2CdSnS4Nucleus, PVP selective oriented growth effect under, Jiang Yante
Fixed direction grows into 3D-Cu2CdSnS4.The method of the present invention is using conventional consersion unit (mainly microwave synthesizer) short
Rapid synthesis is realized in time；Obtained 3D-Cu2CdSnS4There is dispersibility well in organic solvent, using it as hole
Perovskite solar cell made by transport layer has certain J-V performance, is expected to have in fields such as solar cells very big
Application potential.
Compared with prior art, preparation method provided by the invention is simple, easy to operate, quickly；Synthesized 3D-
Cu2CdSnS4Pattern, size are more uniform.
Detailed description of the invention
Fig. 1 is the SEM figure of the white intermediate in the embodiment of the present invention 1；
Fig. 2 is stannite structure 3D-Cu prepared by the embodiment of the present invention 12CdSnS4SEM figure；
Fig. 3 is stannite structure 3D-Cu prepared by the embodiment of the present invention 12CdSnS4TEM figure；
Fig. 4 is stannite structure 3D-Cu prepared by the embodiment of the present invention 12CdSnS4XRD spectra；
Fig. 5 is stannite structure 3D-Cu prepared by the embodiment of the present invention 12CdSnS4Raman spectrogram；
Fig. 6 is stannite structure 3D-Cu prepared by the embodiment of the present invention 12CdSnS4XPS spectrum figure；
Fig. 7 is stannite structure 3D-Cu prepared by the embodiment of the present invention 12CdSnS4Dispersibility in ethyl alcohol and chloroform
Figure.
Fig. 8 is stannite structure 3D-Cu prepared by the embodiment of the present invention 12CdSnS4Hole as perovskite solar cell
Battery J-V performance prepared by transport layer.
Specific embodiment
A kind of 3D-Cu2CdSnS4It is micro-/to receive the preparation method of material, comprising the following steps:
(1) by 0.01mol Cd (NO3)2·4H2O, 0.01mol sodium citrate is dissolved in 100mL water, obtains solution A；It will
0.01mol SnCl4·5H2O is dissolved in 50mL ethyl alcohol, obtained solution B；
(2) solution A is mixed with solution B, the NaOH solution of 2mol/L is added dropwise to precipitating is generated, through centrifugation, washing, drying
White intermediate is made afterwards；Its SEM figure is as shown in Figure 1, as can be seen from the figure it is average grain diameter in the spherical of 100nm or so
Particle；
(3) by 0.5mmol white intermediate, 12.5mmol thiocarbamide, 1mmol CuCl2·2H2O, 0.1g polyvinylpyrrolidine
Ketone is dissolved in 20mL ethylene glycol, reacts 5min at microwave 800W, 180 DEG C.Be centrifugated after cooling through 8000-10000rpm,
Stannite structure 3D-Cu is obtained with ethanol washing and vacuum drying2CdSnS4。
Scanning electron microscope (SEM) figure of product is as shown in Fig. 2, show that product is flower-shaped 3D points that nanometer sheet is assembled into
Level structure, size 500-600nm.
Transmission electron microscope (TEM) photo of product is as shown in figure 3, further demonstrate that product is the flower of 600nm or so
Shape hierarchical structure is formed by by the nanometer sheet assembling of 20-30nm.
Powder x-ray diffraction (XRD) data of product are consistent with JCPDS card #29-0537, show product as yellow tin
Mine Cu2CdSnS4, see Fig. 4.
The Raman spectrum of product is as shown in figure 5, there are two the Raman of feature displacement, i.e. 331cm in figure-1、286cm-1,
Corresponding stannite type Cu2CdSnS4A1 mode, further confirm the product be stannite Cu2CdSnS4。
The photoelectron spectroscopy test chart of product is as shown in fig. 6, Cu2p is split into Cu2p in figure3/2(932eV) and Cu2p1/2
(951.8eV), break-up energy difference are 19.8eV, show that the existence form of Cu is Cu (I)；Cd3d is split into Cd3d5/2
(404.8eV)、Cd3d3/2(411.5eV), break-up energy difference are 6.7eV, show that the existence form of Cd is Cd (II)；Sn3d division
For Sn3d5/2(486.1eV) and Sn3d3/2(494.5eV), break-up energy difference are 8.4eV, show that the existence form of Sn is Sn
(IV)；S2p is split into S2p3/2(161.35eV) and S2p1/2(162.35eV), break-up energy difference are 1.00eV, illustrate that S exists.
The test of element ratio shows that its atomic ratio is Cu:Cd:Sn:S=2.7:1:0.9:4.6 in the XPS of product.To sum up prove institute's shape
At be Cu2CdSnS4。
Fig. 7 is synthesized Cu2CdSnS4Dispersibility experiment, by Cu2CdSnS4Be dispersed in respectively ethyl alcohol (Fig. 7 a left) and
In chloroform (Fig. 7 a is right), after for 24 hours, Cu is found2CdSnS4Sedimentation (Fig. 7 b is left) completely in ethanol, but in chloroform still
It can disperse (Fig. 7 b is right) well.
Fig. 8 is to utilize synthesized Cu2CdSnS4Battery device made by hole transmission layer as perovskite solar cell
J-V performance.3D-Cu is dissolved with chlorobenzene first2CdSnS4, make its concentration 1mg/mL, by the dispersant liquid drop of 100 μ L clean
ITO substrate on, 4000rpm spin coating 30s；Then by the PbI of 690mg2With 220mg CH3NH3I mixture is dissolved in DMF:DMSO
In the mixed liquor of=4:1, stirred at 60 DEG C after 1~2h after membrane filtration with 0.22 μm, with first step 1000rpm spin coating 10s,
Second step 6000rpm spin coating 30s, in second step last 10-15s, the anti-solvent chlorobenzene of 100 μ L of fast drop, is moved back at 100 DEG C
Fiery 10min；Then, the chlorobenzene solution of the PCBM of 20mg/mL is prepared, with 2000rpm spin coating 30s, in 80 DEG C of annealing 10min；Again
The ethanol solution for preparing the rhodamine of 0.5mg/mL, by the solution of 100uL with 4000rpm spin coating 30s；Finally steamed with thermal evaporation
Plate the Ag electrode of 100nm.Prepared battery is ITO/3D-Cu2CdSnS4/CH3NH3PbI3/PCBM/Rhodamine/Ag.It should
The V of batteryocFor 0.82V, JscFor 14.03mA/cm2, FF 60.76%, PCE 6.99%.
Above-mentioned reference embodiment is to Cu2CdSnS4The detailed description that micro-nano material and preparation method carry out, be it is illustrative and
It is not restrictive, several embodiments can be enumerated according to limited range, therefore in the case where not departing from present general inventive concept
Change and modification, should belong within protection scope of the present invention.
Claims (10)
1. a kind of 3D-Cu2CdSnS4It is micro-/to receive the preparation method of material, which is characterized in that the preparation method comprises the following steps:
(1) cadmium salt, sodium citrate are dissolved in deionized water, obtain solution A, pink salt is dissolved in solution B obtained in ethyl alcohol；
(2) solution A is mixed with solution B, aqueous slkali is added dropwise until precipitating generation, then through centrifugation, washing, drying, obtains white
Color intermediate；
(3) white intermediate, thiocarbamide, mantoquita and polyvinylpyrrolidone are dissolved in ethylene glycol, carry out microwave reaction, reaction knot
Shu Hou obtains the 3D-Cu through centrifugation, washing, drying2CdSnS4It is micro-/to receive material.
2. preparation method according to claim 1, which is characterized in that in step (3), the condition of the microwave reaction is
5-20min is reacted at 600-800W, 170-180 DEG C.
3. preparation method according to claim 1 or 2, which is characterized in that in step (1), the cadmium salt is four hydration nitre
Sour cadmium；The pink salt is Tin tetrachloride pentahydrate；Aqueous slkali is sodium hydroxide solution or potassium hydroxide solution.
4. preparation method according to claim 1 or 2, which is characterized in that in step (1), the cadmium salt, sodium citrate
The ratio between amount of substance is 1:1.
5. preparation method according to claim 1 or 2, which is characterized in that in step (1), the cadmium salt is in deionized water
In concentration be 0.05-0.1mol/L；The concentration of the pink salt in ethanol is 0.1-0.2mol/L；The solution A, solution B
The ratio between concentration be 1:2.
6. preparation method according to claim 1 or 2, which is characterized in that in step (2), the concentration of the aqueous slkali is
0.5-2mol/L。
7. preparation method according to claim 1 or 2, which is characterized in that in step (3), the mantoquita is two hydration chlorine
Change copper.
8. preparation method according to claim 1 or 2, which is characterized in that in step (3), the white intermediate, sulphur
The ratio between amount of substance of urea, mantoquita is 1:10:2~1:25:2.
9. preparation method according to claim 1 or 2, which is characterized in that in step (3), the mantoquita is in ethylene glycol
Concentration be 0.05-0.1mol/L；Concentration of the polyvinylpyrrolidone in ethylene glycol is 0.005g/mL.
10. a kind of 3D-Cu that preparation method as described in any one of claims 1-9 is prepared2CdSnS4It is micro-/to receive material,
It is characterized in that, the Cu2CdSnS4Micro-/material of receiving is that the size being assembled by the nanometer sheet of 20-30nm is 500-600nm
Flower-shaped Cu2CdSnS4Hierarchical structure, crystal phase are stannite Cu2CdSnS4Structure, wherein the atomic ratio of Cu:Cd:Sn:S be
2.7:1:0.9:4.6。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111766280A (en) * | 2020-06-01 | 2020-10-13 | 济南大学 | Preparation method and application of photoelectrochemical immunosensor based on tin disulfide/cadmium sulfide |
| CN113823747A (en) * | 2020-06-18 | 2021-12-21 | Tcl科技集团股份有限公司 | Nano material, preparation method thereof and light-emitting diode |
| CN115367785A (en) * | 2022-08-23 | 2022-11-22 | 安徽工程大学 | High-efficiency photocatalyst micro/nano-thorn spherical indium sulfide and preparation method and application thereof, indium sulfide composite membrane and preparation method and application thereof |
-
2019
- 2019-09-12 CN CN201910861516.8A patent/CN110482594B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| HAO GUAN ET AL.: ""Quaternary Cu2CdSnS4 nanoparticles synthesised by microwave irradiation method"", 《MICRO & NANO LETTERS》 * |
| WEI WANG ET AL.: ""Effects of sulfur sources on properties of Cu2ZnSnS4 nanoparticles"", 《J NANOPART RES》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111766280A (en) * | 2020-06-01 | 2020-10-13 | 济南大学 | Preparation method and application of photoelectrochemical immunosensor based on tin disulfide/cadmium sulfide |
| CN113823747A (en) * | 2020-06-18 | 2021-12-21 | Tcl科技集团股份有限公司 | Nano material, preparation method thereof and light-emitting diode |
| CN115367785A (en) * | 2022-08-23 | 2022-11-22 | 安徽工程大学 | High-efficiency photocatalyst micro/nano-thorn spherical indium sulfide and preparation method and application thereof, indium sulfide composite membrane and preparation method and application thereof |
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