JP5782672B2 - Compound semiconductor thin film ink - Google Patents

Compound semiconductor thin film ink Download PDF

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JP5782672B2
JP5782672B2 JP2009255351A JP2009255351A JP5782672B2 JP 5782672 B2 JP5782672 B2 JP 5782672B2 JP 2009255351 A JP2009255351 A JP 2009255351A JP 2009255351 A JP2009255351 A JP 2009255351A JP 5782672 B2 JP5782672 B2 JP 5782672B2
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compound semiconductor
particles
thin film
semiconductor thin
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JP2011099059A (en
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毅聞 張
毅聞 張
山田 明
山田  明
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凸版印刷株式会社
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/54Material technologies
    • Y02E10/541CuInSe2 material PV cells
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/54Material technologies
    • Y02E10/549Material technologies organic PV cells
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/52Manufacturing of products or systems for producing renewable energy
    • Y02P70/521Photovoltaic generators

Description

  The present invention relates to an ink for preparing a compound semiconductor thin film, a compound semiconductor thin film obtained by using the ink, a solar cell including the compound semiconductor thin film, and a method for manufacturing the solar cell.

  A solar cell is a device that converts light energy into electrical energy using the photovoltaic effect, and has recently attracted attention from the viewpoints of prevention of global warming and replacement of exhausted resources.

  Depending on the material of the light-absorbing layer, which is the most important component, the solar cell is composed of silicon (single crystal, polycrystal, amorphous, composite thereof), compound semiconductor (CIGS compound, III-V group compound, II-VI group compounds), organic semiconductor systems, and dye-sensitized systems. Among these, CIGS (CuInGaSe) compound solar cells have a large light absorption coefficient of the light absorption layer, a relatively small number of manufacturing steps, high radiation resistance, and photoelectric conversion exceeding 19% in the laboratory. Since it has excellent properties such as efficiency, it is expected as a next-generation solar cell that plays a role in resource conservation and an energy source for preventing global warming.

  Currently, the light absorption layer, which is the most important component of a CIGS compound solar cell, is mainly formed by a vacuum process such as vapor deposition or sputtering. However, since the vacuum process requires expensive vacuum equipment and the manufacturing process is complicated, the CIGS compound solar cell has a drawback that the power generation cost is high. In addition, there is also a drawback that it is difficult to maintain the uniformity of the distribution of each element in the plane when forming a film with a large area.

  In order to further promote the use of CIGS compound solar cells, it is essential to further reduce power generation costs. Recently, a method of forming a CIGS layer by a low-cost film forming method called a printing process has been proposed (see Patent Document 1). According to this method, an expensive vacuum device is not required and the process is simplified, so that the power generation cost may be significantly reduced. In addition, it is expected that the distribution of each element in the plane becomes uniform and the conversion efficiency is improved.

  However, since the printing method requires a subsequent high-temperature and long-time heat treatment step, Se contained in the CIGS compound is vaporized and removed in the heat treatment step, and it is difficult to obtain the required p-type crystal. Therefore, in the said patent document 1, the heat processing process is performed in selenium atmosphere or sulfur atmosphere. However, the selenium atmosphere is toxic and the sulfur atmosphere is difficult to control. Therefore, there is a problem that the heat treatment process becomes complicated and the manufacturing cost becomes high for countermeasures against such problems.

JP 2009-076842 A

  The present invention has been made in view of the above problems. That is, an object of the present invention is to provide a compound semiconductor thin film preparation ink that enables the manufacture of a low-cost solar cell, a manufacturing method thereof, a compound semiconductor thin film obtained using the ink, a solar cell including the compound semiconductor thin film, And a manufacturing method thereof.

In order to solve the above problems, the first aspect of the present invention includes CuIn x Ga 1-x Se 2 (0 ≦ x <1) particles, AgIn x Ga 1-x Se 2 (0 ≦ x <1) particles, And compound particles containing Se atoms selected from the group consisting of CuIn x Ga 1-x (Se y S 1-y ) 2 (0 ≦ x <1, 0 ≦ y ≦ 1) particles, and Se particles , number less than 10 alcohols, diethyl ether, pentane, hexane, Ri Na are dispersed in an organic solvent selected from the group consisting of cyclohexane, compound particles comprising said Se atoms, CuIn x Ga 1-x Se 2 (0 ≦ x <1) particles, and the molar ratio of the Se particles and the CuIn x Ga 1-x Se 2 (0 ≦ x <1) particles is Se / CuIn x Ga 1-x Se 2 = 0.1-3. Oh it provides a compound semiconductor thin film forming ink according to claim Rukoto.

  In such a compound semiconductor thin film forming ink, Se particles having an average particle diameter of 1 nm or more and 200 nm or less can be used. In addition, compound particles containing Se atoms having an average particle diameter of 1 nm to 200 nm can be used.

  According to a second aspect of the present invention, there is provided a compound semiconductor thin film obtained by applying or printing the above-described compound semiconductor thin film forming ink and performing heat treatment.

  According to a third aspect of the present invention, there is provided a solar cell comprising a light absorption layer comprising the compound semiconductor thin film described above.

  According to a fourth aspect of the present invention, there is provided a step of applying or printing the above-described compound semiconductor thin film forming ink on an electrode formed on a substrate to form a compound semiconductor coating film, and heat treating the compound semiconductor coating film. Then, the manufacturing method of the solar cell characterized by including the process of forming the light absorption layer which consists of a compound semiconductor thin film is provided.

  According to the present invention, a compound semiconductor thin film forming ink capable of producing a solar cell having a high cost photoelectric conversion efficiency and a low cost compound semiconductor thin film, a compound semiconductor thin film obtained using the ink, A solar cell including the compound semiconductor thin film and a method for manufacturing the solar cell are provided.

It is sectional drawing which shows the whole structure of the solar cell which concerns on the Example of this invention.

  Hereinafter, embodiments of the present invention will be described in detail.

  The ink for forming a compound semiconductor thin film according to the first embodiment of the present invention is characterized in that compound particles containing Se atoms and Se particles are dispersed in an organic solvent.

  The average particle size of Se particles is preferably 1 nm or more and 200 nm or less. When the average particle size of Se particles is larger than 200 nm, a gap is easily formed in the compound semiconductor thin film in the heat treatment step of the compound semiconductor thin film, and the photoelectric conversion efficiency tends to be lowered. On the other hand, if the average particle size of the Se particles is less than 1 nm, the fine particles tend to aggregate and it becomes difficult to prepare ink. The average particle size of Se particles is more preferably 5 nm or more and 100 nm or less.

  The particle diameter of the compound particles containing Se atoms is preferably 1 nm or more and 200 nm or less. When the average particle diameter of the compound particles containing Se atoms is larger than 200 nm, a gap is easily formed in the compound semiconductor thin film in the heat treatment step of the compound semiconductor thin film, and the photoelectric conversion efficiency tends to be reduced. On the other hand, if the average particle size of the compound particles containing Se atoms is less than 1 nm, the fine particles are likely to aggregate and it is difficult to prepare ink. The average particle size of the compound particles containing Se atoms is more preferably 5 nm or more and 100 nm or less.

As the compound particles containing Se atoms, the target compound semiconductor material or a material that becomes a compound semiconductor by reaction can be used, and CuIn x Ga 1-x Se 2 (0 ≦ x ≦ 1) particles, AgIn x Ga 1-x Se 2 , (0 ≦ x ≦ 1) particles, CuIn x Ga 1-x (Se y S 1-y ) 2 (0 ≦ x ≦ 1, 0 ≦ y ≦ 1) particles, etc. I can do it. Among these, CuIn x Ga 1-x Se 2 (0 ≦ x ≦ 1) particles are preferable.

When CuIn x Ga 1-x Se 2 (0 ≦ x ≦ 1) particles are used as the compound particles containing Se atoms, the forbidden band width can be appropriately changed by adjusting the ratio of In and Ga. .

Moreover, it is desirable that the molar ratio between the Se particles and the CuIn x Ga 1-x Se 2 (0 ≦ x ≦ 1) particles is Se / CuIn x Ga 1-x Se 2 = 0.1-3. When this molar ratio (Se / CuIn x Ga 1-x Se 2 ) is less than 0.1, Se is lost due to vaporization during heat treatment and Se is insufficient, so that crystal growth of the CIGS layer becomes insufficient, The photoelectric conversion efficiency is lowered. When the molar ratio is larger than 3, Se particles remain even after the heat treatment, and the photoelectric conversion efficiency is lowered.

  The ink for forming a compound semiconductor thin film according to the first embodiment of the present invention can be produced by dispersing compound particles containing Se atoms and Se particles in an organic solvent.

There is no restriction | limiting in particular as an organic solvent. For example, alcohol, ether, ester, aliphatic hydrocarbon, alicyclic hydrocarbon, aromatic hydrocarbon and the like can be used. Preferred organic solvents are methanol, ethanol, alcohol having less than 10 carbon atoms in the Putanoru, diethyl chill ethers are pentane, hexane, cyclohexane, toluene, especially preferred organic solvents are ethanol and methanol.

  In the ink according to the present embodiment, a dispersant can be blended in order to efficiently disperse the compound particles containing Se atoms and the Se particles in an organic solvent. Examples of the dispersant include thiols, selenols, alcohols having 10 or more carbon atoms, and the like.

  In addition, the ink according to the present embodiment can be blended with a binder such as a silica binder in order to obtain a high-strength compound semiconductor thin film.

  The concentration of the particles in the organic solvent is not particularly limited, but is usually 1 to 20% by weight.

  The compound semiconductor thin film according to the second embodiment of the present invention is formed by applying or printing the above-described ink on a substrate, drying to remove the organic solvent, and then performing a heat treatment.

  Examples of the application method include a doctor method and a spin coating method, and examples of the printing method include a gravure printing method and a screen printing method.

  The thickness of the coating film formed by coating or printing is preferably such that the thickness of the compound semiconductor thin film after drying and heat treatment is 0.5 to 10 μm, for example, about 2 μm.

  The heat treatment can be performed by rapid thermal annealing (RTA) in addition to annealing in a heating furnace.

  Since the heat treatment temperature needs to be a temperature necessary for crystallization of the compound semiconductor, it is preferably 400 ° C. or more. When a glass substrate is used as the substrate, the heat treatment temperature must be able to withstand the glass substrate. Therefore, it is desirable that the temperature be 600 ° C. or lower, particularly 550 ° C. or lower.

  In the manufacturing process of the compound semiconductor thin film according to the present embodiment, it is desirable to apply a CuSe nanoparticle layer on the ink coating film from the viewpoint of promoting crystal growth. By applying the CuSe nanoparticle layer in this way, the CuSe layer becomes a liquid phase during the heat treatment, thereby promoting the crystal growth of the compound semiconductor and increasing the particle diameter of the compound semiconductor crystal.

  The average particle size of the CuSe particles is preferably in the range of 1 nm to 200 nm. When the average particle size is larger than 200 nm, a gap is easily formed in the compound semiconductor film in the heat treatment step, and the photoelectric conversion efficiency is lowered. If the average particle size is less than 1 nm, the fine particles are likely to aggregate and it becomes difficult to prepare the ink. Therefore, the average particle size is preferably 1 nm or more, more preferably 5 nm or more.

  As described above, according to the second embodiment of the present invention, by applying or printing the compound particles containing Se atoms capable of forming a compound semiconductor and the ink in which the Se particles are dispersed, drying and heat-treating the conventional method Thus, it is possible to form a compound semiconductor thin film at a low cost by a simple process without requiring a toxic Se atmosphere or a sulfur atmosphere that is difficult to control.

  Next, a solar cell according to a third embodiment of the present invention will be described with reference to FIG.

  FIG. 1 is a cross-sectional view showing a solar cell according to a third embodiment of the present invention. In the solar cell shown in FIG. 1, a back electrode 102 is formed on a substrate 101. As the substrate 101, soda lime glass, a metal plate, a plastic film, or the like can be used. As the back electrode 102, a metal such as molybdenum (Mo), nickel (Ni), or copper (Cu) can be used.

  The compound semiconductor thin film according to the second embodiment of the present invention described above is formed on the back electrode 102 as the light absorption layer 103. That is, the light absorption layer 3 is formed by applying the ink according to the first embodiment of the present invention described above on the back electrode 102, drying, and heat-treating.

A buffer layer 104, an i layer 105, and an n layer 106 are sequentially formed on the light absorption layer 103. As the buffer layer 104, known CdS, Zn (S, O, OH), and In 2 S 3 can be used. As the i layer 105, a known metal oxide such as ZnO can be used. As the n layer 106, known ZnO to which Al, Ga, B, or the like is added can be used.

  Then, the surface electrode 107 is formed on the n layer 106 to complete the solar cell. As the surface electrode 107, a known metal such as Al or Ag can be used.

Although not shown, an antireflection film having a role of suppressing light reflection and absorbing more light by the light absorption layer may be provided on the n layer 106. The material of the antireflection film is not particularly limited, and for example, magnesium fluoride (MgF 2 ) can be used. An appropriate thickness of the antireflection film is about 100 nm.

  The solar cell according to the third embodiment of the present invention configured as described above is applied or printed with compound particles containing Se atoms capable of forming a compound semiconductor and ink dispersed with Se particles, and then dried and heat-treated. Thus, since the light absorption layer is formed, a toxic Se atmosphere and a sulfur atmosphere that is difficult to control as in the conventional method are not required, and therefore, the light absorption layer is manufactured by a simple process at a low cost.

EXAMPLES Hereinafter, the present invention will be described in detail based on examples, but the present invention is not limited to these examples.

(Synthesis of CIGS nanoparticles)
A solution in which CuI, InI 3 and GaI 3 were dissolved in pyridine was mixed with a solution in which Na 2 Se was dissolved in methanol, and reacted at 0 ° C. in an inert gas atmosphere. The mixed solution was prepared such that the molar ratio of CuI, InI 3 , GaI 3 , and Na 2 Se was 0.9: 0.7: 0.3: 2.0.

  The reaction solution was filtered and washed with methanol, and the obtained CIGS nanoparticles were dispersed in ethanol.

(Synthesis of Se nanoparticles)
0.01M H 2 SeO 3 and 0.01M NaBH 4 were mixed in a weight ratio of 1:10 and reacted at 0 ° C. for 5 minutes. The reaction solution was filtered, and the obtained Se nanoparticles were dispersed in ethanol.

(Preparation of ink)
The Se nanoparticle dispersion liquid and the CIGS nanoparticle dispersion liquid obtained as described above were mixed so that the molar ratio of Se nanoparticles to CIGS nanoparticles was 0.5 / 1. Further ink was added to prepare an ink so that the solid content of the mixture was 5% by weight.

  Next, the solar battery cell having the structure shown in FIG. 1 was manufactured as follows.

(Formation of back electrode 102)
On the soda lime glass 101, a back electrode 102 made of a Mo layer having a thickness of 0.6 μm was formed by sputtering.

(Formation of the light absorption layer 103)
On the back electrode 102, the ink obtained above is applied by a doctor method, the solvent is evaporated in an oven at 250 ° C., and then heated at 550 ° C. for 10 minutes, whereby a light absorption layer made of CIGS having a thickness of 2 μm. 103 was formed.

(Formation of buffer layer 104)
The structure in which the light absorption layer 103 is formed has a molar concentration of 0.0015 M, 0.0075 M, and 1.5 M, cadmium sulfate (CdSO 4 ), thiourea (NH 2 CSNH 2 ), aqueous ammonia (NH 4 OH) was added to the mixed aqueous solution at 70 ° C. to form a buffer layer 104 made of CdS having a thickness of 50 nm on the light absorption layer 103.

(Formation of i layer 105)
An i layer 105 made of ZnO having a thickness of 50 nm was formed on the buffer layer 104 using diethyl zinc and water as raw materials by MOCVD.

(Formation of n layer 106)
An n layer 106 made of ZnO: B having a thickness of 1 μm was formed on the i layer 105 by using MOCVD method using diethyl zinc, water, and diborane as raw materials.

(Formation of surface electrode 107)
A surface electrode 107 made of Al having a thickness of 3 μm was formed on the n layer 106 by vapor deposition.

  The CIGS solar cell was completed by the above.

Comparative Example A CIGS solar battery cell was formed in the same manner as in the example except that the light absorption layer 103 was formed using an ink made of an ethanol dispersion containing 5 wt% of CIGS nanoparticles only without Se nanoparticles. Got.

About the photovoltaic cell of said Example and comparative example, evaluation by a standard sunlight simulator (light intensity: 100 mW / cm < 2 >, air mass: 1.5) was performed.

As a result, the photoelectric conversion efficiency of the solar cell according to the example was 1.1%, whereas the photoelectric conversion effect of the solar cell according to the comparative example was not found. This is because, in the solar battery cell according to the example, since the ink containing Se particles in addition to CIGS particles was used for forming the light absorbing layer by coating, a sufficient amount of Se was secured in the light absorbing layer even by heat treatment. In contrast to the growth of p-type semiconductor crystals, the solar cell according to the comparative example used ink containing only CIGS particles without including Se particles, so that Se was vaporized by heat treatment and escaped from CIGS. This is probably because a p-type semiconductor crystal could not be obtained due to a lack of Se amount.
The invention described in the original claims is appended below.
[1]
An ink for forming a compound semiconductor thin film, comprising compound particles containing Se atoms and Se particles dispersed in an organic solvent.
[2]
The compound semiconductor thin film forming ink according to [1], wherein the Se particles have an average particle diameter of 1 nm to 200 nm.
[3]
The compound semiconductor thin film forming ink according to [1] or [2], wherein the compound particles containing Se atoms have an average particle diameter of 1 nm to 200 nm.
[4]
The compound particles containing Se atoms include CuIn x Ga 1-x Se 2 (0 ≦ x ≦ 1) particles, AgIn x Ga 1-x Se 2 , (0 ≦ x ≦ 1) particles, and CuIn x Ga 1−. Any one of [1] to [3], wherein x (Se y S 1-y ) 2 (0 ≦ x ≦ 1, 0 ≦ y ≦ 1) is selected from the group consisting of particles. 2. An ink for forming a compound semiconductor thin film according to 1.
[5]
The compound semiconductor thin film forming ink according to [4], wherein the compound particles containing Se atoms are CuIn x Ga 1-x Se 2 (0 ≦ x ≦ 1) particles.
[6]
The molar ratio of the Se particles and CuIn x Ga 1-x Se 2 (0 ≦ x ≦ 1) particles is Se / CuIn x Ga 1-x Se 2 = 0.1 to 3 [5] 2. An ink for forming a compound semiconductor thin film according to 1.
[7]
A compound semiconductor thin film obtained by applying or printing the compound semiconductor thin film forming ink according to any one of [1] to [6] and heat-treating it.
[8]
[7] A solar cell comprising a light absorption layer comprising the compound semiconductor thin film according to [7].
[9]
A step of applying or printing the compound semiconductor thin film forming ink according to any one of [1] to [6] on an electrode formed on the substrate to form a compound semiconductor coating film; and
A step of heat-treating the compound semiconductor coating to form a light absorption layer comprising a compound semiconductor thin film
The manufacturing method of the solar cell characterized by comprising.

DESCRIPTION OF SYMBOLS 101 ... Glass substrate 102 ... Back electrode 103 ... Light absorption layer 104 ... Buffer layer 105 ... i layer 106 ... n layer 107 ... Surface electrode.

Claims (6)

  1. CuIn x Ga 1-x Se 2 (0 ≦ x <1) particles, AgIn x Ga 1-x Se 2 , (0 ≦ x <1) particles, and CuIn x Ga 1-x (Se y S 1-y ) 2 Compound particles containing Se atoms selected from the group consisting of (0 ≦ x <1, 0 ≦ y ≦ 1) particles, and Se particles are selected from alcohols having less than 10 carbon atoms, diethyl ether, pentane, hexane, and cyclohexane. Dispersed in an organic solvent selected from the group consisting of:
    The compound particles containing Se atoms are CuIn x Ga 1 -x Se 2 (0 ≦ x <1) particles,
    Wherein said Se particles CuIn x Ga 1-x Se 2 (0 ≦ x <1) of you, wherein the molar ratio of the particles is Se / CuIn x Ga 1-x Se 2 = 0.1~3 Compound semiconductor thin film forming ink.
  2.   2. The compound semiconductor thin film forming ink according to claim 1, wherein an average particle diameter of the Se particles is 1 nm or more and 200 nm or less.
  3.   3. The compound semiconductor thin film forming ink according to claim 1, wherein the compound particles containing Se atoms have an average particle diameter of 1 nm to 200 nm.
  4. Claim 1 compound semiconductor thin film forming ink to the coating or printing according to any one of 3, the compound semiconductor thin film characterized by comprising a heat treatment.
  5. A solar cell comprising a light absorption layer comprising the compound semiconductor thin film according to claim 4 .
  6. A step of applying or printing the compound semiconductor thin film forming ink according to any one of claims 1 to 3 on an electrode formed on a substrate to form a compound semiconductor coating, and heat treating the compound semiconductor coating And a step of forming a light absorption layer made of a compound semiconductor thin film.
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JPH01248627A (en) * 1988-03-30 1989-10-04 Matsushita Electric Ind Co Ltd Manufacture of cuinse2 film
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JP2009528680A (en) * 2006-02-23 2009-08-06 ファン デューレン、イェルーン カー.イェー.VAN DUREN Jeroen K.J. High-throughput printing of chalcogen layers and the use of intermetallic materials
KR101144807B1 (en) * 2007-09-18 2012-05-11 엘지전자 주식회사 Ink For Solar Cell And Manufacturing Method Of The Ink, And CIGS Film Solar Cell Using The Ink And Manufacturing Method Therof
KR101030780B1 (en) * 2007-11-14 2011-04-27 성균관대학교산학협력단 Synthesis of i-iii-vi2 nanoparticles and fabrication of polycrystalline absorber layers
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EP2379458A4 (en) * 2009-01-21 2015-02-11 Purdue Research Foundation Selenization of precursor layer containing culns2 nanoparticles
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