TW200811051A - Periodic table group XI or XII metal chalcogenide nanoparticles and production process thereof - Google Patents

Abstract

This invention provides periodic table group XI or XII metal chalcogenide nanoparticles including liquid crystal molecules by a method that can be easily carried out in mass production scale. The periodic table group XI or XII metal chalcogenide nanoparticles being useful for industrial application.

Description

200811051 IX. Description of the invention: [Technical field to which the invention pertains] The servant is a group n or 12 group metal chalcogenide nanoparticle of the periodic table and a method for producing the same. The π-group or (iv) metal chalcogenide nanoparticles of the periodic table, for example, the two-tune T, for example, are useful compounds for lowering the driving voltage of the liquid crystal display. [Prior Art] In the method of manufacturing the Group 11 metal chalcogenide particles in the periodic table, the ionic and chalcogenide precursors are obtained by dissolving and removing the alkali metal and alkaline earth gold by ultrasonic treatment. A method of synthesizing a metal chalcogenized hazelnut (for example, refer to Patent Document 1). However, in this case, it is necessary to use an ultrasonic disperser by the processing of ultrasonic waves, and not f: as a method of mass production in the industry. Further, in Patent Document 1, there is no mention of the group 12 metal chalcogenide nanoparticle of the _ period table [Patent Document 1]: JP-A-2003_1096 [Summary of the Invention] (Problem to be solved by the invention) The problem of the present invention is to solve the above problems, and to provide a liquid crystal molecule containing a liquid crystal molecule of Group 11 or a 12th 1 genus & L gene nanoparticle, and to provide an industrial A preferred method for producing a Group 11 or Group 12 metal chalcogenide nanoparticle of the periodic table containing liquid crystal molecules. (Means for Solving the Problem) 5 319452 200811051 The subject of the present invention is to obtain two or more kinds of liquid crystals by using 丨 or two or more kinds of metal chalcogenides of the periodic table or two or more kinds thereof. The π or 12 group metal chalcogenide nanoparticles of the periodic table of the knife are solved. The subject of the present invention is to produce two or more liquid crystal molecules, a work type, or two or more kinds of metal salts of Group 11 or Group 12 of the periodic table, and Or 2, the above chalcogenide precursor is reacted in a solvent, and is solved by the manufacture of the Group 11 or Group 12 metal chalcogenide nanoparticles of the above periodic table. (Effect of the Invention) - According to the present invention, there is provided a method which can be easily produced in a large amount, and a metal chalcogenide of the group u or 12 of the periodic table having liquid crystal molecules

The present invention also provides an industrially suitable group 11 or group 12 metal chalcogenide nanoparticle of the periodic table containing liquid crystal molecules. [Embodiment] The invention is not invented into two or more types: sulfur a compound, and a periodic epiphany group 11 or a group 12 metal chalcogenide nanoparticle containing one or more liquid crystal molecules, or a seed crystal or two or more kinds of liquid crystal molecules q or more than two kinds of weeks = The phenanthrene-free or Group 12 metal salt and chalcogenide precursor are suitably produced by retanning in a solvent. w The liquid crystal molecule used in the reaction of the present invention may, for example, be a cyano group such as 4, n-pentyl cyanobiphenyl or 4, n-hexyloxy 4 cyanobiphenyl 319452 6 200811051 benzene ;4·(trans-4-n-pentylcyclohexyl)benzonitrile and other cyclohexylbenzonitrile dogs, 4-n-pentyl-4-ethoxy-2,3-difluorobiphenyl, B Oxygen _23__ 'Leading formula I n-decylcyclohexyl) benzene and other gas benzenes; 4_1 resting =, (4-ranyl phenyl) ester, 4-heptyl benzoic acid (cardiocyanophenyl) vinegar, etc. Phenyl vinegar; 4-carboxyphenylethyl carbonate, 4-sided phenyl-n-butyl carbonate vinegar, etc.; 4-(4-n-pentylphenylvinyl) cyanobenzene, 4_( Phenyl E block of 4_n-pentylphenylvinyl)fluorobenzene; 2_(4_ylphenyl)_5_dipentyl, 2_(4·cyanophenyl)_5_正辛基(四)#的phenyl (4) azobenzenes such as 4,4-bis(ethoxylated azo) azobenzene; (4,4,· oxidized azo anion test, 4, 4, _Dihexyl oxyazobenzene, etc., oxidized azo, N_(4_methoxyphenylidene n-butylaniline, N♦ ethoxy, it n-butylaniline, etc. Schiff bases; N, N, bis-benzylidene-based cholesteryl-based genus; poly(Λ^Λ曰, cholesteryl benzoic acid vinegar w ν λ κ (this phenyl group to chelating amine) liquid crystal High score two: This liquid crystal molecule can be used alone or in combination of two or more. The liquid helium/knife mixture can be directly used as a commercial product. The use of the 12-series is relative to the 11th or 12th of the periodic table. Teach metal salt! Moore, preferably 200 m. 1 to 5 (10) Moule, better! To the full range of the periodic table used in the 11th or the & 矣 盥 篱 篱 J J 表 表 11 a salt of a family or a Group 12 metal salt which is formed by a pair of ions. The foregoing week is, for example, selected from the group consisting of AU, Au3+, and A + 1 2 genus, at least one of which is infiltrated into CU, CU a metal ion of the group of the above-mentioned group. The ion of the metal of the above-mentioned periodic table (1), 319452 7 200811051, for example, may be selected from the group consisting of Zn2+, Cd2+, and at least one of the inclusions 2 § g In the middle of the second: the ion can be exemplified by: dentate ion, tooth acid; strontium ion, carboxylic acid ion which can also be substituted, acetamidine嗣其ί Γ ^_子, sulfate ion, meal ion, tetrafluorochemical ion, acid ion, counter ion of the metal of Group 11 of the periodic table, for example, hydride ion, metal such as H Salt-neutral ligands (for example, carbon monoxide, triphenylphosphine, rhyme = ah, etc.) can also be coordinated. Also, the periodic table: the first, !] no or brother The Group 12 metal salt may be used singly or in combination of two or more. The Group 4.5 or Group 12 metal chalcogenide 'character used in the reaction of the present invention means the Group u or Group 12 of the periodic table. The combination of the metal and the elements of the underlying oxygen (sulfur, silli, and samarium) of the table, for example, may be, for example, a claw-like stone carbide or a telluride. Further, the chalcogenide precursor system is a generic term for a metal chalcogenide (e.g., metal sulfide, metal selenide, metal telluride) formed by reacting a disc metal compound (e.g., a metal salt as previously shown). Further, these chalcogenide precursor systems may be used singly or in combination of two or more. ° a chalcogenide precursor (vulcanizing agent) for synthesizing the aforementioned metal sulfide, and examples thereof include thioguanamines such as thioacetamide, hydrazine, hydrazine dimethyl thioacetamide; sulfur; Arsenic sulfide; sulfur compounds such as sulfur urea, hydrazine, hydrazine dimethyl thiourea; alkali metal sulfides such as sodium sulfide and potassium sulfide; alkali metal hydrogen sulfides such as sodium hydrogen sulfide and potassium hydrogen sulfide . Preferably, it is a thiolamine, a sulfur urea, an alkali metal sulfide, and a hydrogen sulfide can also be used in the synthesis of the Group 12 metal sulfide of the periodic table, more preferably a thiourethane or a sulfur urea. 8 200811051 It is also possible to use hydrogen sulfide when it is a metal sulfide of Group 12. Further, these chalcogenide precursors (vulcanizing agents) can be used singly or in combination of two or more. From the chalcogenide precursor used to synthesize Lithium metal selenide (selenization =])', for example, selenium; hydrogen selenide, selenium acetamide, N, N-dimethyl selenide Such as "amines; selenium urea, N-extension dimethyl hydrazine urea, etc. urea / sodium selenide, potassium selenide and other alkali metal selenides; sodium hydrogen selenide, > potassium hydrogen selenide, etc. Alkali metal hydrogen selenide. Preferably, selenium, selenium amide, selenium and urea are used. Further, hydrogen selenide may be used in the synthesis of the 12th metal selenide of the periodic table, more preferably selenium or selenium urea, and the synthesis cycle table Η = metal In the case of Wei Shi, it is also possible to cause hydrogen to collapse. Further, these chalcogenide precursors (selenization agents) may be used singly or in combination of two or more. a chalcogenide precursor (deuteration agent) for synthesizing a metal halide of a box; for example, hydrazine; hydrogen halide; hydrazine, N, dimethylamine indoleamine;碲 urea, N, N-dimercaptopurine, urea, etc.; alkali metal ruthenium such as sodium hydride or potassium hydride; alkali metal hydrazine hydride such as sodium bismuth hydride or potassium hydride class. It is preferred to use hydrazine, hydrazine urea, and alkali metal hydroquinone. Further, in the synthesis of Group 12 metal sulphides of the periodic table, hydrogen halides, more preferably hydrazines, alkali metal hydrazines, and still A vaporization cylinder can also be used for the metal halide of Group 12 of the periodic table. > Μτ 4 people' This chalcogenide precursor (deuterated agent) can be used alone or in combination 2. The amount of the chalcogenide precursor used above is preferably 1 to 5 moles per gram of the metal salt of the Xia or Group 12 metal of the periodic table, and is 319452 9 200811051 0.2 to 3 Moor. The solvent to be used in the reaction of the present invention is not particularly limited as long as it does not inhibit the reverse reaction, and examples thereof include water; ketones such as acetamidine, methyl ethyl hydrazine, and methyl isobutyl hydrazine; Ester of ethyl acetate, succinic acid, methyl diacid, etc.; N,N-dimethylformamide, N,N-dimethyl isopropylamine, N-methyl ketone, etc. Amines, _, _ dimethyl scented sputum II ^ ^ & 素 # ' - methyl slate wind and other sub-stone types; stone stone such as ring stone; acetonitrile, propionitrile and other nitriles Class; diethyl _, diisopropyl ether, tetrahydroanthracene, ^ = = 贞 贞; hexazone, 歧, cyclohexane filament hydrocarbons; #toluene -toluene and other aromatic hydrocarbons. Nitriles, ethers, and Group 2 cigarettes are preferred, and water may also be used in the metal salt of the Group u of the periodic table, and more "_, and water may also be used in the metal salt of the η group of the periodic table. The solvent of the material may be used singly or in combination of two or more kinds. (10) The amount of the solvent to be used is preferably (7) to 500 ml, more preferably 2 to 2 ml, relative to the liquid crystal molecule ig. For example, a mixture of i or two or more kinds of liquid crystals is divided into two or more kinds of metal salts of Group u or Group 12 of the periodic table, :: or two or more kinds of chalcogenide precursors and solvents, depending on the case, It is carried out by a method of heat-side (four) counter-feeding.

Lfc' is better than 4 〇 to Saki, and the reaction pressure at that time is not limited. a chalcogen liquid, a dispersion containing a Group U metallized nanoparticle of the periodic table and a solvent can be obtained by the reaction of the present invention, but by concentrating the dispersion, a metal containing a uniform periodic group u or a lanthanum can be obtained. Chalcogen 319452 10 200811051 Paste of nanoparticle and solvent. Further, the method for concentrating the dispersion is not particularly limited, and it is preferably carried out at 20 to 100 ° C under reduced pressure. ‘[Examples] ^ Next, the present invention will be specifically described by way of examples, but the scope of the invention is not limited thereto. Example 1 (Synthesis of Silver Sulfide Nanoparticles) 4'-n-pentyl-4-cyanobiphenyl 10 0.66 g was added to a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser in an internal volume of 100 ml ( 2.64mmol), four screams of 45,0ml, water 0.051111 and 0.01 mol / liter of thioacetamide in tetrahydroanthracene sulphur solution 1.65ml (0.0165mmol), heated to 65 to 75 ° while stirring the mixed solution C. Then, 3.30 ml of a tetrahydrofuran solution of 0.01 mol/liter of silver trifluoroacetate (0.033 mmol of a silver atom) was slowly dropped to carry out a reaction. After the completion of the reaction, the reaction solution was cooled to room temperature to form a uniform liquid of brownish brown, and 50 ml of a silver sulfide nanoparticle dispersion was obtained. Further, as a result of analysis by a transmission electron microscope, the silver sulfonated silver nanoparticles have a particle diameter of 10 to 30 nm and are uniform (Fig. 1). Further, the dispersion containing the obtained silver sulfide nanoparticles was concentrated under reduced pressure to obtain a silver brown uniform silver sulfide nanoparticle paste 〇.67 g. Example 2 (Synthesis of Silver Sulfide Nanoparticles) In a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser having an internal volume of 100 ml, 4'-n-pentyl-4-cyanobiphenyl 0,66 g ( 2.64 mmol), 45.0 ml of tetrahydrofuran, 0.05 ml of water, and 1.60 ml (0.0165 mmol) of a tetrahydrofuran solution of 0·01 mol/liter of sulphur, and heated to 65 to 75 while stirring the mixed solution. °C. Then, a reaction was carried out by gently dropping 3.30 ml of a 0.01 mol/l chloroauric acid tetrahydrofuran solution (0.033 mmol of a silver atom) under 11 319452 200811051. After the completion of the reaction, the mixture was cooled to room temperature to form a uniform liquid of brownish brown, and silver sulfide nanoparticles and 50 ml of a dispersion were obtained. Further, as a result of analysis by a transmission electron microscope, the particle size of the silver sulfide nanoparticles was 10 to 30 nm and was uniform (Fig. 2). Further, the dispersion containing the obtained silver sulfide nanoparticles was concentrated under reduced pressure to obtain a silver brown uniform silver sulfide nanoparticle paste 〇.67 g. Example 3 (Synthesis of Copper Sulfide Nanoparticles) . In a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser having an internal volume of 100 ml, 4'-n-pentyl-4-cyanobiphenyl 0.66 g ( 2.64 mmol), tetrahydrofuran, 43, 4 ml, water 0.05 ml, and 0.01 mol/L of thioacetamide in tetrahydrofuran, 3.30 ml # (0.033 mmol), and heated to 65 while stirring the mixed solution. 75 ° C. Then, 3.00 ml (copper atom: 0.033 mmol) of a solution of 0.01 mol/liter of copper(II) trifluoroacetate in tetrahydrofuran was gradually dropped to carry out a reaction. After the completion of the reaction, the mixture was allowed to cool to room temperature to form a uniform liquid of brownish brown, and 50 ml of a copper sulfide nanoparticle dispersion was obtained. Further, as a result of analysis by a transmission electron microscope, the particle size of the copper sulfide nanoparticles was about 2 nm and was uniform (Fig. 3). Further, the dispersion containing the obtained copper sulfide nanoparticles was concentrated under reduced pressure to obtain a brownish-smooth copper sulfide nanoparticle paste 0,67 g. Example 4 (Synthesis of copper sulfide nanoparticles) 4, n-pentyl-4-cyanobiphenyl 12 319452 200811051 0.66g (2.64mmol), tetrahydrofuran 43.4ml in a glass vessel with a stirring device, thermometer and reflux cooler. 0.05 ml of water and 0.10 ml of a tetrahydrogenated solution of 0/01 mol/liter of sulphur ethyl s-amine, while stirring the mixture to 65 to 75 ° C while stirring. Then, 3.00 ml of a tetrahydrofuran solution of 0.01 mol/liter of copper (II) acetate (0.033 mmol of copper atom) was slowly dropped to carry out a reaction. After the completion of the reaction, the mixture was cooled to room temperature to form a uniform liquid of brownish brown, and 50 ml of a copper sulfide nanoparticle dispersion was obtained. Further, as a result of analysis by a transmission electron microscope, the particle size of the copper sulfide nanoparticles was 10 to 30 nm and was uniform (Fig. 4). Further, the dispersion containing the obtained copper sulfide nanoparticles was concentrated under reduced pressure to obtain a copper brown uniform copper sulfide nanoparticle paste 67.67 g. Example 5 (Synthesis of Copper Sulfide Nanoparticles) In a glass vessel having a volume of 100 ml with a stirring device, a thermometer and a reflux condenser, '4'-n-decyl-4·glycolbiphenyl 0.66 g (2.64) was added. Methyl), tetrahydroanthracene 43.4ml, water 0.05ml and 0. 01 mole / liter of thioacetic acid amine tetrahydrofuran solution 3.30ml # (0.033mmol), while stirring the mixed solution heated to 65 to 75 °C. Then, a tetrahydrofuran solution of 0.01 mol/liter of copper (II) ethenylacetone ligand was slowly dropped, 3.3 〇 1111 (copper atom: 0.033111111 〇 1), and the reaction was carried out. After the completion of the reaction, the mixture was cooled to room temperature to form a uniform liquid of brownish brown, and 50 ml of a copper sulfide nanoparticle dispersion was obtained. Further, as a result of analysis by a transmission electron microscope, the particle size of the copper sulfide nanoparticles was about 2 nm and was uniform (Fig. 5). Further, the dispersion containing the obtained copper sulfide nanoparticles was concentrated under reduced pressure to obtain a brownish-smooth copper sulfide nanoparticle paste 0.67 g 〇13 319452 200811051 Example 6 (copper sulfide nanoparticle) Synthesis) Add 4'-n-decyl-4 fluorenylbiphenyl v 0.66g (2.64mmol), tetrahydrogen in a glass container with a stirring device, a thermometer and a reflux cooler with an internal volume of -10 0 m 1 43.4 ml of sigma, 0.05 ml of water, and 3.01 ml of sulphur acetamide were added to 3.30 ml # (0.033 mmol), and the mixture was heated to 65 to 75 ° C while stirring. Then, 3.30 ml (copper atom: 0.033 mmol) of a tetrahydrogen humming solution of 0.01 mol/liter of copper (II) tetrafluoroborate was slowly dropped to carry out a reaction. After the completion of the reaction, the mixture was allowed to cool to room temperature to form a brownish homogeneous liquid, and 50 ml of a copper sulfide nanoparticle dispersion was obtained. Further, by analysis by a transmission electron microscope, the copper sulfide nanoparticles have a particle diameter of about 2 nm and are uniform (Fig. 6). Further, the dispersion containing the obtained copper sulfide nanoparticles was concentrated under reduced pressure to obtain a brownish-smooth copper sulfide nanoparticle paste 0.67 g. Example 7 (Synthesis of silver halide nanoparticles) φ In a glass vessel having a 100 ml inner volume of a stirring device, a thermometer, and a reflux condenser, 4, n-pentyl-4-cyanobiphenyl 0.66 g (2.64 mmol), four flavors 43.4 ml, and 4.mg (0.033 mmol) of hoof, then 6.60 ml of a tetrahydrofuran solution of silver 升·〇1 mol/liter of trifluoroacetic acid (0.066 mmol of silver atom), and heated to 65 to 75 ° C while stirring the mixed solution. , carry out the reaction. After the completion of the reaction, the mixture was cooled to room temperature to form a grayish white uniform liquid, and 50 μm of the silver halide nanoparticle dispersion was obtained, and the result of analysis by a transmission electron microscope was carried out. The diameter is 3 to 15 nm and is uniform (Fig. 7). Further, 14 319452 200811051, and the dispersion containing the obtained silver halide nanoparticle was concentrated under reduced pressure to obtain an off-white uniform silver halide nanoparticle paste 〇.67 g. Example 8 (Synthesis of Silver Telluride Nanoparticles) - A liquid crystal molecular mixture (ZLI-5100-100 (manufactured by Merck) was added to a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser in an internal volume of 100 ml. 0.50 g, 44.0 ml of tetrahydrofuran, and 3.8 mg (0.030 mmol) of hydrazine, and then added 6.00 ml of a tetrahydrofuran solution of 0.01 mol/L of trifluoroanthrolate (the silver atom is 0.060 mmol) while stirring The mixed solution is heated to 65 to 75 ° C to carry out the reaction. After the reaction is finished, the mixture is cooled to room temperature to form a grayish white uniform liquid, and a silver halide nanoparticle dispersion liquid is obtained by 50 m. As a result of analysis by a transmission electron microscope, the silver halide nanoparticles have a particle diameter of 3 to 15 nm and are uniform (Fig. 8). Further, the dispersion containing the obtained silver halide nanoparticle is reduced. The mixture was concentrated under pressure to obtain an off-white uniform silver halide nanoparticle paste 0.51 g. φ Example 9 (synthesis of silver halide nanoparticle) The internal volume of the stirring device, the thermometer, and the reflux cooler was 100 ml. In a glass container, liquid crystal molecules are mixed. (MLC-6054-100 (manufactured by Merck) 0.50g, Sikukou South 44.0ml, and 碲3.8mg (0.030mmol), then added 0.01mol / liter of trifluorofuranic acid tetrahydrofuran solution 6.0 〇1111 (the silver atom is 0.06〇111111〇1), and the reaction is carried out while stirring the mixed solution to 65 to 75 ° C. After the reaction is finished, the mixture is cooled to room temperature to form a grayish white uniform liquid. 50 ml of a silver halide nanoparticle dispersion was obtained, and the result of analysis by 15 319452 200811051 by a transmission electron microscope showed that the silver halide nanoparticles had a particle size of 3 to 15 nm and were uniform (Fig. 9). Further, the dispersion liquid containing the obtained silver halide nanoparticle was concentrated under reduced pressure to obtain an off-white uniform silver halide nanoparticle and a sub-paste 0.51 g. Example 10 Synthesis of rice particles) A liquid crystal molecular mixture (MLC-6292-100 (manufactured by Merck), 0.50 g, tetrahydroanthracene, 44.0 ml, was added to a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser in an internal volume of 100 ml. And 碲3.811^ _ (0.030mmol), then add 0.01m / liter three The tetrahydrofuran solution of fluorolu-g complex silver is 6·00πι1 (the silver atom is 0.060 mmol), and the mixture is heated to 65 to 75 ° C while stirring the reaction solution to carry out the reaction. After the reaction is finished, the mixture is cooled to room temperature. , a grayish white homogeneous liquid is formed, and 50 ml of a silver telluride nanoparticle dispersion is obtained. The result of analysis by a transmission electron microscope, the silver halide nanoparticle has a particle size of 3 to 15 nm and is uniform (the first) 10)). Further, the dispersion 0 containing the obtained silver halide nanoparticle was concentrated under a storage pressure to obtain an off-white uniform silver halide nanoparticle paste 0 · 51 g 〇 Example 11 Synthesis of rice particles) A liquid crystal molecular mixture (MLC-6608 (manufactured by Merck), 0.50 g, tetrahydrofuran, 44.0 m, and 碲3.8) was placed in a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser. Mg (0.030 mmol), then 6.00 ml (silver atom: 0.060 mmol) of a tetrahydrofuran solution of 0.01 mol/L of trifluorosilic acid was added, and the mixture was heated to 65 to 75 ° C while stirring, and the reaction was carried out. After the end of the reaction, 16 319452 200811051 The mixture was cooled to room temperature to form a grayish white uniform liquid, and 50 ml of a silver telluride nanoparticle dispersion was obtained. The result of the analysis by a transmission electron microscope was analyzed. The particle size of the rice particles is 3 to 15 nm and is uniform (first image). Further, the dispersion containing the obtained silver halide nanoparticle is concentrated under reduced pressure to obtain a uniform grayish white color. Silver nanoparticle paste 0.51 g of the agent. Example 12 (Synthesis of silver halide nanoparticles) A liquid crystal molecular mixture (MLC-6692 (Merck) was added to a glass container containing a stirring device, a thermometer, and a reflux condenser. Preparation) 0.50g, 44.0ml of tetrahydrofuran, and 3.8mg (0.030mmol) of hoof, then add 0.01ml / liter of silver trifluoroacetate in tetrahydrofuran solution 6.00ml (silver atom is 0.060mmol), while stirring The mixed solution was heated to 65 to 75 ° C to carry out a reaction. After the reaction was completed, the mixture was cooled to room temperature to form a grayish white homogeneous liquid, thereby obtaining 50 ml of a silver halide nanoparticle dispersion. As a result of analysis 10 by an electron microscope, the particle size of the silver telluride nanoparticles was 3 to 15 nm and was uniform (Fig. 12). Further, the dispersion containing the obtained silver halide nanoparticles was decompressed. Concentration was carried out to obtain a grayish white uniform silver halide nanoparticle paste 0.5 lg. Example 13 (Synthesis of tin sulfide nanoparticles) The internal volume of a stirring device, a thermometer, and a reflux condenser was 10 0 Hi 1 In the glass, add 4' - n-mercapto-4 - gas-based stupid 0.7 0 g (2·81 mmo 1), tetrahydrofurfuryl 46.3 ml, water 0.05 ml and cadmium acetate acetone ligand 11.5 mg (0.037 mmol), while stirring The mixed solution was heated to 65 to 75 ° C on the side of 17 319452 200811051. Then, 3.70 ml of a tetrahydrofuran solution of 〇·〇1 mol/liter thioacetamide was slowly dropped to carry out a reaction. After the completion of the reaction, the mixture was cooled to room temperature to form a pale yellow homogeneous liquid to obtain cadmium sulfide. The nanoparticle dispersion was 50 ml. Further, as a result of analysis by a transmission electron microscope, the cadmium sulfide nanoparticles have a particle diameter of 5 to 10 nm and are uniform (Fig. 13). Further, the dispersion containing the obtained cadmium sulfide nanoparticles was concentrated under reduced pressure to obtain a light yellow uniform cadmium sulfide nanoparticle paste 0.71 g of hydrazine 10 Example 14 (Zinc sulfide nanoparticle) Synthetic) Add 4'-n-decyl-4-oxylbiphenyl 0.66g (2.64mmol), tetrahydroanthine to south 43.4ml in a glass container with a stirring device, a thermometer and a reflux condenser. 3.50 ml of a solution of 0.05 ml of water and 0. 01 mol/liter of thioacetamide in tetrahydrofuran, and heating to 65 to 75 ° C while stirring the mixed solution. Then, 3.30 ml (zinc atom: 330.033 mmol) of a tetrahydrofuran solution of 〇·〇1 mol/liter acetoxyacetone ligand was slowly dropped, and the reaction was carried out. After the completion of the reaction, the mixture was cooled to room temperature to form a colorless homogeneous liquid, and 50 ml of a zinc sulfide nanoparticle dispersion was obtained. Further, as a result of analysis by a transmission electron microscope, the zinc sulfide nanoparticles have a particle diameter of 2 to 10 nm and are uniform (Fig. 14). Further, the dispersion containing the obtained sulfided nanoparticles was concentrated under reduced pressure to obtain 0.67 g of a pale yellow uniform zinc sulfide nanoparticle paste. Example 15 (Synthesis of Zinc Sulfide Nanoparticles) A liquid crystal molecular mixture (MLC-6692 18 319452 200811051 (manufactured by Merck) 0.50 g was added to a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser in an internal volume of 100 ml. 47 ml of tetrahydrofuran, 0.05 ml of water, and 7.8 mg (0.03 mmol) of zinc acetoacetone ligand, while stirring the mixed solution, while heating to 65 to 75 T: Then, slowly dropping 0·01 Mo The reaction was carried out by reacting 3.0 ml of a solution of urethane/limine with tetrahydrofuran. After the reaction was completed, the mixture was cooled to room temperature to form a colorless uniform liquid, and a dispersion of 50 μm of the zinc sulfide nanoparticle was obtained by penetrating. As a result of analysis by a type electron microscope, the particle size of the zinc sulfide nanoparticle was 2 to 10 nm and was uniform (Fig. 15). Further, the dispersion 10 containing the obtained zinc sulfide nanoparticle was subjected to a reduced pressure. Concentration to obtain a pale yellow uniform zinc sulfide nanoparticle paste (K51g 〇 Example 16 (synthesis of zinc sulfide nanoparticle) in a glass containing 100 ml of a stirring device, a thermometer, and a reflux cooler A liquid crystal molecule mixture (MLC_6608 (manufactured by Merck), 0.50 g, tetrahydrofuran 47 ml, water 0.05 ηι1, and zinc acetylacetone ligand 7.8 mg (0.03 mmol) were added, and the mixed solution was stirred. The mixture was heated to 65 to 75 ° C. Then, 3.0 ml of a 0.01 mol/liter thioacetamide tetrahydrofuran solution was slowly dropped to carry out a reaction. After the reaction was completed, the mixture was cooled to room temperature to form a colorless uniform liquid. The obtained zinc sulfide nanoparticle dispersion liquid was analyzed by a transmission electron microscope, and the particle diameter of the zinc sulfide nanoparticle was 2 to 10 nm and was uniform (Fig. 16). The obtained dispersion of zinc sulfide nanoparticles was concentrated under reduced pressure to obtain 0.50 g of a pale yellow uniform zinc sulfide nanoparticle paste. Example 17 (Synthesis of zinc telluride nanoparticles) 19 319452 200811051 A mixture of a stirring device, a thermometer, and a reflux condenser was placed in a 100 ml glass vessel, and a liquid crystal molecule mixture (ZLI-5100-100 Le (Merck) 0.50 g, tetrahydrofuran 44.0 ml, zinc acetonitrile acetone was added. - Bit base 8.1 mg (0.030 mmol), then 碲3.8 mg (0.030 mmol) was added, and the mixture was stirred while heating to 65 to 75 ° C to carry out the reaction. After the reaction was completed, the mixture was cooled to room temperature to form a colorless uniformity. The liquid was obtained, and 50 μm of the zinc telluride nanoparticle dispersion was obtained, and as a result of analysis by a transmission electron microscope, the particle size of the deuterated nanoparticle was 3 to 15 nm 10 and was uniform (Fig. 17). Further, the dispersion containing the obtained deuterated Nylon particles was concentrated under reduced pressure to obtain a colorless uniform zinc halide nanoparticle paste 〇.51 g. Example 18 (Synthesis of zinc telluride nanoparticles) A liquid crystal molecular mixture (MLC-6054-100 (manufactured by Merck)) was added to a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser in an internal volume of 100 ml. 50 g, 44.0 ml of tetrahydrofuran, 3.8 mg (0.030 mmol) of zinc acetylacetone with φ, and then added 3.8 mg (0.030 mmol), and heated to 65 to 75 = while stirring the mixed solution. After the reaction was completed, the mixture was cooled to room temperature to form a colorless homogeneous liquid, and 50 ml of a zinc telluride nanoparticle dispersion was obtained. The result of analysis by a transmission electron microscope was used to deuterate the nanoparticles. The particle size is 3 to 15 nm and is uniform (Fig. 18). Further, the dispersion containing the obtained deuterated Nylon particles is concentrated under reduced pressure to obtain a colorless uniform zinc halide. Particle paste 0.51 g. Example 19 (Synthesis of zinc telluride nanoparticles) 20 319452 200811051 A liquid crystal molecular mixture (MLC-6292) was added to a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser in an internal volume of 100 ml. -100 (manufactured by Merck), 0.50 g, tetrahydrofuran (44.0 ml, zinc acetoacetate, 8.1 mg (0.030 mmol), and then 3.8 mg (0.030 mmol) of the hoof, and heated to 6 5 while disturbing the mixed solution. The reaction was carried out at 75 ° C. After the completion of the reaction, the mixture was cooled to room temperature to form a colorless homogeneous liquid, and 50 μm of the zinc telluride nanoparticle dispersion was obtained and analyzed by a transmission electron microscope. The zinc telluride nanoparticle has a particle size of 3 to 15 nm and is uniform (Fig. 19). Further, the dispersion containing the obtained zinc telluride nanoparticles is concentrated under reduced pressure to obtain a colorless color. a uniform zinc halide nanoparticle paste 0.51 g. Example 20 (Synthesis of zinc telluride nanoparticles) Liquid crystal molecules were added to a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser in an internal volume of 100 ml. Mixture (MLC-6608 (manufactured by Merck), 0.50 g, 44.0 ml of tetrahydrocyanate, 8.1 mg (0.030 mmol) of ethyl acetonide, and 3.8 mg (0.030 mmol) of hydrazine, and stirred while stirring The mixed solution is heated to 65 to 75 ° C while being heated. After the reaction is completed, the mixture is allowed to cool to room temperature to form a colorless uniform liquid, and 50 μm of the zinc telluride nanoparticle dispersion is obtained, and the result of analysis by a transmission electron microscope is performed. The particle diameter of the particles is 3 to 15 nm and is uniform (Fig. 20). Further, the dispersion containing the obtained zinc telluride nanoparticles is concentrated under reduced pressure to obtain a colorless uniform zinc phthalide. Rice particle paste 0.51 g. Example 21 (Synthesis of Hoofed Nanoparticles) 21 319452 200811051 A liquid crystal molecular mixture (Mlc_6692 _ (Merck)) was added to a glass vessel having a stirring apparatus, a thermometer, and a reflux condenser in an internal volume of 100 ml. 5〇g, 44.0ml of tetrahydrofuran, zinc acetylacetone, and 8*lmg (0.030mmo1), then 碲3.8mg (〇.〇3〇mm〇1), and heated while stirring the mixture The reaction was carried out at 65 to 75 ° C. After the reaction was completed, the mixture was cooled to room temperature to form a colorless homogeneous liquid, and 5 〇 ml of a zinc telluride nanoparticle dispersion was obtained, which was analyzed by a transmission electron microscope. As a result, the particle size of the zinc telluride nanoparticles is 3 to _ and is uniform (Fig. 21). Further, the dispersion containing the obtained zinc telluride nanoparticles is concentrated under reduced pressure to obtain Colorless uniform zinc halide nanoparticle paste 〇· 51 g. '[Industrial use possibility] This work is about a liquid crystal molecule containing the periodic table 11th 戋 group 12 metal chalcogenide Rice particles and their manufacturing method. The Group 11 or Group 12 metal chalcogenide nanoparticles are, for example, useful compounds for lowering the driving voltage of a liquid 10-crystal display. 彳 [Simplified illustration] Silver sulfide silver nanoparticles of silver sulfide nanoparticles Fig. 1 is a transmission electron micrograph synthesized by the method of Example 1. Fig. 2 is a transmission electron micrograph synthesized by the method of Example 2. Copper sulfide copper nanoparticles of copper sulfide nanoparticles Fig. 3 is a transmission electron micrograph synthesized by the method of Example 3. Fig. 4 is a transmission electron micrograph of 319452 22 200811051 synthesized by the method of Example 4. Fig. 5 is a fifth embodiment. A transmission electron micrograph of the method. The copper sulfide nanoparticle of Fig. 6 is a transmission electron micrograph of the red square of Example 6. The copper sulfide nanoparticle is shown in Fig. 7 Example 7, i. go to 4, telluride) nano-particles of transmissive electrons / smashed silver (silver) weaving micro-pound day

Figure 8 is a diagram showing the method of Example 8. Transmission electron micrograph. The deposited silver nanoparticles are shown in Fig. 9 as a transmission electron micrograph of the method of Example 9. The hoofed silver nanoparticles are shown in the first section as a transmission electron micrograph of the Example 1 〇. The silver halide nanoparticle synthesized by the method Fig. 11 is a transmission electron micrograph of the method of Example 11. The synthesized silver halide nanoparticles Fig. 12 is a transmission electron micrograph of the human and the subunits in the method of Example 12.碲 碲 银 奈 第 第 第 第 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 Sulfide ore nanoparticle Figure 14 is a transmission electron micrograph of the human and child in the method of Example 14. <Silver zinc nitride nanoparticle Fig. 15 is a transmission electron micrograph of the synthesized product by the method of Example 15. '^Zinc sulfide nanoparticle Figure 16 is taken as the method of Example 16. Zinc sulfide nanoparticle 319452 23 200811051 The transmission electron micrograph of the sub-particle. Fig. 17 is a transmission electron micrograph of the human body by the method of Example 17. Fig. 18 is a transmission electron micrograph of Example 18, and Fig. 19 is a transmission electron micrograph of Example J9. Fig. 2 is a transmission electron micrograph of Example 20 The figure is obtained by using a transmission electron micrograph of Example 21 to form a zinc sulphide nanoparticle into a zinc sulphide nanoparticle, a zinc sulphide nanoparticle, and a method of zinc crystallization. The method of combining the methods of the merged method

twenty four

Claims (1)

200811051 X. The scope of application for patents: 1. A metal chalcogenide nanoparticle of the period u or 12, • It contains one or more of the periodic table of the 丨 或 or the 12th group of gold. It is a chalcogenide and a 11th or 12th metal chalcogenide nanoparticle of the periodic table containing one or more liquid crystal molecules. 2. The nanoparticle according to item 1 of the patent application, wherein the particle diameter is 2 to 50 nm 〇 3 · a dispersion containing the nanoparticle and the solvent of the first or second aspect of the patent application. 4. A paste comprising the nanoparticles of the first or second aspect of the patent application and one or more liquid crystal molecules. 5. The method for producing a nanoparticle according to claim 1 or 2, wherein one or more liquid crystal molecules, one or more metal salts of Group 11 or Group 12 of the periodic table are used. And one or two or more chalcogenide precursors are reacted in a solvent. _ 6· The method for producing nano particles according to the scope of claim patent, which is in the range of 4〇 to 1〇〇. The reaction is carried out under the armpits. 7. The method for producing a dispersion according to item 3 of the patent application, which is a work type or two or more kinds of liquid crystal molecules, one or more metal salts of Group II or Group 12 of the periodic table, and one type Or two or more kinds of chalcogenide sodium precursors are reacted in a solvent. 8. The method for producing a dispersion according to claim 7, which is carried out at 4 to 100 c. 9. The paste of claim 4 of the patent application is obtained by the dispersion obtained by the method of claim 319452 25 200811051, item 7 or 8. 10. The paste according to claim 9 of the patent application, wherein the paste is obtained by concentrating the dispersion. 26 319452 200811051 VII. Designated representative map: (1) The representative representative of the case is: (1). (2) Brief description of the symbol of the representative figure: No component symbol 8. If there is a chemical formula in this case, please disclose the chemical formula that best shows the characteristics of the invention: This case does not represent the chemical formula 319452