CN109411553A - A kind of method and application of low temperature preparation copper zinc sulphur nano thin-film - Google Patents
A kind of method and application of low temperature preparation copper zinc sulphur nano thin-film Download PDFInfo
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- CN109411553A CN109411553A CN201810072754.6A CN201810072754A CN109411553A CN 109411553 A CN109411553 A CN 109411553A CN 201810072754 A CN201810072754 A CN 201810072754A CN 109411553 A CN109411553 A CN 109411553A
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- Prior art keywords
- solution
- copper zinc
- preparation
- dimethyl sulfoxide
- copper
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- FENQZYRPJMQVRW-UHFFFAOYSA-N [Cu]S[Zn] Chemical compound [Cu]S[Zn] FENQZYRPJMQVRW-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims description 8
- 239000010409 thin film Substances 0.000 title description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000012528 membrane Substances 0.000 claims abstract description 17
- 239000002105 nanoparticle Substances 0.000 claims abstract description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000280 densification Methods 0.000 claims abstract description 6
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 5
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims abstract description 5
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- 235000010378 sodium ascorbate Nutrition 0.000 claims abstract description 5
- 229960005055 sodium ascorbate Drugs 0.000 claims abstract description 5
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims abstract description 5
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims abstract description 5
- 239000004246 zinc acetate Substances 0.000 claims abstract description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 239000012046 mixed solvent Substances 0.000 claims abstract description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-O pyridinium Chemical compound C1=CC=[NH+]C=C1 JUJWROOIHBZHMG-UHFFFAOYSA-O 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000004528 spin coating Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 3
- 239000011229 interlayer Substances 0.000 claims 1
- 229920000642 polymer Polymers 0.000 claims 1
- 239000011521 glass Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 16
- 239000010408 film Substances 0.000 description 12
- 230000005540 biological transmission Effects 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- QEZYDNSACGFLIC-UHFFFAOYSA-N CN.[I] Chemical compound CN.[I] QEZYDNSACGFLIC-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- LBSAHBJMEHMJTN-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Zn].[Zn] LBSAHBJMEHMJTN-UHFFFAOYSA-N 0.000 description 1
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical group [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
Abstract
The present invention relates to a kind of copper zinc sulphur nanometer grain preparation method and its applications.Its preparation method includes the following steps: for copper acetate, zinc acetate and sodium ascorbate to be dissolved in dimethyl sulfoxide, is configured to solution, sublimed sulfur is dissolved in the mixed solvent, is configured to solution, by above two solution hybrid reaction.Completely reacted solution settles with acetone and uses deionized water redisperse, is repeated twice, obtained copper zinc sulphur nano particle dimethyl sulfoxide or pyridinium dissolution.The solution of preparation is spin-coated on pretreated electro-conductive glass, and smooth densification, the copper zinc-sulfur membrane of even uniform can be obtained.The smooth densification of copper zinc-sulfur membrane of the invention, even uniform, and preparation method is safe, simple, low in cost and environmental-friendly.
Description
Technical field
The present invention relates to copper zinc sulphur technical field of nanometer material preparation, and in particular to a kind of low temperature preparation copper zinc sulphur nanometer thin
The method and its application of film.
Background technique
Copper zinc sulphur is a kind of material that can be applied well by large-scale commercial applications.Copper zinc sulphur nano particle is a kind of combination
Alloy material of the copper sulfide with zinc sulphide structure, therefore be considered as a kind of good inorganic p-type semiconductors material.Because its
Outstanding performance in terms of p-type semiconductor material, including energy level appropriate, good electric conductivity, the stability of height, non-toxic inexpensive
And the advantages that easily preparing, copper zinc sulphur is utilized as solar cell interface material.However high performance solar battery is to boundary
The quality requirement of face material filming is very high, good therefore, it is necessary to obtain a kind of quality of forming film, and electric conductivity is high, low-cost copper
Zinc-sulfur membrane preparation method, to improve the performance of solar battery.
Summary of the invention
In view of the shortcomings of the prior art, that it is an object of the present invention to provide a kind of quality of forming film is good, electric conductivity is high, low-cost copper
Zinc-sulfur membrane preparation method and applications can get smooth densification using this method, and the film of even uniform has operation letter
Single, low in cost advantage, and good effect is obtained as hole transmission layer in perovskite solar battery.
The following steps are included:
(1) copper acetate, zinc acetate and sodium ascorbate are dissolved in dimethyl sulfoxide, are configured to solution;
(2) by sublimed sulfur be dissolved in mixed solvent (dimethyl sulfoxide: NN dimethylformamide: ethyl alcohol=10: in 1: 2),
It is configured to solution;
(3) solution that step (2) is configured to is added in the solution that step (1) is configured to, and heats 3 at 160 DEG C
Hour;
(4) solution completely reacted in step (3) is settled with acetone and is used deionized water redisperse, repeat this operation two
It is secondary;
(5) the copper zinc sulphur nano particle dimethyl sulfoxide or pyridinium dissolution obtained step (4);
(6) solution prepared by step (5) is spin-coated on pretreated electro-conductive glass, smooth densification can be obtained,
The copper zinc-sulfur membrane of even uniform.
The present invention provides the copper zinc-sulfur membranes to answer in perovskite solar battery as hole transport layer material
Related data.
The invention has the following advantages that
1) raw material economics, safety that the present invention uses, material preparation process are environmentally protective.
2) in the present invention, copper zinc-sulfur membrane is synthesized by easy step spin-coating method, and method is simple, low in cost, can
On a large scale, use is prepared in large area.
3) the obtained copper zinc-sulfur membrane of the present invention can obtain high efficiency perovskite solar-electricity as hole transmission layer
Pond.
Detailed description of the invention
Fig. 1: figure a, b are the high resolution transmission electron microscope figure of copper zinc sulphur nano particle produced by the present invention;Scheming c is
The X-ray diffractogram of copper zinc sulphur nano particle obtained;Scheme the Raman spectrogram that d is copper zinc sulphur nano particle obtained;
Fig. 2: CH3NH3PbI3The scanning electron microscope microscope figure (SEM) of film.
Specific embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1
A kind of preparation method of copper zinc-sulfur membrane, includes the following steps:
(1) copper acetate, zinc acetate and sodium ascorbate are dissolved in dimethyl sulfoxide, are configured to solution;
(2) sublimed sulfur is dissolved in mixed solvent (dimethyl sulfoxide: n,N-Dimethylformamide: ethyl alcohol=10: 1: 2)
In, it is configured to solution;
(3) solution that step (2) is configured to is added in the solution that step (1) is configured to, and heats 3 at 160 DEG C
Hour;
(4) solution completely reacted in step (3) is settled with acetone and is used deionized water redisperse, repeat this operation two
It is secondary;
(5) the copper zinc sulphur nano particle dimethyl sulfoxide or pyridinium dissolution obtained step (4);
(6) solution prepared by step (5) is spin-coated on pretreated substrate, smooth densification can be obtained, it is smooth
Uniform copper zinc-sulfur membrane.
The preparation of embodiment 2, copper zinc sulphur nanometer particle film
It is 2mg/ml that the copper zinc sulphur solution that embodiment 1 is prepared, which is diluted to concentration, and 80uL solution is taken to be spin-coated on cleaning
On clean ITO electro-conductive glass, revolving speed 3000rpm/min, time 60s.Spin coating is complete to put its film on hot plate, and 140 DEG C are moved back
Fiery 15min obtains copper zinc-sulfur membrane.
The characterization of copper zinc-sulfur membrane of the present invention:
Fig. 1 (a), 1 (b) is the high resolution transmission electron microscope figure of copper zinc sulphur nano particle produced by the present invention, can
To obtain copper zinc sulphur nanoparticle size about in 4nm or so.
Fig. 1 (c) is copper zinc sulphur powder of nanometric particles;The structure for determining copper zinc sulphur is analyzed with X-ray diffractometer, as a result as schemed
Shown in c, determine that material is copper zinc sulphur.
Fig. 1 (d) is the Raman spectrogram of the copper zinc sulphur nano particle of copper zinc sulphur nano particle obtained.As a result such as Fig. 1 (d)
It is shown, determine that material is copper zinc sulphur.
Embodiment 3 prepares CH on copper zinc-sulfur membrane3NH3PbI3Film
Iodine methylamine and lead iodide are dissolved in 1mL mixed solution DMF and DMSO (volume ratio 4: 1) dissolution, obtain CH3NH3PbI3
Precursor solution will take the 90uL prepared CH3NH3PbI3It is thin that precursor solution is added drop-wise to the copper zinc sulphur prepared in embodiment 2
On film.Spin coating revolving speed 4500rpm/min, spin-coating time 30s.450uL chlorobenzene is added dropwise in spin coating, then reheats and adds for 80 DEG C on plate
CH is made after cooling in hot 10min3NH3PbI3Film, by the CH3NH3PbI3Film is scanned Electronic Speculum microscope figure (SEM) survey
Examination.
CH is found out in Fig. 23NH3PbI3The crystallite dimension that film is spin-coated on generally is greater than 1um.
Claims (7)
1. a kind of preparation method of copper zinc-sulfur membrane, includes the following steps:
(1) copper acetate, zinc acetate and sodium ascorbate are dissolved in dimethyl sulfoxide, are configured to solution.
(2) sublimed sulfur is dissolved in mixed solvent (dimethyl sulfoxide: n,N-Dimethylformamide: ethyl alcohol), is configured to solution.
(3) solution that step (2) is configured to is added in the solution that step (1) is configured to, and is heated 3 hours at 160 DEG C.
(4) solution completely reacted in step (3) is settled with acetone and is used deionized water redisperse, repeat this operation twice.
(5) the copper zinc sulphur nano particle dimethyl sulfoxide or pyridinium dissolution obtained step (4).
(6) solution prepared by step (5) is spin-coated on pretreated substrate, smooth densification, even uniform can be obtained
Copper zinc-sulfur membrane.
2. preparation method according to claim 1, it is characterised in that: the copper acetate, zinc acetate and sodium ascorbate
It is dissolved in dimethyl sulfoxide with 1: 0.5: 1.5 molar ratio.
3. preparation method according to claim 1 or 2, it is characterised in that: dimethyl sulfoxide: n,N-Dimethylformamide:
Ethyl alcohol=10: 1: 2.
4. preparation method according to claim 1, it is characterised in that: the spin speed is 3000~4000rpm/min;
Spin-coating time is 45~65s.
5. preparation method described in any one of -4 according to claim 1, it is characterised in that: the substrate is ITO, FTO, flexibility
Electrode.
6. according to claim 1 the copper zinc-sulfur membrane of -5 the methods preparation as interlayer materials answering in solar cells
With wherein the copper zinc-sulfur membrane is as hole mobile material.
7. application according to claim 6, it is characterised in that: the solar battery is perovskite solar battery,
Polymer solar battery.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115522165A (en) * | 2022-09-02 | 2022-12-27 | 深圳市志凌伟业光电有限公司 | Manufacturing process of vehicle window heating film |
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Cited By (2)
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CN115522165A (en) * | 2022-09-02 | 2022-12-27 | 深圳市志凌伟业光电有限公司 | Manufacturing process of vehicle window heating film |
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Application publication date: 20190301 |