KR101854500B1 - Manufacturing Method of Metal Nano Particle for Preparation of Light Absorbing Layer of Solar Cell - Google Patents
Manufacturing Method of Metal Nano Particle for Preparation of Light Absorbing Layer of Solar Cell Download PDFInfo
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- KR101854500B1 KR101854500B1 KR1020150059461A KR20150059461A KR101854500B1 KR 101854500 B1 KR101854500 B1 KR 101854500B1 KR 1020150059461 A KR1020150059461 A KR 1020150059461A KR 20150059461 A KR20150059461 A KR 20150059461A KR 101854500 B1 KR101854500 B1 KR 101854500B1
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- Prior art keywords
- flow path
- metal nanoparticles
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- fluids
- branched
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- 238000004519 manufacturing process Methods 0.000 title claims description 14
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- 238000000034 method Methods 0.000 claims abstract description 44
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- 239000002904 solvent Substances 0.000 claims abstract description 18
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 16
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- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 9
- 239000000872 buffer Substances 0.000 claims abstract description 8
- 238000002347 injection Methods 0.000 claims description 54
- 239000007924 injection Substances 0.000 claims description 54
- 238000002156 mixing Methods 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 28
- 150000003839 salts Chemical class 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
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- 235000011083 sodium citrates Nutrition 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
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- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
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- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
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- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
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- 229940074439 potassium sodium tartrate Drugs 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 1
- 229940047670 sodium acrylate Drugs 0.000 description 1
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 1
- 235000010378 sodium ascorbate Nutrition 0.000 description 1
- 229960005055 sodium ascorbate Drugs 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 1
- 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 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 229960002920 sorbitol Drugs 0.000 description 1
- 235000010356 sorbitol Nutrition 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical class [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
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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
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
- H01L31/02168—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells the coatings being antireflective or having enhancing optical properties for the solar cells
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
-
- 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
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The present invention relates to a method for synthesizing bimetallic or intermetallic metal nanoparticles for producing a solar cell light absorbing layer,
(i) preparing a first solution containing a reactant, a second solution containing a reducing agent, and a buffer solvent, and storing them in a first tank, a second tank, and a third tank, respectively;
(ii) injecting nitrogen gas into the tanks, respectively, and injecting the fluids stored in the tanks into the flow path reactor through individual paths; And
(iii) purifying the synthesized metal nanoparticles while passing through the flow path reactor;
The present invention also relates to a method for synthesizing metal nanoparticles.
Description
The present invention relates to a method of synthesizing metal nanoparticles for manufacturing a solar cell light absorbing layer and metal nanoparticles produced thereby.
Recently, as concerns about environmental problems and depletion of natural resources have increased, there is no problem about environmental pollution, and there is a growing interest in solar cells as energy-efficient alternative energy sources. Solar cells are classified into silicon solar cells, thin film compound solar cells, and stacked solar cells depending on their constituents, among which silicon semiconductor solar cells have been extensively studied.
However, in recent years, thin film type compound solar cells have been researched and developed in order to overcome the shortcomings of silicon solar cells.
Cu (In 1-x Ga x ) (Se y S 1-y ) (CI (G) S) which is an I-III-VI group belonging to a ternary compound semiconductor in the thin film type compound semiconductor has a direct transitional energy band Gap, a high optical absorption coefficient, and a very electro-optically stable material, making it a very ideal material for a light absorbing layer of a solar cell.
Recently, attention has been paid to CZTS (Cu 2 ZnSn (S, Se) 4 ) -based solar cells containing copper, zinc, tin, sulfur, or selenium as an ultra low cost metal element as an alternative to the CIGS- have. The CZTS has a direct band gap of about 1.0 to 1.5 eV and an absorption coefficient of 10 4 cm -1 or more, and has an advantage of using Sn and Zn, which are relatively rich in reserves and low in cost.
The thin film of CI (G) S or CZTS may be formed by sputtering, hybrid sputtering, pulse laser deposition, spray pyrolysis, electrodeposition / thermal sulfurization, E- (E-beam) Cu / Zn / Sn / thermal sulphide, and sol-gel methods.
On the other hand, recently, a method of forming a thin film by applying nanoparticle-type precursor material under non-vacuum and then heat-treating the precursor material has been introduced. Such a process can lower the process cost and has an advantage that a large area can be uniformly manufactured.
As a method for producing such nanoparticles, a batch type synthesis method has been used in which solutions containing a reducing agent and a metal salt chalcogenide element are prepared and reacted with a mixture prepared by mixing them.
However, the synthesis method of the batch type is limited to a few tens of grams at a time because of the limitation of the vessel, so that the amount of the synthetic particles is very limited, and it takes at least 3 hours to complete the synthesis, There are long disadvantages.
The disadvantage of this problem is that the nanoparticles used in various parts of the solar cell thin film production need to be mass-produced in a short time, and therefore, the invention for improving the nanoparticles is more urgently needed.
Therefore, there is a high need for techniques for synthesizing nanoparticles that improve the efficiency and convenience of manufacturing while maintaining the uniformity of shape and composition of the particles compared with the particles prepared by the conventional synthesis method.
SUMMARY OF THE INVENTION Accordingly, the present invention has been made to solve the above-mentioned problems of the prior art and the technical problems required from the past.
The inventors of the present application have conducted intensive research and various experiments and have found that when metal nanoparticles are synthesized using a flow reactor of a novel structure according to the present invention, The particles can be synthesized more effectively and the process can be simplified while maintaining the uniformity. Thus, it has been confirmed that the particles can be mass-produced in a short time, and the present invention has been accomplished.
Therefore, a method for synthesizing bimetallic or intermetallic metal nanoparticles for the production of a solar cell light absorbing layer according to the present invention,
(i) preparing a first solution containing a reactant, a second solution containing a reducing agent, and a buffer solvent, and storing them in a first tank, a second tank, and a third tank, respectively;
(ii) injecting nitrogen gas into the tanks, respectively, and injecting the fluids stored in the tanks into the flow path reactor through individual paths; And
(iii) purifying the synthesized metal nanoparticles while passing through the flow path reactor;
And a control unit.
At this time, the fluids represented by the first solution, the second solution, and the buffer solvent may be simultaneously introduced into the flow path reactor.
Specifically, the first tank, the second tank, and the third tank for storing the fluids are connected to the flow path reactor by separate paths, and further connected to a nitrogen pump including nitrogen gas. Therefore, when the nitrogen gas is injected into the tanks by the nitrogen pump, the fluids are moved to the respective paths connected to the flow path reactor by the injection pressure of the gas, . ≪ / RTI >
This is because the contents of reactants, reducing agents and the like are calculated and included in the solution so that the metals are present in the desired ratio in the final particles, and it is easier to ensure the homogeneity of the final particle composition to be.
Meanwhile, the flow path reactor according to the present invention for synthesizing metal nanoparticles by transferring and passing the fluids from tanks,
The upper plate and the lower plate having a flat plate shape having respective flow paths,
Wherein the flow path includes at least one injection flow path through which the fluids are respectively injected, a mixing flow path through which the respective fluids injected into the injection flow paths are merged, and a discharge flow path through which the fluid merged by the mixing flow path is discharged,
Wherein the mixing flow path includes a stem flow path extending from the injection flow paths to the discharge flow path and one or more branch flow paths branched off from the stem flow path,
In the mixing of the fluids that repeat the branching and the merging, the fluids may be configured to be subjected to a mixing process in which the fluids are vertically branched and then merge in the left-right direction.
Generally, the flow path reactor has a fine flow path with a flow path width of about 10 to 1000 mu m, and in the flow path reactor, at least two kinds of fluids are mixed after being divided into a minute flow by the fine flow path. Further, in the flow path reactor, the fluid is divided into minute flows, and the diffusion distance of the fluid is shortened. As a result, the mixing speed of the fluid is increased and the fluid can be efficiently mixed in a shorter time than the conventional arrangement type reactor.
Particularly, the flow path reactor according to the present invention is configured so as to be subjected to a mixing process which is a lamination type in the conventional lamination type, that is, a laminar flow state, that is, The precipitation occurs in the portion of the lower plate and the clogging phenomenon is intensified. Therefore, unlike the flow reactor in which the mixing efficiency is lowered and the stability of the reaction is also serious, unlike the present invention, As a flow path reactor having an optimized structure in the reaction, the fluid is subjected to a mixing process of branching in the up and down direction and merging in the left and right direction. As a result, there is no flow path that disappears discontinuously and consequently, fluid congestion can be minimized, And the reaction occurs when the particles are formed Total efficiency is a flow reactor of the novel structure can be increased, in the case of using this synthesis the solar cell light-absorbing layer for producing metal nanoparticles, it is possible to synthesize particles more efficiently and simplify the manufacturing process.
The structure of each flow path of the flow path reactor according to the present invention will be described in more detail below.
In one specific example, the injection flow paths into which the different fluids are injected are largely divided into a first injection flow channel located on the central axis and a second injection flow channel located on the central axis, And a second injection flow path and a third injection flow path branched from each other at a predetermined angle.
The fluids to be injected into the respective injection channels may be arbitrarily determined. For example, the first injection channel may be filled with the buffer solution from the first tank, The second solution containing the reducing agent from the second tank and the first solution containing the reactant from the first tank into the third injection path may be injected into the second injection path.
More specifically, the second infusion passage and the third infusion passage may be branched in different directions with respect to the central axis so that the fluids injected by the infusion passage can naturally meet in the stem passage.
The branching angle of the second injection path and the third injection path may range from 30 degrees to 60 degrees with respect to the central axis.
If it is out of the above range and less than 30 degrees, it is difficult to manufacture the flow path. If it exceeds 60 degrees, natural mixing with other fluids can not be formed, and the flow of the fluid may be stagnated due to the bent portion. It is not preferable.
Also, in one specific example, the diameter of the injection channels may be from 1.5 millimeters to 5.0 millimeters. This is because it is not necessary to form a pressure formed by the flow of the fluid in the mixing flow passage from the injection flow passage within a range larger than the diameter of the mixing flow passage described below and to lower the pressure caused by the flow of the fluid, It is for this reason.
On the other hand, as described above, the mixing channel is divided into a stem channel and a branch channel.
The branch flow path is added to the stem flow path of the facing plate so as to enlarge the diameter thereof. Since the branch flow path is formed only in a part thereof, it is not necessary to separately describe the sections, but the stem flow path is formed entirely in the mixing flow path. And the two sides are divided into two sections according to the aspect of joining and joining.
Specifically, one is the section where the fluids are joined and the other is the section where the fluids are branched to the left and right.
In this case, the diameter of the stem channel of the section where the fluids are joined may be 0.5 to 1.5 millimeters, and the diameter of the stem channel of the section where the fluids are branched to the right and left is 0.5 Fold to 1.0 fold.
This is because the diameters of the stub channels in the branching section compared to the stub flow paths in the merging section can be made small so that the branching fluid is merged again.
Therefore, in order to keep the diameters of the stem channels of the section where the fluids are joined, the diameters of the stem channels of the sections where the fluids are branched to the right and left gradually decrease as the fluid joins, The diameter of the end of the stem flow path is preferably 0.5 times the diameter of the stem flow path in the region where the fluids are joined.
In the meantime, the stem flow path may be symmetrical with respect to the path from the point where the fluids are branched to the point where they are merged, and the branch flow path is symmetric with respect to the stem flow path, Lt; / RTI > Therefore, when the upper plate and the lower plate face each other, the stem flow path and the branch flow path overlap each other. At this time, the plane structure formed by the stem flow path and branch flow path is not limited as long as it is a symmetrical structure, .
At this time, the branching direction of the branch channels is formed so as to be merged with the branch channel of the plate facing at any one point of the branching section so that the vertically branched fluid can join right and left. In one specific example, And the branching angle may be in the range of 10 degrees to 45 degrees with respect to the line connecting the portion where the fluid is branched and merged as the central axis.
If the branching angle is out of the above range and less than 10 degrees, it is difficult to manufacture the flow path. If the branching angle is more than 45 degrees, the natural flow of the fluid can not be formed due to the bent portion.
On the other hand, in order to further prevent clogging of the flow path due to the precipitation phenomenon, it is possible to design such that the flow path depth continuously changes so that the flow path does not appear rapidly due to the branch flow path when the upper plate and the lower plate face each other, May include at least one section in which the depth continuously changes with respect to the surface of the plate, and a section in which the depth continuously changes is a point at which the fluid flowing through the stem flow path first meets the branch flow path I.e., a structure in which the fluid flowing in the flow path is tapered downward to the point where the fluid flows in the right and left directions.
At this time, the downwardly tapered structure may have a slope of 30 to 45 degrees. If the slope is out of the above range but less than 30 degrees, the length of the branch flow path is relatively long until the depth of the flow path of the stem flow path becomes equal to the depth It is inefficient. If it exceeds 45 degrees, the fluid may be stagnant immediately below the sloped inclined portion, and precipitation of particles may occur, which is not preferable.
Finally, the fluids that are injected into the injection channels and mixed uniformly through the mixing channel are discharged through the discharge channel. The diameters of the discharge channel are adjusted such that the mixed fluids are smoothly discharged without clogging. Lt; RTI ID = 0.0 > 5 < / RTI >
That is, the method of synthesizing metal nanoparticles according to the present invention is characterized in that a flow path reactor having a novel structure as described above is used, and therefore, through the process in which fluids are branched vertically and left- The metal nanoparticles can be stably obtained without clogging, and also the loss due to precipitation in the reactor can be prevented, and a continuous reaction process can be performed, thereby enabling mass production in a short time.
Hereinafter, fluids used for forming metal nanoparticles by passing through the flow path reactor will be described in detail.
In one specific example, the reactant contained in the first solution means materials that substantially constitute metal nanoparticles, and more specifically, may include two or more metal salts.
Specifically, the bimetallic or intermetallic metal nanoparticles may include Cu-In bimetallic metal nanoparticles, Cu-Sn bimetallic metal nanoparticles, Cu-Zn bimetallic metal nanoparticles, Sn-Zn Bimetallic metal nanoparticles, Cu-In-Ga intermetallic metal nanoparticles, and Cu-Sn-Zn intermetallic metal nanoparticles. The reactant is contained in the final particles to be synthesized Metal salts. For example, when the final particles to be synthesized are Cu-In bimetallic metal nanoparticles, the reactants may include copper (Cu) salts and indium (In) salts, and the final particles to be synthesized may be Cu- In the case of Zn intermetallic metal nanoparticles, the reactants may include copper (Cu) salts, tin (Sn) salts and zinc (Zn) salts.
The metal salt may be at least one selected from the group consisting of chloride, bromide, iodide, nitrate, nitrite, sulfate, acetate, sulfite, A salt of one or more types selected from the group consisting of acetylacetonate and hydroxide.
In addition, the reactant may further include a capping agent. Since the capping agent is contained in the solution process to control the size of the metal nanoparticles and the phase of the particles as well as atoms such as N, O, S, etc., So that the metal nanoparticles can be prevented from being oxidized.
Examples of such a capping agent include, but are not limited to, polyvinylpyrrolidone (PVP), polyvinyl alcohol, ethyl cellulose, sodium L-tartrate dibasic dehydrate, Potassium sodium tartrate, sodium acrylate, poly (acrylic acid sodium salt), sodium citrate, trisodium citrate, citric acid di But are not limited to, disodium citrate, sodium gluconate, sodium ascorbate, sorbitol, triethyl phosphate, ethylene diamine, propylene diamine, Is selected from the group consisting of 1,2-ethanedithiol, ethanethiol, ascorbic acid, citric acid, and tartaric acid. It may be more than one.
The content of the capping agent may be, for example, 20 mol or less based on 1 mol of the metal salts contained in the reactant.
When the content of the capping agent is more than 20 times the mole of the metal salt, the purification process of the metal nanoparticles is difficult and the purity of the metal nanoparticles may be lowered.
In one specific example, the reducing agent contained in the second solution is hydrazine, LiBH4, NaBH4, KBH4, Ca (BH4)2, Mg (BH4)2, LiB (Et)3H2, NaBH3(CN), NaBH (OAc)3,Ascorbic acid, triethanolamine, and the like.
At this time, the content of the reducing agent may be such that the total amount of the metal salt of the reactant and the mixing ratio of the reducing agent may be, for example, 1: 1 to 1:20 in a molar ratio.
When the content of the reducing agent is too small relative to the amount of the metal salt, reduction of the metal salt is not sufficiently performed, so that it is possible to obtain only a small or small amount of metal nanoparticles or to obtain particles having a desired element ratio. In addition, when the content of the reducing agent is more than 20 times the content of the metal salt, it is difficult to remove the reducing agent and by-products in the purification process.
In one specific example, the buffering solvent, and the solvent of the first solution and the second solution are selected from the group consisting of water, isopropyl alcohol, diethylene glycol (DEG), methanol, ethanol ), Oleylamine, ethyleneglycol, triethylene glycol, dimethyl sulfoxide, dimethyl formamide and N-methyl-2-pyrrolidone (NMP) And may be one or more selected from the group consisting of
In this case, the respective solvents may be selected independently of each other, and the respective solvents may be different from each other. In particular, the solvent and the buffer solvent may be mixed to reduce the possibility of additional reaction due to mixing, , The solvents of the first solution and the second solution may be equal to each other.
On the other hand, the present invention also relates to bimetallic or intermetallic metal nanoparticles for manufacturing a solar cell light absorbing layer,
The bimetallic metal nanoparticles are synthesized through a flow path reactor,
The flow path reactor is connected to a first tank for storing a first solution containing a reactant, a second tank for storing a second solution containing a reducing agent, and a third tank for storing a buffer solvent, The second tank, and the third tank are connected to the nitrogen pump, respectively, so that the fluids stored in the tanks by the nitrogen pump are introduced into the flow path reactor through separate paths to synthesize the metal nanoparticles. do.
As described above, the method of synthesizing metal nanoparticles according to the present invention is a method of synthesizing metal nanoparticles according to the present invention, by using a flow path reactor having a novel structure, by maintaining the uniformity of the particles prepared by the conventional synthesis method, It is possible to reduce the time to moisture and to simplify the process. Therefore, it is possible to synthesize metal nanoparticles in a large amount in a short time.
1 is a schematic diagram of a method of synthesizing metal nanoparticles according to the present invention;
2 is a schematic view of an upper plate and a lower plate of a flow path reactor according to the present invention;
3 is an enlarged schematic view of the lower plate A portion of Fig. 2;
FIG. 4 is a side view schematically showing the channel depth shape of the portion B in FIG. 3; FIG.
FIG. 5 is a schematic view of the upper plate and the lower plate of FIG. 2 facing each other;
FIG. 6 is a schematic view showing mixing behavior in cross sections occurring in each part of the flow path reactor of FIG. 5; FIG.
7 is an electron microscope (SEM) photograph of the metal nanoparticles according to Example 1;
8 is an XRD graph of the metal nanoparticles according to Example 1;
9 is an electron micrograph (SEM) photograph of the metal nanoparticles according to Comparative Example 1;
10 is an XRD graph of the metal nanoparticles according to Comparative Example 1;
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings, but the present invention is not limited by the scope of the present invention.
1 is a schematic view showing a method of synthesizing metal nanoparticles according to one embodiment of the present invention.
Referring to FIG. 1, the
At this time, fluids can pass through the flow path reactor at the same time, which is possible by controlling the injection pressure of the nitrogen gas.
2 to 6 are schematic views for explaining the structure of the flow path reactor of FIG. 1 in more detail.
2 is a schematic view showing an upper plate and a lower plate of a flow path reactor according to one embodiment of the present invention, and FIG. 3 is a schematic diagram showing an enlarged view of an A portion of the lower plate of FIG. Hereinafter, for convenience, the fluid injected from the first injection path is referred to as a first solution, the fluid injected from the second injection path is referred to as a second solution, and the fluid injected from the third injection path is defined as a buffer solvent.
Referring to FIG. 2, the flow path reactor according to the present invention is divided into an
Hereinafter, the injection channels and the mixing channel will be described in detail with reference to FIG. 3, based on what is formed in the
The first
The diameter d1 of the
The mixing flow path is divided into a
Referring again to FIG. 3, the
Specifically, the diameter (w1) of the stem flow path of the confluence section in which the fluids are confluent and the diameter (w2, w2) of the branch section in which the fluids are diverged to the right and left are present in the
The diameter (w1) of the stem channel of the section where the fluids are joined is 0.5 to 1.5 millimeters and the diameter (w2, w3) of the stem channel of the section where the fluids are diverged to the right and left, Is 0.5 to 1.0 times the diameter (w1).
The diameters (w2, w3) of the stem channels of the section where the fluids are branched to the right and left are described in more detail. The diameter (w2) of the stem channels of the section where the first fluids are confluent, , The diameter (w3) of the stem flow path of the section where the fluid flows is 1.0 times the stem flow diameter (w1) of the section where the fluids are joined, and the section where the second fluids are joined, Of the first fluid is 0.5 times the diameter (w1) of the flow channel of the second fluid at the portion where the first fluid is confluent, and then the portion where the second fluid is confluent.
Needless to say, the branch flow paths 215 symmetrical to the branch flow path 214 also have diameters corresponding to the branch flow paths.
As described above, when the mixing flow path is formed, the stem flow path diameter w1 of the section where the fluids are joined is constantly maintained throughout the mixing flow path, so that a certain amount of fluids flow through the flow path reactor.
On the other hand, Fig. 4 schematically shows a side view for showing the channel depth shape of the portion B in Fig.
4, the depth of the branched flow path 215 is set such that the stop point E of the branched flow path 215, that is, the branch point S at the point where the fluid flowing in the flow path first meets the branch flow path, And the slope a4 of the downward tapered structure is 30 degrees to 45 degrees. Although only the branch flow path of the lower plate is shown in this specification, the branch flow path of the upper plate may have the same shape as the branch flow path of the lower plate.
When the upper plate and the lower plate are faced to each other, the flow path reactor of the above-described structure does not show the flow path rapidly due to the branch flow path, so that the clogging of the flow path due to the precipitation of particles in the abrupt flow path forming portion can be prevented more effectively .
FIG. 5 shows a
Hereinafter, the process of branching and merging fluids in the
Referring to FIG. 5, as described above, the
Referring to FIG. 6 together with FIG. 5, the
6 (b), the mixed fluid is branched in the Y section, which is the first branch portion, and partly flows into the stem flow channel of the upper plate and the rest is directed to the stem flow channel of the lower plate, . The mixed fluid branched in this manner moves along the bent flow path at a predetermined angle. The diameter of the stem flow path in the section where the fluid is branched is sequentially decreased from the branch point. In the Z section, ).
The fluid that has branched into the upper plate and the lower plate is then brought into contact with the branch flow paths of the plates facing each other. Thus, the mixed fluid that has branched vertically flows in the left and right directions as shown in FIG. 6 (e) (F) of FIG. 6 at the U-th merging section.
When the mixing behavior is performed for each of the rhombic mixing channels, the mixed fluids discharged to the last discharge channel are mixed by the rhombic number n, so that 2 n mixed fluids as shown in FIG. 6 (b) Shape.
That is, in the flow path reactor according to the present invention, fluids flow naturally in the up-and-down direction and then merge in the left-right direction. As a result, there is no discontinuous flow path, so that the mixing performance can be maintained while minimizing fluid congestion Therefore, it is possible to produce metal nanoparticles having uniform composition. In addition, when the flow path reactor according to the present invention is used, since fluids are automatically mixed to obtain metal nanoparticles, a large amount of metal nanoparticles can be produced within a short time, and the process is simplified, The convenience can be enhanced.
Hereinafter, the present invention will be described with reference to Examples. However, the following Examples are intended to illustrate the present invention and the scope of the present invention is not limited thereto.
≪ Example 1 >
CuCl 2 * 5H 2 O 20 mmol,
≪ Comparative Example 1 &
20 mmol of CuCl 2 * 5H 2 O, 10 mmol of InCl 3 and 30 mmol of sodium citrate in 250 ml of distilled water. 300 mmol of NaBH 4 was dissolved in 250 ml of distilled water in a nitrogen atmosphere, and the mixed solution was added dropwise thereto over one hour. The mixture was stirred, filtered through a reduced pressure filtration method and purified with distilled water to obtain Cu-In metal nano-particles.
<Experimental Example 1>
The metal nanoparticles prepared in Example 1 and Comparative Example 1 were observed with an electron microscope (SEM) and subjected to XRD analysis, and they are shown in FIG. 7 to FIG.
Comparing the SEM photograph (FIG. 7) of the metal nanoparticles prepared in Example 1 with the SEM photograph (FIG. 9) of the metal nanoparticles prepared in Comparative Example 1, And the XRD analysis graph (FIG. 8 and FIG. 10) are compared, it can be confirmed that the composition is also similar.
<Experimental Example 2>
The time required for obtaining the same amount of metal nanoparticles from Example 1 and Comparative Example 1 was measured, and the results are shown in Table 1 below. In the case of Comparative Example 1, the synthesis process was repeated several times to obtain the same amount of metal nanoparticles.
Referring to Table 1, it can be confirmed that the time required for obtaining the same amount of metal nanoparticles was reduced by 1/30 as compared with Comparative Example 1 when the method of Example 1 was used.
From this, it can be seen that the method of synthesizing metal nanoparticles according to the present invention significantly reduces the reaction time while maintaining the shape and composition of the particles in comparison with the case of the conventional batch type synthesis method. Efficiency and convenience, which are suitable for mass production.
While the present invention has been described with reference to the drawings and embodiments, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (22)
(i) preparing a first solution containing a reactant containing two or more metal salts, a second solution containing a reducing agent, and a buffer solvent and storing them in a first tank, a second tank, and a third tank, respectively;
(ii) injecting nitrogen gas into the tanks, respectively, and injecting the fluids stored in the tanks into the flow path reactor through individual paths; And
(iii) purifying the synthesized metal nanoparticles while passing through the flow path reactor,
The flow path reactor includes:
The upper plate and the lower plate having a flat plate shape having respective flow paths,
Wherein the flow path includes at least one injection flow path through which the fluids are respectively injected, a mixing flow path through which the respective fluids injected into the injection flow paths are merged, and a discharge flow path through which the fluid merged by the mixing flow path is discharged,
Wherein the mixing flow path includes a stem flow path extending from the injection flow paths to the discharge flow path and one or more branch flow paths branched off from the stem flow path,
The fluid is subjected to a mixing process in which the fluid is branched vertically and merged laterally in the mixing of the fluid that repeats the branching and the merging,
Wherein the branch flow paths include at least one section in which the depth continuously changes with respect to the plate surface,
The bimetallic or intermetallic metal nanoparticles may be selected from the group consisting of Cu-In bimetallic metal nanoparticles, Cu-Sn bimetallic metal nanoparticles, Cu-Zn bimetallic metal nanoparticles, Sn-Zn bimetalic metal Nanoparticles, Cu-In-Ga intermetallic metal nanoparticles, and Cu-Sn-Zn intermetallic metal nanoparticles.
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