WO2006009124A1 - 蛍光体、及びその製造方法 - Google Patents
蛍光体、及びその製造方法 Download PDFInfo
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- WO2006009124A1 WO2006009124A1 PCT/JP2005/013185 JP2005013185W WO2006009124A1 WO 2006009124 A1 WO2006009124 A1 WO 2006009124A1 JP 2005013185 W JP2005013185 W JP 2005013185W WO 2006009124 A1 WO2006009124 A1 WO 2006009124A1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
- C09K11/621—Chalcogenides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
- C09K11/582—Chalcogenides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
Definitions
- the present invention relates to a phosphor and a method for producing the same. Specifically, the present invention relates to a phosphor that generates near-infrared fluorescence from visible light and a method for manufacturing the same. More specifically, the present invention relates to phosphors including semiconductor nanoparticles capable of performing modification or staining of biological materials, phosphors for semiconductor light sources used for illumination, displays, and the like, and methods for producing the phosphors. . Background art
- Patent Document 1 Special Table 2003-524147
- the present inventors completed the present invention by evaluating the fluorescence characteristics by making a composite with a II-VI group compound such as ZnS.
- the present invention has been made based on the above technical background, and achieves the following object.
- An object of the present invention is to provide a low-toxic phosphor and a method for producing the same.
- Another object of the present invention is to synthesize a compound having a chalcopyrite structure, such as ZnS
- Still another object of the present invention is to synthesize a compound having a chalcopyrite structure, and III-
- a phosphor by compounding with a group V compound and a method for producing the same.
- the present invention employs the following means.
- the phosphor of the present invention provides a phosphor characterized in that it comprises a first compound having a chalcopyrite structure and also an I-III-VI group elemental force, or a composite particle or composite compound containing the first compound. To do.
- the first compound, the composite particle, or the composite compound has a particle diameter of 0.5 to 20. Onm.
- the composite compound is a compound other than the first compound, which is composed of an element of Group II VI or III V, and forms a solid solution with the first compound, thereby forming a band gap. Is desirable.
- the composite particle or composite compound is a compound other than the first compound and has a band gap force of a second compound consisting of an II-VI group or III-V group element. It contains a second compound larger than the band gap of the compound, and the lattice mismatch ratio between the lattice constant of the first compound and the lattice constant of the second compound is 5% or less. desirable.
- the first compound is composed of elements of copper (Cu), indium (In), and sulfur (S), and the second compound is zinc sulfate (ZnS), and the composite particles
- the composite compound has a composition ratio (preparation ratio) of raw materials of zinc (Zn), copper (Cu), indium (In), and sulfur (S) of 1: A: B: 4, and A is 0. 5 ⁇ 5.0, B is 0.5 ⁇ 5.0.
- the composition ratio is This does not necessarily mean the composition ratio of the phosphor, but the meaning of the raw material charge ratio (mol).
- the first compound is an elemental force of silver (Ag), indium (In), and sulfur (S)
- the second compound is zinc zinc sulfate (ZnS)
- the composite particles or The composite compound is composed of zinc (Zn), silver (Ag), indium (In), and sulfur (S) in a composition ratio (preparation ratio) of 1: A: B: 4, and A is 0.5 to 5 0, B «0.5 to 5.0 It is good to be manufactured.
- the quantum efficiency at which the first compound is excited by excitation light to emit light waves is 0.1% to 10.0% at room temperature.
- the fluorescence emitted from the first compound is a light wave having a wavelength of 550 to 800 nm.
- a raw material salt of a plurality of types of elements constituting a chalcopyrite structure compound is dissolved and mixed in a solution to which a complexing agent that coordinates to the plurality of types of elements is added.
- the first solution and the second solution in which the chalcogenite compound is dissolved are mixed and heat-treated under predetermined heating conditions.
- Examples of the chalcogenide compound include dimethyldithiocarnomic acid, dithiolcarbamate such as dimethyldithiocarbamate and dihexyldithiocarbamate, xanthate such as hexadecylxanthate and dodecylxanthate, Trithiocarboxylates such as oxadecyltrithiocarboxylic acid dodecyltrithiocarboxylic acid, zinc cadmium, magnesium, dithiophosphoric acid such as hexadecyldithiophosphoric acid dodecyldithiophosphoric acid, manganese, nickel, copper, lead, etc., sulfur, etc.
- the predetermined condition may be that the first solution and the second solution are mixed and heat-treated at a temperature of 70 to 350 ° C. Further, the predetermined condition is that the first solution and the second solution are mixed and heat-treated for 1 second or longer and within 30 hours. The predetermined condition is that the first solution and the second solution are mixed in a microreactor having a channel with a flow path of 50 / zm to 5 mm and then reacted by heating. Furthermore, the sulfur compound is preferably zinc sulfate zinc (ZnS).
- a copper (I) or copper (II) salt and an indium (III) salt are dissolved in a solution to which a complexing agent that coordinates copper (I) and indium (III) is added. And a mixed solution.
- the composition ratio (preparation ratio) of zinc (Zn), copper (Cu), indium (In), and sulfur (S) is 1: A: B: 4, A is 0.5 to 5.0, B «0. It may be produced from a raw material strength of 5 to 5.0.
- the first solution is a solution in which a silver (I) salt and an indium (III) salt are dissolved and mixed in a solution to which a complexing agent that coordinates silver (I) and indium (III) is added. It is good to be.
- the composition ratio (preparation ratio) of zinc (Zn), silver (A g), indium (In), and sulfur (S) is 1: A: B: 4, A is 0.5 to 5.0, B is 0 The raw material strength which is 5 ⁇ 5.0 is good to be manufactured.
- the first compound a compound of chalconolite structure that also has an elemental force of group I III-VI
- the group I element is Cu
- a group III element is a compound containing one or more types of elements from In, Ga, A1
- a group VI element from S, Se, Te. It is desirable.
- the mixing ratio of the chalcopyrite compound and the compound that forms the composite can be freely changed within a range in which a solid solution or a composite structure is formed. It is desirable to compound a compound that is compounded in a molar ratio of 0.05 to 3.00, preferably 0.1 to 3.0, with respect to the group I element of the chalcopyrite compound.
- the phosphor described above is preferably spherical or spindle-shaped.
- the phosphor of the present invention and the method for producing the same are a compound comprising a group I III VI element having a chalcopyrite structure considered to be low toxicity, or a composite particle or a composite compound containing the compound. Since this composite particle or composite compound contains a group II VI or group III V element, it has become possible to provide a low-toxic semiconductor nanoparticle phosphor.
- Example 1 in which the phosphor of the present invention was manufactured is shown.
- All adjustments were made in an argon atmosphere using argon gas.
- Copper (I) iodide and indium iodide (III) were each dissolved in the complexing agent oleylamine, and further mixed using octadecene as a solvent to give solution A.
- Zinc jetyldithiocarbamate was dissolved in trioctylphosphine and mixed with octadecene to obtain solution C.
- Liquid A and liquid C were mixed and heated at 160 to 280 ° C. for a predetermined time.
- the obtained product was diluted with toluene and the absorption / fluorescence spectrum was measured. The measurement results were graphed.
- the graph of Fig. 1 illustrates the results of generating phosphors in a plurality of synthesis times.
- Figure 1 illustrates the intensity versus spectrum of light waves emitted by the generated phosphor.
- the synthesis time is 45 seconds, 60 seconds, 120 seconds, and 300 seconds.
- the vertical axis of the graph in Fig. 1 indicates the fluorescence intensity, and the horizontal axis indicates the wavelength.
- Fluorescence intensity is an arbitrary relative value (hereinafter the same) o Unit of wavelength is nanometer (hereinafter the same) o
- the composition ratio (preparation ratio) of each raw material of the phosphor Aal 211: 11: 111: 3 is 1. 0: 1. 0: 1. 0: 4.0.
- FIG. 2 shows a result of producing the phosphor at a plurality of synthesis temperatures.
- Figure 2 illustrates the intensity versus spectrum of the light wave emitted by the generated phosphor. Each graph is for synthetic temperatures of 160 ° C, 200 ° C, and 240 ° C. The vertical axis of the graph in Fig. 2 indicates the fluorescence intensity, and the horizontal axis indicates the wavelength.
- FIG. 3 shows the spectrum of a light wave emitted by irradiating a phosphor with excitation light of multiple types of wavelengths.
- Each graph shows the case where the wavelength of the excitation light is 320 nm, 380 nm, 440 nm, and 500 nm.
- the vertical axis of the graph in FIG. 3 indicates the fluorescence intensity, and the horizontal axis indicates the wavelength.
- FIG. 4 shows a graph of fluorescence intensity when the composition ratio (preparation ratio) of raw materials is changed.
- the composition ratio (preparation ratio) for each graph is shown in Table 1 below.
- the vertical axis of the graph in Fig. 4 indicates the fluorescence intensity, and the horizontal axis indicates the wavelength.
- Table 1 shows the quantum yields indicating the ratio of photons emitted by fluorescence with respect to the number of photons of excitation light absorbed by the phosphor in each graph of FIG.
- the quantum yield is obtained by dividing the number of photons in the fluorescence by the number of photons absorbed by the particles. This value was determined based on a relative comparison of the absorbance (definition will be described later) and fluorescence intensity using rhodamine B or the like having a known quantum yield as a standard substance.
- FIG. 5 shows the absorbance indicating the amount of excitation light absorbed by the phosphor of each graph of FIG.
- the vertical axis of the graph in FIG. 6 shows the absorbance as a relative value, and the horizontal axis shows the wavelength.
- Absorbance is a physical quantity defined as follows.
- Absorbance A is the intensity of incident light I and the intensity of transmitted light.
- FIG. 6 shows an emission spectrum according to the molar ratio of atoms Zn and Cu, In constituting the phosphor of each graph of FIG.
- the vertical axis of the graph in Fig. 6 shows the molar ratio of Zn, Cu, and In, and the horizontal axis shows the wavelength.
- the composition ratio (preparation ratio) for each graph is the value in Table 1.
- the size of the circle in the figure of Fig. 6 corresponds to the magnitude of the emission intensity.
- Example 1 The product of Example 1 was measured by X-ray diffraction (XRD), and the result is shown in the chart of FIG.
- the charge composition Zn: Cu: In: S in the chart of FIG. 7 is 1.0: n: n: 4.0.
- the black line directly above the horizontal axis (X axis) of the chart in Fig. 7 is Balta's CuInS, and the gray line is the bar.
- the diffraction line of Luk ZnS (from JCPDS database) is shown. From this chart, the product basically shows a chalcopyrite type structure and a Urut type structure.
- the product of Example 1 was of a spindle shape to a nearly spherical shape.
- Example 2 is basically the same as Example 1 described above, and only the differences are described below.
- the composition ratio of the phosphor raw material 211: 01: 111: 3 is 1.0: 0. 8: 0.8: 8: 4.0.
- the results of measuring the properties of the produced phosphor were graphed.
- the absorbance of the phosphor in each graph of Fig. 8 is shown in the graph of Fig. 9.
- the graph in Fig. 8 shows the intensity of the fluorescence emitted by the phosphor produced by heat treatment at a predetermined temperature of 160, 200, and 240 ° C. Heating time is 5 minutes
- the vertical axis indicates the fluorescence intensity
- the horizontal axis indicates the wavelength.
- the quantum yields of the phosphors produced by heat treatment for 5 minutes at 160, 200, and 240 ° C. were 6%, 4%, and 6%, respectively.
- the quantum yield is obtained by dividing the number of photons in the fluorescence by the number of photons absorbed by the particles. This value was obtained based on a relative comparison of absorbance and fluorescence intensity using rhodamine B or the like having a known quantum yield as a standard substance.
- the vertical axis of the graph in FIG. 9 represents the excitation light absorbance of the phosphor, and the horizontal axis represents the wavelength.
- Example 3 in which the phosphor of the present invention was produced is shown.
- the production method of Example 3 is basically the same as that of Examples 1 and 2 above, and only the differences are described below.
- Copper iodide (I) and indium iodide ( ⁇ ) were dissolved in dodecylamine as a complexing agent, respectively, and further mixed using octadecene as a solvent to give solution A.
- copper (Cu) is 0.1 mmol
- indium (In) is 0.1 mmol
- dodecylamine is 2 ml
- octadecene is 5 ml.
- the graph of Fig. 10 shows the intensity of fluorescence emitted from a phosphor produced by exciting a phosphor generated by heat treatment at predetermined temperatures of 200 and 240 ° C with 420 nm excitation light.
- the heating time is 3.5 seconds and 28.0 seconds.
- the vertical axis of the graph in FIG. 10 indicates the fluorescence intensity, and the horizontal axis indicates the wavelength.
- the maximum fluorescence wavelengths were 538, 614, and 672 nm, and the spectrum half widths (FWHM) at that time were 136, 102, and lOOnm, respectively.
- FIG. 11 shows the absorbance of the excitation light of the phosphor corresponding to the graph of FIG.
- the vertical axis indicates the excitation light absorbance of the phosphor
- the horizontal axis indicates the wavelength.
- Example 4 in which the phosphor of the present invention was manufactured will be shown.
- the production method of Example 4 is basically the same as that of Example 1 described above, and only the differences are described below.
- Silver acetate and indium acetate were each dissolved in oleylamine, a complexing agent, and further mixed using otatadecene as a solvent to give solution A.
- Zinc jetyldithiocarbamate was dissolved in trioctylphosphine and mixed with octadecene to give solution C.
- Liquid A and liquid C were mixed and heated at 160 to 280 ° C for a predetermined time.
- the obtained product is diluted with toluene and the absorption / fluorescence spectrum is measured, and the measurement result is shown in a graph in FIG.
- the vertical axis of the graph in FIG. 12 indicates the fluorescence intensity, and the horizontal axis indicates the wavelength.
- the composition ratio of raw materials (preparation ratio) for each graph in Fig. 12 is shown in Table 3.
- the conditions are a synthesis temperature of 200 ° C and a synthesis time of 300 seconds.
- Example 5 The production method of Example 5 is basically the same as that of Example 1 described above, and only the differences are described below.
- Gallium iodide, copper iodide, and indium iodide were dissolved in oleylamine, which is a complexing agent, respectively, and further mixed using octadecene as a solvent to prepare solution A.
- Zetyl dithiocarbamate was dissolved in trioctylphosphine and mixed with octadecene to give solution C.
- the synthesis temperature is specified in the diagram of FIG. 13, and the synthesis time is 300 seconds.
- the maximum value of the absorption wavelength and the fluorescence wavelength can be controlled by the molar ratio of InZGa and the heating temperature. It is also shown that the maximum value of the fluorescence wavelength can be controlled in the range of 475 to 725 nm depending on the InZGa ratio and the heating temperature!
- Example 6 The production method of Example 6 is basically the same as that of Example 1 described above, and only the differences are described below.
- zinc bisjetyl ditylcarbamate was added and heated at 200 ° C for 5 minutes to synthesize composite particles with ZnS as the shell.
- the fluorescence intensity of the ZnS composite structure particles as the product was measured.
- the excitation wavelength at the time of measurement is 340 nm.
- Figure 14 shows the measurement results. As shown in FIG. 14, an increase in fluorescence intensity was observed.
- Example 7 in which the phosphor of the present invention was manufactured is shown. Synthesis was performed using trioctylphosphine selenide as the selenium source, octadecene as the solvent, and oleylamine as the complexing agent. Zinc acetate, copper acetate ( ⁇ ) and indium iodide were all dissolved in oleylamine and mixed with octadecene, and then trioctylphosphine selenide was mixed with dissolved trioctylphosphine. This solution was heated at 220 ° C for 5 minutes to obtain the product. The resulting product produced fluorescence with a fluorescence wavelength of 600 nm by photoexcitation at 400 nm.
- Example 8 in which the phosphor of the present invention was manufactured is shown.
- the synthesis was carried out using thioacetamide as the ion source and dodecanethiol as the solvent and complexing agent.
- Yowi copper and indium iodide were all dissolved in dodecanethiol and thioacetamide was added, followed by heating at a temperature of 100 ° C for 22 hours to obtain a product.
- Figure 15 shows the fluorescence vector of the product obtained. Fluorescence with a fluorescence wavelength of about 700 nm was obtained from the photoexcited light at 460 nm.
- the present invention is preferably used in the following fields.
- the phosphor of the present invention can be used as a phosphor including semiconductor nanoparticles capable of modifying or staining a biological substance.
- the nanoparticle phosphor of the present invention exhibits various fluorescence of 450 nm to 800 nm by monochromatic excitation, and the stability of the nanoparticle is high. For this reason, in addition to its use as a fluorescent reagent for biomolecule analysis, which is commonly used in biochemical research and diagnosis, a fluorescent tag for observing the dynamics of biomolecules A wide range of uses such as fluorescent tags for simultaneous analysis of multiple molecules can be expected.
- this nano-particle phosphor is composed of a low-toxic element, and the visible light power of 450 to 800 nm can be freely controlled in the near-infrared range, so that the EL display or plasma can be controlled. It can be used as a very wide range of optical materials such as phosphors used in displays and field emission displays, phosphors for light emitting diodes, and phosphors for lasers. It can also be used as a semiconductor light source for illumination. Brief Description of Drawings
- FIG. 1 shows a fluorescence intensity graph of the phosphor of Example 1.
- FIG. 2 is a graph illustrating the results of producing phosphors at a plurality of synthesis temperatures.
- FIG. 3 shows the spectrum of light waves emitted from a phosphor at a plurality of excitation wavelengths.
- FIG. 4 shows a graph of fluorescence intensity when the composition ratio (preparation ratio) of raw materials is changed.
- FIG. 5 shows the absorbance graph of the phosphor of each graph of FIG.
- FIG. 6 shows an emission spectrum according to the molar ratio of atoms constituting the phosphor of FIG.
- FIG. 7 is an XRD diffraction result of the product in Example 1.
- FIG. 8 shows a fluorescence intensity graph of the phosphor of Example 2.
- FIG. 9 shows an absorbance graph of the phosphor of FIG.
- FIG. 10 shows a fluorescence intensity graph of the phosphor of Example 3.
- FIG. 11 illustrates an absorbance graph of the phosphor of FIG.
- FIG. 12 shows a fluorescence intensity graph of the phosphor of Example 4.
- FIG. 13 is a graph showing the maximum value of absorption wavelength and the maximum value of fluorescence wavelength in Example 5.
- FIG. 14 is a diagram illustrating measurement results of fluorescence intensity of product ZnS composite structure particles in Example 6.
- FIG. 15 is a diagram illustrating the measurement results of the fluorescence intensity of the product in Example 7.
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JP2006529200A JP5136877B2 (ja) | 2004-07-16 | 2005-07-15 | 蛍光体、及びその製造方法 |
US11/632,288 US20080277625A1 (en) | 2004-07-16 | 2005-07-15 | Phosphor And Production Process Of Same |
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JP2004210548 | 2004-07-16 | ||
JP2004-210548 | 2004-07-16 |
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WO2007060889A1 (ja) * | 2005-11-24 | 2007-05-31 | National Institute Of Advanced Industrial Science And Technology | 蛍光体、及びその製造方法 |
JP2007146008A (ja) * | 2005-11-28 | 2007-06-14 | Kyocera Corp | 蛍光体及び波長変換器並びに発光装置 |
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