CN109368685A - A kind of preparation method of the p-type cuprous iodide film of highly transparent conduction - Google Patents
A kind of preparation method of the p-type cuprous iodide film of highly transparent conduction Download PDFInfo
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- CN109368685A CN109368685A CN201811335104.2A CN201811335104A CN109368685A CN 109368685 A CN109368685 A CN 109368685A CN 201811335104 A CN201811335104 A CN 201811335104A CN 109368685 A CN109368685 A CN 109368685A
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- film
- cuprous iodide
- iodine
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- copper film
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/04—Halides
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention discloses a kind of preparation methods of the p-type cuprous iodide film of highly transparent conduction, belong to transparent conductive film material preparation and p-type semiconductor material application field.It is characterized in that processing step is as follows: (1) by thermal evaporation, the copper film of various thickness can be grown on the substrate surfaces such as glass, plastics；(2) the p-type cuprous iodide film of highly transparent conduction is prepared using the ethanol solution of iodine by copper film iodate by solution at room temperature method.Preparation method of the present invention have many advantages, such as it is high-efficient, at low cost, can be mass-produced, prepared cuprous iodide film have transparency height, good conductivity, can transporting holes carrier.
Description
Technical field
The present invention relates to a kind of preparation methods of the p-type cuprous iodide film of highly transparent conduction, especially realize room
Under temperature by copper film iodate be cuprous iodide film.
Background technique
Cuprous iodide is a kind of simple p-type inorganic semiconductor material of component, has excellent optically and electrically characteristic,
Band gap width is 3.1eV, and carrier mobility is up to 40cm2V-1s-1, exciton bind energy 62meV, in the wave of 400~1000nm
Transmitance is up to 80% or more in long range.Based on the above advantage, cuprous iodide is a kind of to answer photoelectricity and energy field are great
With the p-type thin film material of value.As the patent CN201610209921.8 and CN201610209913.3 that have authorized are all based on
The composite conducting fiber of cuprous iodide preparation, CN201510277818.2 utilize cuprous iodide synthetic compound luminescent material,
Cuprous iodide is applied to catalytic field by CN201110345147.0, and CN201611103654.2 is disclosed based on cuprous iodide
Solar battery.But to realize industrial applications, the method for preparing cuprous iodide film also needs to improve.Preparation iodate at present is sub-
The method of Copper thin film mainly has magnetron sputtering method, thermal evaporation, chemical synthesis and copper film iodide process.Due to magnetron sputtering method and
To instrument seriously corroded, chemical synthesis quality of forming film is low, is not appropriate for industrial life for the valuableness of equipment needed for thermal evaporation, iodine vapor
It produces.Common copper film iodide process is one layer of copper film of deposition in substrate, and then copper film is placed in high temperature iodine vapor and is reacted, this
The copper film translucency that method is prepared is poor, and needs high temperature iodine vapor, is unfavorable for industrializing.A kind of method of invention
Simply, the low-cost method for preparing cuprous iodide film.
Summary of the invention
It is an object of the invention to overcome the shortcomings of above-mentioned existing technologies, a kind of ethanol solution using iodine is provided by copper film
Iodate is the method for cuprous iodide film, more importantly this method can be realized at room temperature.
Specific step is as follows for the technical solution adopted in the present invention:
(1) by thermal evaporation, one layer of copper film is grown in substrate surface；
(2) iodine is dissolved in ethyl alcohol, prepares the ethanol solution of iodine；
(3) copper film is immersed in the ethanol solution of iodine, is cleaned after taking-up with ethyl alcohol, obtain cuprous iodide film.
Substrate can be glass, plastics, sheet metal in the step (1), wherein using plastics as substrate can get it is flexible, can
The copper film of folding.
Copper film thickness is can be controlled between 5~800nm in the step (1).
The ethanol solution concentration of iodine is 0.8mMol/L to supersaturated solution in the step (2)
Growth temperature is room temperature (5~35 DEG C) in the step (3).
Beneficial effects of the present invention: providing a kind of simple copper film iodide process, can be in the substrate surfaces such as glass or plastics
Prepare the cuprous iodide film of various thickness.The present invention is simple, reproducible, at low cost, and prepared iodate is sub-
Copper thin film transparency height, good conductivity, can satisfy the application in terms of transparent electrode and photoelectric device.
Detailed description of the invention
Fig. 1 film of the present invention grows flow diagram
The XRD spectrum for the cuprous iodide film that Fig. 2 is prepared in method in attached drawing 1.
Fig. 3 based on different original depth copper films, through ethyl alcohol iodine solution processing after obtain cuprous iodide film it is saturating
Cross map.
The cuprous iodide film that Fig. 4 is handled by the ethyl alcohol iodine solution of various concentration penetrates map.
The resistivity picture for the cuprous iodide film that Fig. 5 is handled by the ethyl alcohol iodine solution of various concentration.
The contents of the present invention are described in further detail with reference to the accompanying drawing, but the spy that the present invention is not limited to be exemplified below
Usual practice.
Embodiment
Attached drawing 1 is film growth flow diagram of the present invention.One is deposited on glass, plastics or sheet metal surface
Layer copper film, copper film is immersed in the ethanol solution of iodine, is cleaned after taking-up with ethyl alcohol, and it is sub- to can be obtained transparent, p-type electric-conducting iodate
Copper thin film.
Attached drawing 2 is the XRD spectrum of the cuprous iodide film prepared in method in attached drawing 1.Map shows that the method can obtain
Must have highly crystalline quality, free from admixture phase, high crystal orientation cuprous iodide film.
Attached drawing 3 is the obtained cuprous iodide film after the processing of ethyl alcohol iodine solution based on different original depth copper films
Penetrate map.The corresponding initial copper film thickness of difference curve is respectively 20nm, 25nm, 30nm, 35nm, 40nm in figure.
Attached drawing 4 is the cuprous iodide film handled by the ethyl alcohol iodine solution of various concentration through map.In figure
The ethanol solution concentration of the corresponding iodine of different curves is respectively 0.8mMol/L, 4mMol/L, 8mMol/L and 20mMol/L.
Fig. 5 is the resistivity picture of the cuprous iodide film handled by the ethanol solution of various concentration iodine.Ethyl alcohol
Iodine solution concentration distinguishes 0.8mMol/L, 4mMol/L, 8mMol/L, and corresponding resistivity is respectively 0.59 Ω cm, 0.04 Ω
Cm and 0.1 Ω cm.
Embodiment 1 (using glass as substrate grown cuprous iodide film)
(1) glass is cut into the shape and size of any needs, makes glass surface wash with distilled water, is dried for standby.
(2) by thermal evaporation, the copper film of one layer of 40nm thickness is grown in glass surface.
(3) iodine is dissolved in ethyl alcohol, compound concentration is the ethanol solution of the iodine of 4mMol/L.
(4) copper film is immersed in ethyl alcohol iodine solution about 10 seconds, is cleaned after taking-up with ethyl alcohol, it is thin can be obtained cuprous iodide
Film.
Embodiment 2 (using plastics as substrate grown cuprous iodide film)
(1) plastics are cut into the shape and size of any needs, make frosting wash with distilled water, are dried spare.
(2) by thermal evaporation, the copper film of one layer of 40nm thickness is grown in frosting.
(3) iodine is dissolved in ethyl alcohol, compound concentration is the ethanol solution of the iodine of 4mMol/L.
(4) copper film is immersed in ethyl alcohol iodine solution about 10 seconds, is cleaned after taking-up with ethyl alcohol, it is thin can be obtained cuprous iodide
Film.
Embodiment 3 (without the preparation of the cuprous iodide film of thickness)
(1) using glass or the material of other materials as substrate, the shape and size of needs are cut into, clean base surface,
It is dried for standby.
(2) by thermal evaporation, in the copper film of glass surface growth different-thickness, thickness from 20nm be sequentially increased to
25nm、30nm、35nm、40nm。
(3) iodine is dissolved in ethyl alcohol, compound concentration is the ethanol solution of the iodine of 4mMol/L.
(4) copper film is immersed in ethyl alcohol iodine solution about 10 seconds, is cleaned after taking-up with ethyl alcohol, can be obtained different-thickness
Cuprous iodide film.
To sum up experimental result may be implemented to prepare in substrate surfaces such as glass, plastics or metals through the invention various
The cuprous iodide film of thickness, translucency are more than 73%, and resistivity is less than 0.04 Ω cm.Preparation process is simple, it is at low cost,
Sample repeatability is good, performance is stable, has important application value in fields such as transparent conductive electrode, photoelectric devices.
Claims (6)
1. a kind of preparation method of the p-type cuprous iodide film of highly transparent conduction, it is characterised in that its processing step is as follows:
(a) by thermal evaporation, the copper film (5~800nm) of various thickness can be grown on the substrate surfaces such as glass, plastics；
(b) by solution at room temperature method, using the ethanol solution of iodine by copper film iodate, the p-type iodate for preparing highly transparent conduction is sub-
Copper thin film.
2. preparation method according to claim 1, it is characterised in that: using the ethanol solution of iodine, at room temperature by copper film
The p-type cuprous iodide film of highly transparent conduction is prepared in iodate.
3. base material according to claim 1, it is characterised in that: substrate can be glass, plastics, sheet metal, wherein
It can get flexible, folding electrically conducting transparent cuprous iodide film by substrate of plastics.
4. copper film thickness according to claim 1, it is characterised in that: copper film thickness is between 5~800nm.
5. the ethanol solution of iodine according to claim 1, it is characterised in that: solution is the ethanol solution for having dissolved iodine, molten
Liquid concentration can be 0.8mMol/L (0.8 mM every liter) to supersaturated solution.
6. growth temperature according to claim 1, it is characterised in that: growth temperature is room temperature (5~35 DEG C).
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| CN201811335104.2A CN109368685A (en) | 2018-11-10 | 2018-11-10 | A kind of preparation method of the p-type cuprous iodide film of highly transparent conduction |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109979675A (en) * | 2019-03-12 | 2019-07-05 | 天津大学 | A kind of preparation method of high transmittance p-type cupric iodide transparent conductive film |
| WO2021232577A1 (en) * | 2020-05-20 | 2021-11-25 | 中国科学院微电子研究所 | Method for preparing copper iodide thin film |
| CN113699506A (en) * | 2020-05-20 | 2021-11-26 | 中国科学院微电子研究所 | Preparation method of cuprous iodide film |
| CN113699505A (en) * | 2020-05-20 | 2021-11-26 | 中国科学院微电子研究所 | Preparation method of doped cuprous iodide film |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102368503A (en) * | 2011-10-17 | 2012-03-07 | 清华大学 | CNT (carbon nano tube)-silicon heterojunction solar cell and manufacturing method thereof |
| CN108677155A (en) * | 2018-05-23 | 2018-10-19 | 哈尔滨工业大学 | A method of preparing cuprous iodide p-type transparent semiconductor film material at room temperature |
-
2018
- 2018-11-10 CN CN201811335104.2A patent/CN109368685A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102368503A (en) * | 2011-10-17 | 2012-03-07 | 清华大学 | CNT (carbon nano tube)-silicon heterojunction solar cell and manufacturing method thereof |
| CN108677155A (en) * | 2018-05-23 | 2018-10-19 | 哈尔滨工业大学 | A method of preparing cuprous iodide p-type transparent semiconductor film material at room temperature |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109979675A (en) * | 2019-03-12 | 2019-07-05 | 天津大学 | A kind of preparation method of high transmittance p-type cupric iodide transparent conductive film |
| WO2021232577A1 (en) * | 2020-05-20 | 2021-11-25 | 中国科学院微电子研究所 | Method for preparing copper iodide thin film |
| CN113699506A (en) * | 2020-05-20 | 2021-11-26 | 中国科学院微电子研究所 | Preparation method of cuprous iodide film |
| CN113699505A (en) * | 2020-05-20 | 2021-11-26 | 中国科学院微电子研究所 | Preparation method of doped cuprous iodide film |
| CN113699506B (en) * | 2020-05-20 | 2022-08-30 | 中国科学院微电子研究所 | Preparation method of cuprous iodide film |
| CN113699505B (en) * | 2020-05-20 | 2022-08-30 | 中国科学院微电子研究所 | Preparation method of doped cuprous iodide film |
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