CN102603201A - Method for preparing cuprous selenide thin film - Google Patents

Method for preparing cuprous selenide thin film Download PDF

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Publication number
CN102603201A
CN102603201A CN201110290892XA CN201110290892A CN102603201A CN 102603201 A CN102603201 A CN 102603201A CN 201110290892X A CN201110290892X A CN 201110290892XA CN 201110290892 A CN201110290892 A CN 201110290892A CN 102603201 A CN102603201 A CN 102603201A
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film
thin film
selenkupfer
preparation
substrate
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刘科高
石磊
纪念静
田彬
许斌
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Shandong Jianzhu University
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Shandong Jianzhu University
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Abstract

The invention provides a method for preparing a cuprous selenide thin film, belonging to the technical field of photoelectric thin film preparation. The method comprises the following steps: firstly washing a substrate, then putting CuCl2.2H2O and SeO2 into solvents and adjusting the pH value, obtaining a precursor thin film on the substrate by a spin coating method and drying the precursor thin film, putting the precursor thin film into a closed container with diamide hydrate and ensuring the precursor thin film sample not to be contacted with diamide and finally drying, thus obtaining the cuprous selenide photoelectric thin film. The method has the following beneficial effects: the method dispenses with the conditions of high temperature and high vacuum, has low requirements for apparatuses, is low in production cost and high in production efficiency and is easy to operate; the obtained cuprous selenide photoelectric thin film has better continuity and uniformity; and the preparation method which is low in cost and can realize industrialization is provided for preparing the cuprous selenide photoelectric thin film with high performance.

Description

A kind of preparation method of selenkupfer film
Technical field
The invention belongs to the optoelectronic film preparing technical field, relate in particular to a kind of preparation method who prepares the selenkupfer film.
Background technology
Along with society and expanding economy; The development and application clean energy is the important channel of reducing the pollution that the consumption energy brings; Because sun power is the renewable resources of cleaning, safety and environmental protection, so the research of solar cell and application have received the attention of countries in the world.Because key is the thin-film material that constitutes it in the solar cell device; Particularly thin-film material such as absorption layer is determining the efficiency of conversion and the work-ing life of solar cell; Therefore be the research focus in field of new about novel materials such as solar cell absorption layers; Selenide thin film is to have excellent photoelectric performance, can be used to make solar cell.
The selenium compound of copper has several kinds of forms, CuSe for example, Cu 2-δSe (0≤δ＜1), CuSe 2, Cu 3Se 2, Cu 5Se 4Deng.Stoichiometric ratio is different, and crystalline structure also has several kinds of forms such as a cube type, cubic type, six squares.Cu wherein 2-δSe is a P-type semiconductor, indirect band gap band gap width 1.1～1.5eV, direct band gap width 2.0～2.3eV.The value of indirect band gap width extremely adapts to solar battery apparatus.As a kind of important photovaltaic material, the selenkupfer film is widely used in optics, electricity field, for example aspects such as solar cell, spectral filter, nanotube switch, thermoelectricity or photoelectric commutator, conductive electrode, superconductor, vessel transmitter.
The preparation Cu that reports at present 2The method of Se is also less, and the preparation method of copper selenium compound film mainly contains electrochemical method, chemical bath deposition, sonochemistry method, vacuum-evaporation, sputter reaction.Because the raw materials cost of selenkupfer film is low, be a kind of very rising optoelectronic thin film material therefore, but existing operational path is complicated, preparation cost is high, thereby need explores preparation technology cheaply equally.
As method noted earlier, other method also has different defects.Relevant with the present invention also have following document:
[1]Aiyu?Zhang，Qian?Ma，Zhaoguang?Wang，et?al，Controllable?synthesis?of?copper?selenide?nanocrystals?through?a?green?paraffin-acetate?method，Materials?Chemistry?and?Physics?124(2010)916-921.
Preparation CuSe, Cu under non-vacuum condition have mainly been reported 2-δThe nanometer sheet of Se six squares, nano wire etc., and studied the phase structure of the parameter of reaction to product. become to be grouped into, the influence of pattern etc.
[2]G.B.Sakr，I.S.Yahia，M.Fadel，S.S.Fouad，N.Romcevic，Optical?spectroscopy，optical?conductivity，dielectric?properties?and?new?methods?for?determining?the?gap?states?of?CuSe?thin?films，Journal?of?Alloys?and?Compounds?507(2010)557-562.
The main photoelectric properties of having described the CuSe film have been measured the bandwidth of CuSe with diverse ways.
[3]Pushpendra?Kumar，Kedar?Singh，O.N.Srivastava，Template?free-solvothermaly?synthesized?copper?selenide?(CuSe，Cu 2-δSe，β-Cu 2Se?and?Cu 2Se)hexagonal?nanoplates?from?different?precursors?at?low?temperature.
Mainly described under the low temperature with the synthetic CuSe of template solvent-thermal method, Cu 2-δSe, β-Cu 2Se, Cu 2The various copper tin compounds of Se.
[4]S.R.Gosavi，N.G.Deshpande，Y.G.Gudage，Ramphal?Sharma，Physical，optical?and?electrical?properties?of?copper?selenide(CuSe)thin?films?deposited?by?solution?growth?technique?at?room?temperature，Journal?of?Alloys?and?Compounds?448(2008)344-348.
Mainly described under the room temperature and on sheet glass, prepare the CuSe film with the solution growth technology, characterized physics, the optics electric property of film, the energy gap of film is 2.03eV.
[5] Yan Wei, Hu Chenguo, Liu Hong etc., nanometer Cu 2The preparation of Se and growth mechanism analysis thereof, functional materials, 2009 the 3rd phases (40) volume has mainly been reported and has been utilized compound alkali mediator method in meeting the oxyhydroxide molten mass, at 200 ℃ of synthetic Cu 2The Se nanocrystal.This method synthetic Cu 2The Se crystal belongs to isometric system.
[6] woods flies, and the solvent thermal of sulfide epitaxial is grown with property research [D], University Of Suzhou, Suzhou, Jiangsu, in April, 2009.
Mainly reported with solvent-thermal method and on copper base, prepared Cu 2The Se film.Experimental result shows that the change of reaction parameter as changing solvent, tensio-active agent, can change the pattern of film.
[7]P.Peranantham，Y.L.Jeyachandran，C.Viswanathan，N.N.Praveena?et.al，The?effect?of?annealing?on?vacuum-evaporated?copper?selenide?and?indium?telluride?thin?films，Materials?Characterization?58(2007)756-764.
Mainly described and utilized vacuum evaporation technique to prepare copper tin compound and indium tellurium compound film; And studied the influence of annealing temperature to thin film composition and structure and optical property, utilize the direct band gap and the indirect band gap width of the CuSe film of this method preparation to be respectively 1.87～2.03eV and 0.91～0.95eV.
[8]Kegao?Liu，Hong?Liu，JiyangWang，Lei?Shi，Synthesis?and?characterization?of?Cu 2Se?prepared?by?hydrothermal?co-reduction，Journal?of?Alloys?and?Compounds?484(2009)674-676.
Reported that mainly hydrothermal synthesis method is at a lower temperature from CuSO 45H 2O and SeO 2The aqueous solution in prepare Cu 2The Se nanometer powder, and its phase structure and pattern characteristics studied.The Cu for preparing in this article 2The Se powder is six square crystalline structure.
Summary of the invention
The present invention is in order to solve the deficiency of prior art, and invented a kind of and the preparation technology diverse selenkupfer film of preparation method prior art.
The present invention adopts spin coating-chemical co-reducing process to prepare the selenkupfer thin-film material, and adopting soda-lime glass or silicon chip is substrate, with CuCl 22H 2O and SeO 2Be raw material; Two or more mixture with deionized water, ethanol, ammoniacal liquor, these four kinds of raw materials of hydrochloric acid is a solvent; With ammoniacal liquor, hydrochloric acid is the pH value that assist medium is adjusted solution, prepares the certain thickness precursor thin-film that contains copper compound with spin-coating method earlier, is reductive agent with the hydrazine hydrate; Heating at a lower temperature in encloses container makes precursor thin-film reduce concurrent intercrescence and becomes reaction to obtain title product.
Concrete preparation method of the present invention comprises the step of following order:
A. carrying out the cleaning of substrate, is that the substrate of 2mm * 2mm is put into trichloromethane by volume with size: the solution of ethanol=5: 1, ultrasonic cleaning 30min; Again sheet glass, silicon chip are put into acetone: the solution of zero(ppm) water=5: 1, ultrasonic cleaning 30min; In zero(ppm) water, glass substrate is used sonic oscillation 30min again; The above-mentioned sheet glass that obtains or silicon chip be emitted on send in the glass dish in the baking oven, 100 ℃ down oven dry supply the system film to use.
B. with CuCl 22H 2O puts into solvent, fully dissolving, and regulate the pH value.Specifically, can be with 1.5～3.0 parts of CuCl 22H 2O and 1.0～2.0 parts of SeO 2Put into 30～150 parts solvent, solution is mixed, can add the pH value that ammoniacal liquor, hydrochloric acid auxiliary are adjusted solution, wherein solvent is at least two kinds a mixing solutions in deionized water, ethanol, hydrochloric acid, the ammoniacal liquor.
C. make the outside evenly substrate of the said solution of smearing step b, and oven dry, the precursor thin-film sample obtained.Can above-mentioned solution be dripped on the glass substrate that is placed on the sol evenning machine; Restart sol evenning machine with 200～3500 rev/mins of rotation certain hours; After making solution on dripping be coated with evenly, 100 ℃ substrate dried after, repeat once more to drip and dry again after going up aforementioned solution and rotary coating; So repeat 5～15 times, so on substrate, obtained certain thickness precursor thin-film sample.
D. step c gained precursor thin-film sample is placed on the support, but put into the encloses container of hydrazine hydrate, the precursor thin-film sample is not contacted with hydrazine.The hydrazine hydrate of putting into is 15.0～30.0 parts.
E. with the steps d gains, carry out heated drying, obtain the selenkupfer film.Can the above-mentioned encloses container that the precursor thin film sample is housed be put into baking oven, be heated between 160～220 ℃, soaking time 10～20 hours, cool to room temperature takes out then, make its seasoning after, promptly obtain the selenkupfer film;
The present invention does not need the high temperature high vacuum condition, and low to the plant and instrument requirement, production cost is low, and production efficiency is high, easy handling.Gained selenkupfer film has continuity and homogeneity preferably, and the structure of the easy controlled target product of this novel process provides the method that a kind of cost is low, can realize large-scale industrial production for preparing high performance selenkupfer film.
Description of drawings
Accompanying drawing 1 is 200 ℃ of XRD figure spectrums that get down the selenkupfer film behind the reaction 20h at silicon substrate, and the solvent of precursor solution is deionized water, hydrochloric acid.
Embodiment
Embodiment 1
A. the cleaning of glass substrate: (size is 2mm * 2mm) to carry out the glass cleaning substrate as previously mentioned;
B. with 1.54 parts of CuCl 22H 2O and 1 part of SeO 2Put into vial, add 109.09 parts of deionized waters, 36.364 parts of hydrochloric acid utilize more than the ultrasonic vibration 30min, make the material uniform mixing in the solution;
C. above-mentioned solution is dripped on the glass substrate that is placed on the sol evenning machine, restart sol evenning machine, sol evenning machine rotated 5 seconds with 200 rev/mins; With 3000 rev/mins of rotations 15 seconds; After making solution on dripping be coated with evenly, 100 ℃ substrate dried after, repeat once more to drip and dry again after going up aforementioned solution and rotary coating; So repeat 10 times, so on glass substrate, obtained certain thickness precursor thin-film sample;
D. the precursor thin-film sample of above-mentioned technology gained is put into sealable container, and put into 18.182 parts of hydrazine hydrates, the precursor thin film sample places it is not contacted with hydrazine;
E. the above-mentioned encloses container that the precursor thin film sample is housed is put into baking oven, is heated to 180 ℃, soaking time 20 hours, cool to room temperature takes out then, make its seasoning after, promptly obtain the selenkupfer film;
Embodiment 2
A. the cleaning of silicon substrate: (size is 2mm * 2mm) to clean silicon substrate as previously mentioned;
B. with 1.54 parts of CuCl 22H 2O and 1 part of SeO 2Put into the mixing solutions of 14.55 parts of zero(ppm) water, 14.55 parts of hydrochloric acid, utilize more than the ultrasonic vibration 30min, make the material uniform mixing in the solution;
C. above-mentioned solution is dripped on the silicon substrate that is placed on the sol evenning machine, restart sol evenning machine, sol evenning machine rotated 5 seconds with 200 rev/mins; With 3000 rev/mins of rotations 15 seconds; After making solution on dripping be coated with evenly, 100 ℃ substrate dried after, repeat once more to drip and dry again after going up aforementioned solution and rotary coating; So repeat 10 times, so on glass substrate, obtained certain thickness precursor thin-film sample;
D. the precursor thin-film sample of above-mentioned technology gained is put into sealable container, and put into 18.182 parts of hydrazine hydrates, the precursor film sample places it is not contacted with hydrazine;
E. the above-mentioned encloses container that the precursor thin film sample is housed is put into baking oven, is heated to 200 ℃, soaking time 20 hours, cool to room temperature takes out then, make its seasoning after, promptly obtain the selenkupfer film.
Remarks: the experiment among the present invention has obtained Shandong Province institution of higher education plan of science and technology project and has subsidized (No.J11LD10).

Claims (7)

1. the preparation method of a selenkupfer film comprises the step of following order:
A. the cleaning of glass substrate or silicon substrate;
B. with CuCl 22H 2O, SeO 2Put into 30～150 parts solvent, the material in the solution is fully dissolved, and adjustment pH value to 3～10;
C. make the outside evenly substrate of the said solution of smearing step b, and oven dry, the precursor thin-film sample obtained;
D. step c gained precursor thin-film sample is placed on the support, but put into the encloses container of hydrazine hydrate, the precursor thin-film sample is not contacted with hydrazine;
E. with the steps d gains, carry out drying, obtain the selenkupfer film.
2. the preparation method of selenkupfer film as claimed in claim 1 is characterized in that, the said washing of step a is to be 2mm * 2mm sheet glass, silicon chip with size, puts into the volume ratio trichloromethane: the solution of ethanol=5: 1, ultrasonic cleaning; Again sheet glass, silicon chip are put into acetone: the solution of zero(ppm) water=5: 1, ultrasonic cleaning; In zero(ppm) water, substrate is used sonic oscillation again; The above-mentioned substrate that obtains is emitted on sends in the baking oven oven dry in the glass dish and supply the system film to use.
3. the preparation method of selenkupfer film as claimed in claim 1 is characterized in that, the described CuCl of step b 22H 2O1.5～3.0 part, SeO 21.0～2.5 parts.
4. the preparation method of selenkupfer film as claimed in claim 1 is characterized in that, the described solvent of step b is at least a in deionized water, ethanol, ammoniacal liquor, the hydrochloric acid.
5. the preparation method of selenkupfer film as claimed in claim 1; It is characterized in that the said substrate of evenly smearing of step c is to smear through sol evenning machine; Sol evenning machine is with 200～3500 rev/mins of rotations; After then substrate being dried, so repeat once more 5～15 times, obtained certain thickness precursor thin-film sample.
6. the preparation method of selenkupfer film as claimed in claim 1 is characterized in that, puts into 15.0～30.0 parts of hydrazine hydrates in the said encloses container of steps d.
7. the preparation method of selenkupfer film as claimed in claim 1 is characterized in that, the said drying of step e is heated between 160～220 ℃ for putting into baking oven, soaking time 10～20 hours, and cool to room temperature takes out then.
CN201110290892XA 2011-09-29 2011-09-29 Method for preparing cuprous selenide thin film Pending CN102603201A (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864027A (en) * 2014-03-03 2014-06-18 山东建筑大学 Method for preparing cuprous telluride film
CN105181617A (en) * 2015-09-21 2015-12-23 安徽师范大学 Sensor for mercury ion detection and preparation method and application thereof
CN105439106A (en) * 2015-12-17 2016-03-30 山东建筑大学 Method for preparing bismuth selenide thermoelectric thin film with bismuth sulfate
CN105552205A (en) * 2015-12-17 2016-05-04 山东建筑大学 Method for preparing bismuth selenide thermoelectric film from bismuth chloride
CN105576114A (en) * 2015-12-17 2016-05-11 山东建筑大学 Method for preparing bismuth selenide thermoelectric film by use of bismuth acetate
CN106329306A (en) * 2016-09-28 2017-01-11 佛山科学技术学院 Nanometer aperture structure based disordered gain medium preparing method
CN109082650A (en) * 2018-06-26 2018-12-25 合肥萃励新材料科技有限公司 A kind of Cu2Se film forming method
CN109087967A (en) * 2018-08-10 2018-12-25 暨南大学 A kind of cuprous oxide film and the preparation method and application thereof
CN109243836A (en) * 2018-08-31 2019-01-18 浙江大学 Cu as electrode material for super capacitor2Se nano material and preparation method thereof
CN109336070A (en) * 2018-11-06 2019-02-15 桂林理工大学 A kind of preparation method of upper fast-growth Berzeline nanometer sheet copper-based at room temperature
CN109659356A (en) * 2018-12-18 2019-04-19 河南师范大学 The nano-device with negative differential resistance and on-off action based on copper selenide single layer
CN110739387A (en) * 2019-10-25 2020-01-31 陕西师范大学 Cu2Preparation method of Se thin film material
CN111471196A (en) * 2019-01-23 2020-07-31 同济大学 Preparation method of PEDOT (polymer stabilized alumina)/PSS (copper sulfide)/Cu-doped silver selenide flexible composite film with high thermoelectric property
CN113555459A (en) * 2021-07-20 2021-10-26 陕西师范大学 Selenium sulfide doped copper oxide with strong luminescence characteristic

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CN101262027A (en) * 2008-04-18 2008-09-10 天津大学 Method for making CIS film based on neutral pH condition double potential step electrodeposit
CN101312218A (en) * 2008-04-18 2008-11-26 天津大学 Method for preparing copper indium selenium compound thin film by continuous ion sheath adsorption reaction method
CN101630701A (en) * 2008-12-03 2010-01-20 山东建筑大学 Method for preparing copper-indium-selenium optoelectronic thin film material of solar cell

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Publication number Priority date Publication date Assignee Title
CN101150151A (en) * 2007-11-08 2008-03-26 北京科技大学 A making method of copper, indium and selenium film for solar battery
CN101262027A (en) * 2008-04-18 2008-09-10 天津大学 Method for making CIS film based on neutral pH condition double potential step electrodeposit
CN101312218A (en) * 2008-04-18 2008-11-26 天津大学 Method for preparing copper indium selenium compound thin film by continuous ion sheath adsorption reaction method
CN101630701A (en) * 2008-12-03 2010-01-20 山东建筑大学 Method for preparing copper-indium-selenium optoelectronic thin film material of solar cell

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864027B (en) * 2014-03-03 2016-01-20 山东建筑大学 A kind of method preparing cuprous telluride film
CN103864027A (en) * 2014-03-03 2014-06-18 山东建筑大学 Method for preparing cuprous telluride film
CN105181617B (en) * 2015-09-21 2019-04-16 安徽师范大学 The preparation method and application of sensor for mercury ion detecting
CN105181617A (en) * 2015-09-21 2015-12-23 安徽师范大学 Sensor for mercury ion detection and preparation method and application thereof
CN105439106A (en) * 2015-12-17 2016-03-30 山东建筑大学 Method for preparing bismuth selenide thermoelectric thin film with bismuth sulfate
CN105552205A (en) * 2015-12-17 2016-05-04 山东建筑大学 Method for preparing bismuth selenide thermoelectric film from bismuth chloride
CN105576114A (en) * 2015-12-17 2016-05-11 山东建筑大学 Method for preparing bismuth selenide thermoelectric film by use of bismuth acetate
CN105552205B (en) * 2015-12-17 2018-05-11 山东建筑大学 A kind of method that bismuth selenide thermal electric film is prepared with bismuth chloride
CN105576114B (en) * 2015-12-17 2018-05-15 山东建筑大学 A kind of method that bismuth selenide thermal electric film is prepared with bismuth acetate
CN106329306A (en) * 2016-09-28 2017-01-11 佛山科学技术学院 Nanometer aperture structure based disordered gain medium preparing method
CN109082650A (en) * 2018-06-26 2018-12-25 合肥萃励新材料科技有限公司 A kind of Cu2Se film forming method
CN109087967A (en) * 2018-08-10 2018-12-25 暨南大学 A kind of cuprous oxide film and the preparation method and application thereof
CN109243836A (en) * 2018-08-31 2019-01-18 浙江大学 Cu as electrode material for super capacitor2Se nano material and preparation method thereof
CN109336070A (en) * 2018-11-06 2019-02-15 桂林理工大学 A kind of preparation method of upper fast-growth Berzeline nanometer sheet copper-based at room temperature
CN109659356A (en) * 2018-12-18 2019-04-19 河南师范大学 The nano-device with negative differential resistance and on-off action based on copper selenide single layer
CN111471196A (en) * 2019-01-23 2020-07-31 同济大学 Preparation method of PEDOT (polymer stabilized alumina)/PSS (copper sulfide)/Cu-doped silver selenide flexible composite film with high thermoelectric property
CN111471196B (en) * 2019-01-23 2021-10-08 同济大学 Preparation method of PEDOT (polymer stabilized alumina)/PSS (copper sulfide)/Cu-doped silver selenide flexible composite film with high thermoelectric property
CN110739387A (en) * 2019-10-25 2020-01-31 陕西师范大学 Cu2Preparation method of Se thin film material
CN113555459A (en) * 2021-07-20 2021-10-26 陕西师范大学 Selenium sulfide doped copper oxide with strong luminescence characteristic
CN113555459B (en) * 2021-07-20 2022-08-30 陕西师范大学 Selenium sulfide doped copper oxide with strong luminescence characteristic

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Application publication date: 20120725