WO2021124934A1 - 半導体ナノ粒子集合体、半導体ナノ粒子集合体分散液、半導体ナノ粒子集合体組成物及び半導体ナノ粒子集合体硬化膜 - Google Patents
半導体ナノ粒子集合体、半導体ナノ粒子集合体分散液、半導体ナノ粒子集合体組成物及び半導体ナノ粒子集合体硬化膜 Download PDFInfo
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- WO2021124934A1 WO2021124934A1 PCT/JP2020/045282 JP2020045282W WO2021124934A1 WO 2021124934 A1 WO2021124934 A1 WO 2021124934A1 JP 2020045282 W JP2020045282 W JP 2020045282W WO 2021124934 A1 WO2021124934 A1 WO 2021124934A1
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- semiconductor nanoparticle
- nanoparticle aggregate
- semiconductor
- semiconductor nanoparticles
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
- H01L33/504—Elements with two or more wavelength conversion materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/507—Wavelength conversion elements the elements being in intimate contact with parts other than the semiconductor body or integrated with parts other than the semiconductor body
Definitions
- the present invention relates to an aggregate of semiconductor nanoparticles, a semiconductor nanoparticle aggregate dispersion liquid using the same, a semiconductor nanoparticle aggregate composition, and a semiconductor nanoparticle aggregate cured film.
- Semiconductor nanoparticles (quantum dots: QD) with a fine particle size are used as the wavelength conversion material for displays.
- Such semiconductor nanoparticles are minute particles capable of exhibiting a quantum confinement effect, and the width of the band gap changes depending on the size of the nanoparticles.
- excitons formed in the semiconductor particles by means such as photoexcitation and charge injection emit photons of energy according to the band gap by recombination. Therefore, by adjusting the crystal size of the semiconductor nanoparticles, light emission is performed. The wavelength can be controlled, and light emission of a desired wavelength can be obtained.
- a QD device using semiconductor nanoparticles is a QD film obtained by forming an aggregate of semiconductor nanoparticles into a film, which whitens blue light and converts the obtained white light into red, green, and blue through a color filter.
- QD film method and a method (QD color filter method) in which blue light is directly converted into red and green by a QD color filter using an aggregate of semiconductor nanoparticles.
- the blue light from the blue LED 1 which is the light source is not converted into white light, but is directly converted from blue light to red light or from blue light to green light by using the QD pattern (7, 8). ..
- the QD pattern (7, 8) is formed by patterning an aggregate of semiconductor nanoparticles dispersed in a resin, and the thickness is about 5 to 10 ⁇ m due to the structural limitation of the display.
- blue blue light from the blue LED 1 which is a light source is transmitted through a diffusion layer 9 containing a diffusing material.
- Reference numeral 3 is a liquid crystal, and the polarizing plate is omitted in FIG.
- a blue LED 101 is used as a light source, and first, the blue light is converted into white light.
- a QD film 102 formed by dispersing an aggregate of semiconductor nanoparticles in a resin to form a film having a thickness of about 100 ⁇ m is preferably used.
- the white light obtained by the wavelength conversion layer such as the QD film 102 is further subjected to the red light and the green light by the color filter (R) 104, the color filter (G) 105, and the color filter (B) 106, respectively. And converted to blue light.
- Reference numeral 103 is a liquid crystal, and the polarizing plate is omitted in FIG.
- the QD color filter method directly converts blue light into each color, so the wavelength conversion efficiency of the entire QD device is high. Therefore, in recent years, the QD color filter method has attracted attention.
- semiconductor nanoparticles are inherently required to have high quantum efficiency in order to increase the wavelength conversion efficiency of QD devices, and to have a narrow half-value width in order to prevent color mixing. ..
- Cd chalcogenide semiconductor nanoparticles and InP-based semiconductor nanoparticles are known (for example, Patent Documents 1 to 3).
- Patent Documents 1 to 3 In the past, much research has been conducted on Cd-based semiconductor nanoparticles. This is because the Cd-based semiconductor nanoparticles have high quantum efficiency and the emission wavelength changes relatively slowly due to the change in particle size, so that the emission wavelength can be easily adjusted.
- non-Cd-based semiconductor nanoparticles include InP-based semiconductor nanoparticles.
- InP-based semiconductor nanoparticles based on InP have lower quantum efficiency than Cd-based semiconductor nanoparticles, and the change in emission wavelength due to a change in particle size is large, so that the emission wavelength is adjusted. There is a problem that it is difficult.
- Patent Document 4 discloses semiconductor nanoparticles having a core-shell structure (hereinafter, also referred to as InP / ZnSe / ZnS core / shell structure) formed of a core made of InP and a shell made of ZnSe and ZnS. Attempts have been made to increase the absorbance.
- Patent Document 5 discloses semiconductor nanoparticles in which a halogen is contained in an InP / ZnSe / ZnS core / shell structure, and an attempt is made to improve quantum efficiency.
- Patent Document 6 discloses semiconductor nanoparticles having a core-shell structure (hereinafter, also referred to as InP / ZnSe / ZnS core / shell structure) formed of a core made of InP and a shell made of ZnSe and ZnS. Attempts have been made to improve quantum efficiency and narrow the half-price range.
- a core-shell structure hereinafter, also referred to as InP / ZnSe / ZnS core / shell structure
- an object of the present invention is an aggregate of core / shell type semiconductor nanoparticles composed of a core containing In and P and one or more layers of shells, and the semiconductor nanoparticles can achieve both high quantum efficiency and a narrow half-price width. Is to provide a collection of.
- semiconductor nanoparticles having a core / shell type structure composed of a core containing In and P and a shell having one or more layers.
- the quantum efficiency of the particles is obtained by exciting the semiconductor nanoparticles constituting the semiconductor nanoparticle aggregate with excitation light of 445 nm, in addition to the full width at half maximum of the emission spectrum ( ⁇ 1) of the entire aggregate of semiconductor nanoparticles.
- the present invention (1) is a semiconductor nanoparticle aggregate which is an aggregate of core / shell type semiconductor nanoparticles having a core containing In and P and one or more layers of shells.
- the peak wavelength ( ⁇ 1 MAX ) of the emission spectrum ( ⁇ 1 ) when the semiconductor nanoparticle aggregate is dispersed in a dispersion medium and excited with excitation light of 450 nm is between 605 and 655 nm.
- the full width at half maximum (FWHM 1 ) of the emission spectrum ( ⁇ 1) is 43 nm or less.
- the emission spectrum ( ⁇ 2 ) for each particle obtained by exciting the semiconductor nanoparticles constituting the semiconductor nanoparticles aggregate with excitation light of 445 nm has the following requirements (1) to (3): (1) The average value of the full width at half maximum (FWHM 2 ) of the emission spectrum ( ⁇ 2 ) is 28 nm or less. (2) The standard deviation (SD 1 ) of the peak wavelength ( ⁇ 2 MAX ) of the emission spectrum ( ⁇ 2 ) is 10 nm or more and 30 nm or less. (3) the standard deviation of the half-value width of the emission spectrum ( ⁇ 2) (FWHM 2) (SD 2) is 12nm or less, It is intended to provide a semiconductor nanoparticle aggregate characterized by satisfying all of the above.
- the present invention (2) provides the semiconductor nanoparticle aggregate of (1), which is characterized in that the full width at half maximum (FWHM 1) is 38 nm or less.
- the present invention (3) provides an aggregate of semiconductor nanoparticles according to (1) or (2) , wherein the average value of the full width at half maximum (FWHM 2) is 25 nm or less.
- the present invention (4) provides an aggregate of semiconductor nanoparticles according to any one of (1) to (3) , wherein the standard deviation (SD 2) is 7 nm or less.
- the half width (FWHM 1 ) is 35 nm or less
- the average value of the half width (FWHM 2 ) is 24 nm or less
- the standard deviation (SD 2 ) is 6 nm or less.
- the present invention provides an aggregate of semiconductor nanoparticles according to any one of (1) to (4).
- the present invention (6) provides the semiconductor nanoparticle aggregate according to any one of (1) to (5), wherein the quantum efficiency (QY) of the semiconductor nanoparticle aggregate is 80% or more. To do.
- the present invention (7) provides the semiconductor nanoparticle aggregate of (6), which is characterized in that the quantum efficiency (QY) of the semiconductor nanoparticle aggregate is 85% or more.
- the present invention (8) provides the semiconductor nanoparticle aggregate of (7), which is characterized in that the quantum efficiency (QY) of the semiconductor nanoparticle aggregate is 90% or more.
- the semiconductor nanoparticles contain at least In, P, Zn, Se and halogen.
- the molar ratios of P, Zn, Se and halogen to In in terms of atoms are P: 0.20 to 0.95, Zn: 11.00 to 50.00, Se: 7.00. ⁇ 25.00, halogen: 0.80 ⁇ 15.00,
- the present invention provides an aggregate of semiconductor nanoparticles according to any one of (1) to (8).
- the present invention (10) provides a semiconductor nanoparticle aggregate dispersion liquid in which any of the semiconductor nanoparticle aggregates (1) to (9) is dispersed in an organic dispersion medium.
- the present invention (11) provides a semiconductor nanoparticle aggregate composition in which the semiconductor nanoparticle aggregate according to any one of (1) to (9) is dispersed in a monomer or a prepolymer.
- the present invention (12) provides a semiconductor nanoparticle aggregate cured film in which any of the semiconductor nanoparticle aggregates (1) to (9) is dispersed in a polymer matrix.
- the present invention is an aggregate of core / shell type semiconductor nanoparticles composed of a core containing In and P and a shell having one or more layers, and has both high quantum efficiency and a narrow half-price width, and has excellent characteristics.
- a semiconductor nanoparticle aggregate can be provided.
- the semiconductor nanoparticle aggregate of the present invention is a semiconductor nanoparticle aggregate which is an aggregate of core / shell type semiconductor nanoparticles having a core containing In and P and a shell having one or more layers.
- the peak wavelength ( ⁇ 1 MAX ) of the emission spectrum ( ⁇ 1 ) when the semiconductor nanoparticle aggregate is dispersed in a dispersion medium and excited with excitation light of 450 nm is between 605 and 655 nm.
- the full width at half maximum (FWHM 1 ) of the emission spectrum ( ⁇ 1) is 43 nm or less.
- the emission spectrum ( ⁇ 2 ) for each particle obtained by exciting the semiconductor nanoparticles constituting the semiconductor nanoparticles aggregate with excitation light of 445 nm has the following requirements (1) to (3): (1) The average value of the full width at half maximum (FWHM 2 ) of the emission spectrum ( ⁇ 2 ) is 28 nm or less. (2) The standard deviation (SD 1 ) of the peak wavelength ( ⁇ 2 MAX ) of the emission spectrum ( ⁇ 2 ) is 10 nm or more and 30 nm or less. (3) the standard deviation of the half-value width of the emission spectrum ( ⁇ 2) (FWHM 2) (SD 2) is 12nm or less, It is a semiconductor nanoparticle aggregate characterized by satisfying all of the above.
- the symbol "-" indicating the numerical range indicates a range including the numerical values described before and after the symbol "-” unless otherwise specified. That is, ⁇ to ⁇ represent ⁇ or more and ⁇ or less.
- the semiconductor nanoparticles constituting the semiconductor nanoparticles aggregate of the present invention are core / shell type semiconductor nanoparticles having a core containing In and P and a shell having one or more layers.
- the shell may have at least one layer, and the semiconductor nanoparticles include, for example, a core / shell type semiconductor nanoparticles consisting of a core and a one-layer shell, and a core / shell composed of a core and a two-layer shell. Examples thereof include type semiconductor nanoparticles and core / shell type semiconductor nanoparticles composed of a core and a shell having three or more layers.
- the fluorescence quantum efficiency of the semiconductor nanoparticles can be maintained, and it is possible to have a high fluorescence quantum efficiency as a semiconductor nanoparticle aggregate.
- the structure of the semiconductor nanoparticles may be such that the shell covers at least a part of the surface of the core, but a structure in which the shell covers the entire surface of the core is preferable, and the shell uniformly covers the entire surface of the core. A covering structure is particularly preferred.
- the shell preferably contains a shell having a composition containing Zn and Se, and it is preferable that at least one of the shells is formed of ZnSe.
- the outermost layer is preferably a shell having a composition containing Zn and S, and more preferably ZnS.
- the shell when the shell is formed of at least ZnSe and comprises a first shell that covers the outer surface of the core particles and a second shell that is formed of ZnS and covers the outer surface of the first shell, it is fluorescent. Quantum efficiency can be increased.
- the composition in the shell does not necessarily have to be a stoichiometric composition, and each shell may contain elements other than Zn, Se, and S, and the shell is composed in the shell. It may have one or more gradient-type shells in which the ratio of elements to be produced changes.
- whether or not the shell covers at least a part of the core and the element distribution inside the shell are determined by, for example, energy dispersive X-ray spectroscopy (TEM-EDX) using a transmission electron microscope. It can be confirmed by analyzing the composition using.
- TEM-EDX energy dispersive X-ray spectroscopy
- the semiconductor nanoparticles constituting the semiconductor nanoparticles aggregate of the present invention can contain halogen.
- the molar ratio of halogen to In in the semiconductor nanoparticles is preferably 0.80 to 15.00, particularly preferably 1.00 to 15.00 in terms of atoms.
- the halogen contained in the semiconductor nanoparticles is preferably F, Cl, Br.
- the semiconductor nanoparticles contain halogen in the above range, high fluorescence quantum efficiency and a narrow full width at half maximum can be obtained.
- the halogen is present at the interface between the core and the shell of the semiconductor nanoparticles and / or in the shell of the semiconductor nanoparticles, so that the above-mentioned effects can be further obtained.
- the elements constituting the semiconductor nanoparticles can be analyzed by using a high frequency inductively coupled plasma emission spectrometer (ICP) or a fluorescent X-ray analyzer (XRF).
- ICP inductively coupled plasma emission spectrometer
- XRF fluorescent X-ray analyzer
- the semiconductor nanoparticles constituting the semiconductor nanoparticles aggregate of the present invention contain at least In, P, Zn, Se and halogen, and the molar ratios of P, Zn, Se and halogen to In in terms of atoms are P: 0.20 to 0.95, Zn: 11.00 to 50.00, Se: 7.00 to 25.00, halogen: 0.80 to 15.00, preferably 1.00 to 15.00.
- P 0.20 to 0.95
- Zn 11.00 to 50.00
- Se 7.00 to 25.00
- halogen 0.80 to 15.00
- the Cd content of the semiconductor nanoparticles constituting the semiconductor nanoparticles aggregate of the present invention is 100 mass ppm or less, preferably 80 mass ppm or less, and particularly preferably 50 mass ppm or less.
- a core of semiconductor nanoparticles can be formed by heating a precursor mixture obtained by mixing a precursor of In, a precursor of P, and, if necessary, an additive in a solvent.
- a solvent a coordinating solvent or a non-coordinating solvent is used.
- solvents include 1-octadecene, hexadecane, squalene, oleylamine, trioctylphosphine, trioctylphosphine oxide and the like.
- the precursor of In include, but are not limited to, the acetate containing In, a carboxylate, and a halide.
- the precursor of P include, but are not limited to, the organic compounds and gases containing P. When the precursor is a gas, the core can be formed by reacting while injecting the gas into the precursor mixture containing other than the gas.
- the semiconductor nanoparticles may contain one or more elements other than In and P as long as the effects of the present invention are not impaired.
- a precursor of the elements may be added at the time of core formation.
- the additive include, but are not limited to, carboxylic acids, amines, thiols, phosphines, phosphine oxides, phosphinic acids, and phosphonic acids as dispersants.
- the dispersant can also serve as a solvent.
- the emission characteristics of the semiconductor nanoparticles can be improved by adding a halide as needed.
- the In precursor and, if necessary, a precursor solution in which a dispersant is added to a solvent are mixed under vacuum, once heated at 100 ° C. to 300 ° C. for 6 to 24 hours, and then further P.
- the precursor is added and heated at 200 ° C. to 400 ° C. for 3 to 60 minutes, and then cooled.
- a halogen precursor and heat-treating at 25 ° C. to 300 ° C., preferably 100 ° C. to 300 ° C., more preferably 150 ° C. to 280 ° C., a core particle dispersion liquid containing core particles can be obtained. ..
- the semiconductor nanoparticles By adding the shell-forming precursor to the synthesized core particle dispersion, the semiconductor nanoparticles have a core / shell structure, and the fluorescence quantum efficiency (QY) and stability can be improved.
- the elements that make up the shell are thought to have a structure such as an alloy, heterostructure, or amorphous structure on the surface of the core particles, but it is also possible that some of them have moved to the inside of the core particles due to diffusion.
- the added shell-forming element mainly exists near the surface of the core particles and has a role of protecting the semiconductor nanoparticles from external factors.
- the shell preferably covers at least a part of the core, and more preferably uniformly covers the entire surface of the core particles.
- the Zn precursor and the Se precursor are added to the core particle dispersion described above, heated at 150 ° C. to 300 ° C., preferably 180 ° C. to 250 ° C., and then the Zn precursor and the S precursor are added. Then, it is heated at 200 ° C. to 400 ° C., preferably 250 ° C. to 350 ° C. As a result, core / shell type semiconductor nanoparticles can be obtained.
- the Zn precursor includes carboxylates such as zinc acetate, zinc propionate and zinc myristate, halides such as zinc chloride and zinc bromide, and organics such as diethyl zinc. Salt or the like can be used.
- phosphine serenides such as tributylphosphine serenide, trioctylphosphine serenide and tris (trimethylsilyl) phosphine serenide, selenols such as benzenelenol and selenocysteine, and selenium / octadecene solution are used. can do.
- phosphine sulfides such as tributylphosphine sulfide, trioctylphosphine sulfide and tris (trimethylsilyl) phosphine sulfide, thiols such as octanethiol, dodecanethiol and octadecanethiol, and sulfur / octadecene solutions should be used. Can be done.
- the shell precursor may be mixed in advance and added once or in multiple times, or each may be added separately in one time or in multiple times.
- the temperature may be changed and heated after each shell precursor is added.
- the method for producing semiconductor nanoparticles is not particularly limited, and in addition to the methods shown above, conventional methods such as a hot injection method, a uniform solvent method, a reverse micelle method, and a CVD method can be used. Any method may be adopted.
- 1 MAX is between 605 and 655 nm.
- red emission having a wavelength of 595 to 665 nm can be achieved by excitation with blue light of 430 to 500 nm.
- the full width at half maximum (FWHM) of the emission spectrum ( ⁇ 1 ) when the semiconductor nanoparticle aggregate of the present invention is excited with excitation light of 450 nm in a state of being dispersed in a dispersion medium. 1 ) is 43 nm or less, preferably 38 nm or less, and particularly preferably 35 nm or less.
- the full width at half maximum (FWHM 1 ) of the emission spectrum ( ⁇ 1 ) is within the above range, high-purity emission can be obtained.
- the emission spectrum ( ⁇ 2 ) for each particle obtained by exciting the semiconductor nanoparticles constituting the semiconductor nanoparticles aggregate of the present invention with excitation light of 445 nm is as follows. Satisfy all of requirements (1) to (3).
- the average value of the full width at half maximum (FWHM 2 ) of the emission spectrum ( ⁇ 2 ) is 28 nm or less, preferably 25 nm or less, and particularly preferably 24 nm or less.
- the "average value of the half-value width (FWHM 2 ) of the emission spectrum ( ⁇ 2 )" is defined as each particle obtained by exciting the semiconductor nanoparticles constituting the semiconductor nanoparticle aggregate with excitation light of 445 nm.
- the half-value width (FWHM 2 ) of the emission spectrum ( ⁇ 2 ) was measured 5 times for each particle for 40 semiconductor nanoparticles, and a total of 200 measured values obtained were averaged. Refers to the value to be.
- the standard deviation (SD 1 ) of the peak wavelength ( ⁇ 2 MAX ) of the emission spectrum ( ⁇ 2 ) is 10 nm or more and 30 nm or less, preferably 10 nm or more and 25 nm or less.
- the "standard deviation (SD 1 ) of the peak wavelength ( ⁇ 2 MAX ) of the emission spectrum ( ⁇ 2 )" is obtained by exciting the semiconductor nanoparticles constituting the semiconductor nanoparticle aggregate with excitation light of 445 nm.
- the peak wavelength ( ⁇ 2 MAX ) of the emission spectrum ( ⁇ 2 ) for each particle was measured 5 times for each particle for 40 semiconductor nanoparticles, and a total of 200 measurements were obtained. Refers to the standard deviation value calculated from the value.
- the standard deviation (SD 2 ) of the full width at half maximum (FWHM 2 ) of the emission spectrum ( ⁇ 2 ) is 12 nm or less, preferably 7 nm or less, and particularly preferably 6 nm or less.
- the "standard deviation of the half-value width of the emission spectrum ( ⁇ 2) (FWHM 2) (SD 2) " is obtained by the semiconductor nanoparticles of the semiconductor nanoparticle aggregates, being excited by the excitation light 445nm
- the half-value width (FWHM 2 ) of the emission spectrum ( ⁇ 2 ) for each particle was measured 5 times for each particle for 40 semiconductor nanoparticles, and from a total of 200 measured values obtained. Refers to the calculated standard deviation value.
- the present inventors have conducted a semiconductor nanoparticle aggregate having a peak wavelength ( ⁇ 1 MAX ) of an emission spectrum ( ⁇ 1) between 605 and 655 nm with excitation light of 450 nm.
- the individual semiconductor nanoparticles are produced under as uniform and homogeneous manufacturing conditions as possible in order to control the average value of the full width at half maximum (FWHM 2 ) and the standard deviation (SD 2).
- the temperature rise rate should be 5 ° C. or higher per minute.
- the rate of temperature rise is preferably 10 ° C. or higher per minute.
- the manufacturing apparatus In manufacturing the semiconductor nanoparticle aggregate of the present invention, there is no particular upper limit to the heating rate, but if the manufacturing apparatus becomes complicated in order to increase the heating rate, the manufacturing cost will increase, so that it is industrial / commercial. From the viewpoint, it is realistic to use 3000 ° C. or less per minute.
- the semiconductor nanoparticle aggregate of the present invention the average value of the full width at half maximum (FWHM 2 ) of the requirement (1) emission spectrum ( ⁇ 2 ) is 28 nm or less, and the peak wavelength of the requirement (2) emission spectrum ( ⁇ 2). (lambda 2 MAX) standard deviation (SD 1) is at 10nm or more 30nm or less, and the requirement (3) the standard deviation of the half-value width of the emission spectrum ( ⁇ 2) (FWHM 2) (SD 2) is 12nm or less Therefore, the semiconductor nanoparticle aggregate of the present invention can achieve both high quantum efficiency (QY) and high full width at half maximum (FWHM 1).
- the semiconductor nanoparticle aggregate of the present invention has a half width (FWHM 1 ) of 35 nm or less, an average half width (FWHM 2 ) of 24 nm or less, and a standard deviation (SD 2 ) of 6 nm or less. Some are preferable because they can obtain a particularly narrow full width at half maximum (FWHM 1).
- the quantum efficiency (QY) of the semiconductor nanoparticle aggregate of the present invention is preferably 80% or more, more preferably 85% or more, and particularly preferably 90% or more.
- elemental analysis can be performed using a high frequency inductively coupled plasma emission spectrometer (ICP) or a fluorescent X-ray analyzer (XRF).
- ICP inductively coupled plasma emission spectrometer
- XRF fluorescent X-ray analyzer
- ICP measurement purified semiconductor nanoparticles are dissolved in nitric acid, heated, diluted with water, and measured by a calibration curve method using an ICP emission spectrometer (ICPS-8100, manufactured by Shimadzu Corporation).
- ICPS-8100 ICP emission spectrometer
- XRF fluorescent X-ray analyzer
- ZSX100e fluorescent X-ray analyzer
- the fluorescence quantum efficiency measurement system (manufactured by Otsuka Electronics, QE) -2000), can be measured using a visible ultraviolet spectrophotometer (manufactured by JASCO Corporation, V670).
- An emission spectrum is obtained by irradiating a dispersion liquid in which semiconductor nanoparticles are dispersed in a dispersion medium with excitation light of 450 nm.
- the peak wavelength ( ⁇ 1 MAX ) was obtained from the re-excitation corrected emission spectrum ( ⁇ 1 ) excluding the re-excitation fluorescence emission spectrum of the portion that was re-excited and fluorescently emitted from the emission spectrum obtained here, and the fluorescence quantum was obtained.
- the dispersion medium include normal hexane, octadecene, toluene, acetone, and PGMEA.
- the excitation light used for the measurement is a single light of 450 nm, and the dispersion liquid is one in which the concentration of semiconductor nanoparticles is adjusted so that the absorption rate is 20 to 30%.
- the absorption spectrum can be measured by irradiating a dispersion liquid in which semiconductor nanoparticles are dispersed in a dispersion medium with ultraviolet to visible light.
- the peak wavelength ( ⁇ 2 MAX ) and half-value width (FWHM ) of the emission spectrum ( ⁇ 2 ) of each particle obtained by exciting individual semiconductor nanoparticles constituting the semiconductor nanoparticle aggregate with excitation light of 445 nm.
- 2 for example, “Kameyama et al., ACS Appl. Meter, Interfaces 2018, 10, 42844-42855", “Ematsu et al., NPG Asia Materials (2016) 10,713-726", ". It can be carried out by a known method described in "Sharma et al., ACS Nano 2019, 13, 624-632” and the like.
- the procedure for measuring the peak wavelength ( ⁇ 2 MAX ) and the full width at half maximum (FWHM 2 ) of the emission spectrum ( ⁇ 2 ) for each particle is described in Examples described later.
- SD 2 was calculated from the peak wavelength ( ⁇ 2 MAX ) and full width at half maximum (FWHM 2 ) of the emission spectrum ( ⁇ 2) for each particle obtained as described above.
- the wavelength ( ⁇ 2 MAX ) and the full width at half maximum (FWHM 2 ) all measurements were taken up to the 3rd digit of the decimal point and rounded to the 2nd digit of the decimal point. Further, from the measured values thus obtained, the average value of the half width (FWHM 2 ) of the emission spectrum ( ⁇ 2 ) for each particle, the standard deviation (SD 1 ) of the peak wavelength ( ⁇ 2 MAX ), and the half width (SD 1).
- the peak wavelength ( ⁇ 2 MAX ) and the full width at half maximum (FWHM 2 ) of the emission spectrum data ( ⁇ 2 ) measured for each particle in Experimental Example 3 (Example) and Experimental Example 8 (Comparative Example) described later. ) (200 pieces in each example) are shown as FIG.
- the distribution tendency of the peak wavelength ( ⁇ 2 MAX ) and the full width at half maximum (FWHM 2 ) is clearly different between the experimental example belonging to the embodiment of the present invention and the experimental example belonging to the comparative example. , Such a distribution tendency was also observed in other examples and comparative examples.
- the semiconductor nanoparticle aggregate of the present invention can be dispersed in a polar dispersion medium to form a semiconductor nanoparticle aggregate dispersion liquid.
- the state in which the semiconductor nanoparticle aggregate is dispersed in the dispersion medium is a state in which the semiconductor nanoparticle composite does not precipitate when the semiconductor nanoparticle aggregate and the dispersion medium are mixed, or is visible. Indicates that the state does not remain as turbidity (cloudiness).
- a semiconductor nanoparticle aggregate dispersed in a dispersion medium is referred to as a semiconductor nanoparticle aggregate dispersion liquid.
- alcohols such as methanol, ethanol, isopropyl alcohol and normal propyl alcohol, acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclopentanone, cyclohexanone and the like are used.
- Estels such as ketones, methyl acetate, ethyl acetate, isopropyl acetate, normal propyl acetate, normal butyl acetate, ethyl lactate, ethers such as diethyl ether, dipropyl ether, dibutyl ether, tetrahydrofuran, ethylene glycol monomethyl ether, ethylene glycol Monoethyl ether, diethylene glycol monomethyl ether, ethylene glycol diethyl ether, diethylene glycol dimethyl ether, propylene glycol monomethyl ether (PGME), propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monobutyl ether, propylene glycol dimethyl ether, dipropylene glycol dimethyl ether, Glycol ethers such as propylene glycol diethyl ether and dipropylene glycol diethyl ether, ethylene glycol acetate,
- a monomer can be selected as the dispersion medium of the semiconductor nanoparticle aggregate dispersion liquid of the present invention.
- the monomer is not particularly limited, but is preferably a (meth) acrylic monomer from which a wide range of applications of semiconductor nanoparticles can be selected.
- the (meth) acrylic monomer is methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, isobutyl (meth) acrylate, isoamyl, depending on the application of the semiconductor nanoparticle aggregate dispersion liquid.
- the acrylic monomer may be one or a mixture of two or more selected from lauryl (meth) acrylate and 1,6-hexadioldi (meth) acrylate depending on the application of the semiconductor nanoparticle aggregate dispersion liquid. preferable.
- a prepolymer can be selected as the dispersion medium of the semiconductor nanoparticle aggregate dispersion liquid of the present invention.
- the prepolymer is not particularly limited, and examples thereof include an acrylic resin prepolymer, a silicone resin prepolymer, and an epoxy resin prepolymer.
- the semiconductor nanoparticle aggregate composition of the present invention is a semiconductor nanoparticle aggregate composition in which the semiconductor nanoparticle aggregate of the present invention is dispersed in a monomer or a prepolymer.
- the monomer or prepolymer is not particularly limited, and examples thereof include a radically polymerizable compound containing an ethylenically unsaturated bond, a siloxane compound, an epoxy compound, an isocyanate compound, and a phenol derivative.
- the monomer include the monomers used as the above-mentioned dispersion medium.
- the prepolymer used as the above-mentioned dispersion medium can be mentioned.
- the semiconductor nanoparticle aggregate composition of the present invention can contain a cross-linking agent.
- the cross-linking agent may be a polyfunctional (meth) acrylate, a polyfunctional silane compound, a polyfunctional amine, a polyfunctional carboxylic acid, a polyfunctional thiol, a polyfunctional alcohol, depending on the type of monomer in the semiconductor nanoparticle aggregate composition of the present invention.
- polyfunctional isocyanates and the like may be a polyfunctional (meth) acrylate, a polyfunctional silane compound, a polyfunctional amine, a polyfunctional carboxylic acid, a polyfunctional thiol, a polyfunctional alcohol, depending on the type of monomer in the semiconductor nanoparticle aggregate composition of the present invention.
- polyfunctional isocyanates and the like are examples of the like.
- the semiconductor nanoparticle aggregate composition of the present invention comprises aliphatic hydrocarbons such as pentane, hexane, cyclohexane, isohexane, heptane, octane and petroleum ether, alcohols, ketones, esters, glycol ethers, etc. It can further contain various organic solvents that do not affect curing, such as glycol ether esters, aromatic hydrocarbons such as benzene, toluene, xylene and mineral spirits, and alkyl halides such as dichloromethane and chloroform.
- the above-mentioned organic solvent can be used not only for diluting the semiconductor nanoparticle aggregate composition but also as an organic dispersion medium. That is, it is also possible to disperse the semiconductor nanoparticle aggregate of the present invention in the above-mentioned organic solvent to obtain a semiconductor nanoparticle aggregate dispersion liquid.
- the semiconductor nanoparticle aggregate composition of the present invention is suitable as an initiator, a scattering agent, a catalyst, a binder, a surfactant, an adhesion accelerator, and an antioxidant depending on the type of the monomer in the semiconductor nanoparticle aggregate composition.
- Agents, UV absorbers, anti-aggregation agents, dispersants and the like may be included.
- the semiconductor nanoparticle aggregate composition may contain a scattering agent. ..
- the scattering agent is a metal oxide such as titanium oxide or zinc oxide, and the particle size of these is preferably 100 nm to 500 nm. From the viewpoint of the effect of scattering, the particle size of the scattering agent is more preferably 200 nm to 400 nm. By including the scattering agent, the absorbance is improved by about twice.
- the content of the scattering agent in the semiconductor nanoparticle aggregate composition of the present invention is preferably 2% by mass to 30% by mass with respect to the composition, and from the viewpoint of maintaining the patternability of the composition, 5% by mass to More preferably, it is 20% by mass.
- the absorbance of the film with respect to light having a wavelength of 450 nm from the normal direction is preferably 1.0 or more, preferably 1.3 or more. More preferably, it is more preferably 1.5 or more.
- the light from the backlight can be efficiently absorbed, so that the thickness of the cured film described later can be reduced, and the device to be applied can be miniaturized.
- the diluted composition is obtained by diluting the above-mentioned semiconductor nanoparticle aggregate composition of the present invention with an organic solvent.
- the organic solvent for diluting the semiconductor nanoparticle aggregate composition is not particularly limited, and for example, aliphatic hydrocarbons such as pentane, hexane, cyclohexane, isohexane, heptane, octane and petroleum ether, alcohols and ketones.
- aliphatic hydrocarbons such as pentane, hexane, cyclohexane, isohexane, heptane, octane and petroleum ether, alcohols and ketones.
- Classes, esters, glycol ethers, glycol ether esters, aromatic hydrocarbons such as benzene, toluene, xylene and mineral spirit, and alkyl halides such as dichloromethane and chloroform are preferable from the viewpoint of solubility in a wide range of resins and film uniformity at the time of coating film.
- the semiconductor nanoparticle aggregate cured film of the present invention is a film containing the semiconductor nanoparticle aggregate of the present invention and represents a cured film.
- the semiconductor nanoparticle aggregate cured film of the present invention can be obtained by curing the above-mentioned semiconductor nanoparticle aggregate composition or diluted composition into a film.
- the semiconductor nanoparticle aggregate cured film of the present invention contains the semiconductor nanoparticles according to the semiconductor nanoparticle aggregate of the present invention, a ligand coordinated on the surface of the semiconductor nanoparticles, and a polymer matrix.
- the semiconductor nanoparticle aggregate cured film of the present invention is a cured film in which the semiconductor nanoparticle aggregate of the present invention is dispersed in a polymer matrix.
- the polymer matrix is not particularly limited, and examples thereof include (meth) acrylic resin, silicone resin, epoxy resin, silicone resin, maleic acid resin, butyral resin, polyester resin, melamine resin, phenol resin, and polyurethane resin.
- the semiconductor nanoparticle aggregate cured film of the present invention may be obtained by curing the semiconductor nanoparticle aggregate composition of the present invention described above.
- the semiconductor nanoparticle aggregate cured film of the present invention may further contain a cross-linking agent.
- the method for curing the film is not particularly limited, but the film can be cured by a curing method suitable for the composition constituting the film, such as heat treatment and ultraviolet treatment.
- the absorbance is preferably 1.0 or more with respect to light having a wavelength of 450 nm from the normal direction of the semiconductor nanoparticle composite cured film. It is more preferably 3 or more, and further preferably 1.5 or more.
- the semiconductor nanoparticle aggregate cured film of the present invention contains a semiconductor nanoparticle aggregate having high light emitting characteristics, it is possible to provide a semiconductor nanoparticle aggregate cured film having high light emitting characteristics.
- the fluorescence quantum efficiency of the semiconductor nanoparticle composite assembly of the present invention is preferably 70% or more, more preferably 80% or more.
- the thickness of the semiconductor nanoparticle aggregate cured film of the present invention is preferably 50 ⁇ m or less, more preferably 20 ⁇ m or less, and more preferably 10 ⁇ m in order to reduce the size of the device to which the semiconductor nanoparticle aggregate cured film is applied. The following is more preferable.
- Semiconductor nanoparticles were prepared according to the following method, and the composition and optical characteristics of the obtained semiconductor nanoparticles were measured.
- composition Composition analysis was performed using a radio frequency inductively coupled plasma emission spectrometer (ICP) and a fluorescent X-ray analyzer (XRF). Table 1 shows the analysis results in terms of molar ratio to indium.
- ICP radio frequency inductively coupled plasma emission spectrometer
- XRF fluorescent X-ray analyzer
- the emission spectrum ( ⁇ 1 ) of the semiconductor nanoparticle aggregate is measured using the quantum efficiency measurement system, and the quantum efficiency (QY) of the semiconductor nanoparticle aggregate and the half-value width of the semiconductor nanoparticle aggregate (QY) are measured.
- FWHM 1 ) and peak wavelength ( ⁇ 1 MAX ) were measured.
- the excitation light was set to a single wavelength of 450 nm.
- the dispersion liquid used for the measurement a liquid whose concentration was adjusted so that the absorption rate was 20 to 30% was used.
- the dispersion of semiconductor nanoparticles was irradiated with visible light from the ultraviolet and the absorption spectrum was measured.
- the dispersion liquid used for measuring the absorption spectrum a dispersion medium whose concentration was adjusted so that the amount of semiconductor nanoparticles was 1 mg with respect to 1 mL was used. Table 2 shows the analysis results.
- TC-20-4450 manufactured by NeoArc Co., Ltd. which can emit a blue laser light having a wavelength of 445 nm, is used, and the laser light is introduced into a microscope and converged, and then will be described later. It was configured to irradiate the measurement sample. At this time, in order to prevent unnecessary excitation light and scattered light from entering the detector, an optical filter is appropriately installed at a necessary place.
- the semiconductor nanoparticles to be measured were dispersed on a quartz substrate by the method shown below to prepare a measurement sample.
- the semiconductor nanoparticles constituting the semiconductor nanoparticles aggregate to be measured are aggregated in a toluene solution obtained by dissolving about 2 to 3% by mass of polymethylmethacrylate (PMMA) in toluene for optical analysis.
- PMMA polymethylmethacrylate
- a synthetic quartz substrate (Labo-CG manufactured by Daiko Seisakusho Co., Ltd.) that does not emit light by excitation by blue laser light is attached to a spin coater, and an appropriate amount of a toluene solution in which the above semiconductor nanoparticles are dispersed is dropped on the spin coater, and the rotation speed is 1000 to 3000 rpm.
- a thin film in which semiconductor nanoparticles were dilutedly dispersed in the PMMA film was formed on a quartz substrate. This was placed on the objective lens of the microscope as a sample substrate for measurement. In the above preparations and operations, care must be taken not to mix impurities emitted by the excitation laser light.
- the wavelength is calculated by comparing with the spectral image of the reference light whose wavelength is known in advance, and the intensity is calculated from the overall intensity with the intensity of the particle-free portion as the background.
- the emission spectrum ( ⁇ 2 ) of each semiconductor nanoparticle is obtained by making corrections such as subtraction, obtaining the wavelength and intensity data points of the individual semiconductor nanoparticles, and then gauss-fitting them using appropriate graph software. , the peak wavelength (lambda 2 MAX) of the emission spectrum (lambda 2), and quantifies the half width (FWHM 2) of the emission spectrum (lambda 2).
- the above quantification was performed on a spectrum of 5 points randomly selected for each particle by randomly selecting 40 semiconductor nanoparticles from all the captured images. Based on the total of 200 measurement data obtained in this way, the average value of the full width at half maximum (FWHM 2 ), the standard deviation of the peak wavelength ( ⁇ 2 MAX ) (SD 1 ), and the standard deviation of the full width at half maximum (FWHM 2) (FWHM 2) SD 2 ) was obtained. The analysis results are also shown in Table 2.
- Tables 1 and 2 show the results of the same analysis as in Experimental Example 1 after producing semiconductor nanoparticles in the same manner as in Experimental Example 1 except that the composition ratio of the raw materials used in the production was changed.
- ⁇ 1 MAX is the peak wavelength of the emission spectrum ( ⁇ 1 )
- FWHM 1 is the half width of the emission spectrum ( ⁇ 1 )
- average of FWHM 2 is emission. It is the average value of the full width at half maximum (FWHM 2 ) of the spectrum ( ⁇ 2 )
- SD 1 of ⁇ 2 MAX is the standard deviation of the peak wavelength ( ⁇ 2 MAX ) of the emission spectrum ( ⁇ 2 )
- FWHM. 2 SD 2 is the standard deviation of the full width at half maximum (FWHM 2 ) of the emission spectrum ( ⁇ 2).
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Abstract
Description
半導体ナノ粒子が知られている(例えば、特許文献1~3)。そして、従来は、Cd系の半導体ナノ粒子の研究が多く行われていた。Cd系の半導体ナノ粒子は、量子効率が高い上に、粒径変化による発光波長の変化が比較的緩やかなので、発光波長の調整がし易いためである。
前記半導体ナノ粒子集合体を分散媒中に分散させた状態で450nmの励起光で励起させたときの発光スペクトル(λ1)のピーク波長(λ1 MAX)が605~655nmの間にあり、前記発光スペクトル(λ1)の半値幅(FWHM1)が43nm以下であり、
前記半導体ナノ粒子集合体を構成する半導体ナノ粒子を、445nmの励起光で励起させて得られる1粒子毎の発光スペクトル(λ2)が、以下の要件(1)~(3):
(1)発光スペクトル(λ2)の半値幅(FWHM2)の平均値が28nm以下であること、
(2)発光スペクトル(λ2)のピーク波長(λ2 MAX)の標準偏差(SD1)が10nm以上30nm以下であること、
(3)発光スペクトル(λ2)の半値幅(FWHM2)の標準偏差(SD2)が12nm以下であること、
の全てを満たすことを特徴とする半導体ナノ粒子集合体を提供するものである。
前記半導体ナノ粒子において、原子換算で、Inに対するP、Zn、Se及びハロゲンの各モル比が、P:0.20~0.95、Zn:11.00~50.00、Se:7.00~25.00、ハロゲン:0.80~15.00であること、
を特徴とする(1)~(8)の何れかの半導体ナノ粒子集合体を提供するものである。
前記半導体ナノ粒子集合体を分散媒中に分散させた状態で450nmの励起光で励起させたときの発光スペクトル(λ1)のピーク波長(λ1 MAX)が605~655nmの間にあり、前記発光スペクトル(λ1)の半値幅(FWHM1)が43nm以下であり、
前記半導体ナノ粒子集合体を構成する半導体ナノ粒子を、445nmの励起光で励起させて得られる1粒子毎の発光スペクトル(λ2)が、以下の要件(1)~(3):
(1)発光スペクトル(λ2)の半値幅(FWHM2)の平均値が28nm以下であること、
(2)発光スペクトル(λ2)のピーク波長(λ2 MAX)の標準偏差(SD1)が10nm以上30nm以下であること、
(3)発光スペクトル(λ2)の半値幅(FWHM2)の標準偏差(SD2)が12nm以下であること、
の全てを満たすことを特徴とする半導体ナノ粒子集合体である。
なお、以下において数値範囲を示す符号「~」は、特に断らない限り、符号「~」の前後に記載された数値を含む範囲を示す。つまり、〇~△とは、〇以上且つ△以下を表す。
本発明の半導体ナノ粒子集合体を構成する半導体ナノ粒子は、InおよびPを含有するコアと、1層以上のシェルとを有するコア/シェル型半導体ナノ粒子である。半導体ナノ粒子において、シェルは少なくとも1層あればよく、半導体ナノ粒子としては、例えば、コアと1層のシェルからなるコア/シェル型の半導体ナノ粒子、コアと2層のシェルからなるコア/シェル型の半導体ナノ粒子、コアと3層以上のシェルからなるコア/シェル型の半導体ナノ粒子が挙げられる。特にシェルが2層以上からなることにより、半導体ナノ粒子の蛍光量子効率を維持することができ、半導体ナノ粒子集合体として高い蛍光量子効率を有することが可能となる。また、半導体ナノ粒子の構造としては、シェルがコアの表面の少なくとも一部を覆っていればよいが、シェルがコアの表面全体を覆っている構造が好ましく、シェルがコアの表面全体を均一に覆っている構造が特に好ましい。
Inの前駆体、Pの前駆体、および必要に応じて添加物を溶媒中で混合し得られた前駆体混合液を加熱することで、半導体ナノ粒子のコアを形成することができる。溶媒としては配位性溶媒や非配位性溶媒が用いられる。
溶媒の例としては、1-オクタデセン、ヘキサデカン、スクアラン、オレイルアミン、トリオクチルホスフィン、およびトリオクチルホスフィンオキシドなどが挙げられる。
Inの前駆体としては、前記Inを含む酢酸塩、カルボン酸塩、およびハロゲン化物等が挙げられるが、これらに限定されるものではない。
Pの前駆体としては、前記Pを含む有機化合物やガスが挙げられるが、これらに限定されるものではない。前駆体がガスの場合には、前記ガス以外を含む前駆体混合液にガスを注入しながら反応させることでコアを形成させることができる。
Se前駆体としては、トリブチルホスフィンセレニド、トリオクチルホスフィンセレニドおよびトリス(トリメチルシリル)ホスフィンセレニドなどのホスフィンセレニド類、ベンゼンセレノールおよびセレノシステインなどのセレノール類、およびセレン/オクタデセン溶液などを使用することができる。
S前駆体としては、トリブチルホスフィンスルフィド、トリオクチルホスフィンスルフィドおよびトリス(トリメチルシリル)ホスフィンスルフィドなどのホスフィンスルフィド類、オクタンチオール、ドデカンチオールおよびオクタデカンチオールなどのチオール類、および硫黄/オクタデセン溶液などを使用することができる。
本発明の半導体ナノ粒子集合体は、極性分散媒に分散されて、半導体ナノ粒子集合体分散液を形成することができる。本発明において、半導体ナノ粒子集合体が分散媒に分散している状態とは、半導体ナノ粒子集合体と分散媒とを混合させた場合に、半導体ナノ粒子複合体が沈殿しない状態、もしくは目視可能な濁り(曇り)として残留しない状態であることを表す。なお、半導体ナノ粒子集合体が分散媒に分散しているものを半導体ナノ粒子集合体分散液と表す。
本発明では、本発明の半導体ナノ粒子集合体分散液の分散媒として、モノマーまたはプレポリマーを選択し、半導体ナノ粒子集合体組成物を形成することができる。つまり、本発明の半導体ナノ粒子集合体組成物は、本発明の半導体ナノ粒子集合体が、モノマーまたはプレポリマーに分散された半導体ナノ粒子集合体組成物である。モノマーまたはプレポリマーは、特に限定されないが、エチレン性不飽和結合を含むラジカル重合性化合物、シロキサン化合物、エポキシ化合物、イソシアネート化合物、およびフェノール誘導体などが挙げられる。モノマーとしては、例えば、上述した分散媒として用いられるモノマーが挙げられる。また、プレポリマーとしては、上述した分散媒として用いられるプレポリマーが挙げられる。
希釈組成物は、前述の本発明の半導体ナノ粒子集合体組成物が有機溶媒で希釈されてなるものである。
本発明の半導体ナノ粒子集合体硬化膜とは、本発明の半導体ナノ粒子集合体を含有した膜であり、硬化しているものを表す。本発明の半導体ナノ粒子集合体硬化膜は、前述の半導体ナノ粒子集合体組成物または希釈組成物を膜状に硬化することで得られる。
<コア粒子の製造>
酢酸インジウム(0.3mmol)およびオレイン酸亜鉛(0.55mmol)を、オレイン酸(0.9mmol)と1-ドデカンチオール(0.1mmol)とオクタデセン(10mL)との混合物に加え、真空下(<20Pa)で毎分10℃の昇温速度で室温から120℃まで加熱し、1時間反応させた。真空(<20Pa)で反応させた混合物を25℃、窒素雰囲気下にして、トリス(トリメチルシリル)ホスフィン(0.23mmol)を加えたのち、毎分10℃の昇温速度で300℃まで加熱し、10分間反応させた。さらに、反応液を25℃に冷却し、オクタン酸クロリド(0.60mmol)を注入し、毎分10℃の昇温速度で250℃まで加熱し、30分間反応させた後、25℃に冷却して、コア粒子の分散溶液を得た。
40mmolのオレイン酸亜鉛と75mLのオクタデセンを混合し、真空化で110℃にて1時間加熱し、[Zn]=0.4MのZn前駆体溶液を調整した。
22mmolのセレン粉末と10mLのトリオクチルホスフィンを窒素中で混合し、全て溶けるまで撹拌して[Se]=2.2Mのセレン化トリオクチルホスフィンを得た。
22mmolの硫黄粉末と10mLのトリオクチルホスフィンを窒素中で混合し、全て溶けるまで撹拌して[S]=2.2Mの硫化トリオクチルホスフィンを得た。
コア粒子の分散溶液を250℃まで加熱した。250℃において4.3mLのZn前駆体溶液と1.5mLのセレン化トリオクチルホスフィンを添加し、30分間反応させ、InP系半導体ナノ粒子の表面にZnSeシェルを形成した。さらに、3.8mLのZn前駆体溶液と0.5mLの硫化トリオクチルホスフィンを添加し、280℃に昇温して1時間反応させ、ZnSシェルを形成した。
得られた半導体ナノ粒子を、STEM-EDSによって観察したところ、コア/シェル構造をしていることが確認された。
上記のようにして得られたコア/シェル型構造の半導体ナノ粒子が分散している溶液にアセトンを加え、半導体ナノ粒子を凝集させた。次いで、遠心分離(4000rpm、10分間)後、上澄みを除去し、半導体ナノ粒子をヘキサンに再分散させた。これを繰り返して、精製された半導体ナノ粒子を得た。
(組成)
高周波誘導結合プラズマ発光分析装置(ICP)と蛍光X線分析装置(XRF)を用いて、組成分析を行った。表1に当該分析結果をインジウムに対するモル比で示した。
前述したように、量子効率測定システムを用いて、半導体ナノ粒子集合体の発光スペクトル(λ1)を測定し、半導体ナノ粒子集合体の量子効率(QY)、半導体ナノ粒子集合体の半値幅(FWHM1)及びピーク波長(λ1 MAX)を測定した。この時、励起光を450nmの単一波長とした。測定に用いる分散液としては吸収率が20~30%になるように濃度を調整したものを用いた。さらに、紫外可視分光光度計を用いて、半導体ナノ粒子の分散液に紫外から可視光を照射し吸収スペクトルを測定した。吸収スペクトルの測定に用いる分散液としては、分散媒を1mLに対して半導体ナノ粒子の量が1mgになるように濃度を調整したものを用いた。表2に当該分析結果を示した。
<測定準備>
以下の実験例において、個々の半導体ナノ粒子が発する蛍光発光の分光スペクトル測定には、倒立型サーチ光学顕微鏡(オリンパス社製IX73)を用い、高開口数対物レンズとしてオリンパス社製UPlan FNL 100×/1.30 NA, Oilを用いた。また、顕微鏡には、画像分光測定タイプの顕微鏡接続用イメージング分光器として分光計器社製CLP-50-D型と、高感度電子増倍型CCDカメラとしてAndor Technology社製 iXonを接続した。
個々の半導体ナノ粒子からの蛍光発光は、上記イメージング分光器によって変換されたスペクトル画像として、顕微鏡を介してCCDカメラに一定取込間隔で連続記録されるようにした。
また、顕微鏡と分光器の間には、幅100nmのスリットを配置し、全視野の一部分のみの像を取り込めるようにした。
半導体ナノ粒子を励起するための半導体レーザーとしては、波長445nmの青色レーザー光を発することができるネオアーク社製TC-20-4450を用い、当該レーザー光を顕微鏡に導入し収束させた後、後述する測定サンプルに対して照射されるように構成した。
なお、この際、不必要な励起光や散乱光が検出器に入るのをカットするため、必要な箇所に適宜光学フィルターを設置する。
測定対象の半導体ナノ粒子は、以下に示す方法で石英基板上に分散させて、測定サンプルとした。
先ず、2~3質量%程度のポリメチルメタクリレート(PMMA)を光学分析用のトルエンに溶解させて得られたトルエン溶液に対し、測定対象の半導体ナノ粒子集合体を構成する半導体ナノ粒子を、凝集が生じないよう分散させた。この際、後述するスペクトル測定において、複数個の粒子を一個の粒子と誤認しないよう、半導体ナノ粒子同士の間隔は1μm以上となるように、密度を調整すると良い。
そして、青色レーザー光によって励起発光しない合成石英基板(大興製作所製、Labo-CG)をスピンコーターに取り付け、その上に上記の半導体ナノ粒子を分散させたトルエン溶液を適量落とし、回転数1000~3000rpmの範囲で10~30秒間スピンコートした後、自然乾燥させることによって、PMMA膜中に半導体ナノ粒子が希薄に分散した薄膜を石英基板上に形成した。
これを測定用のサンプル基板として、顕微鏡の対物レンズ上に設置した。なお、以上の準備や作業においては、励起レーザー光により発光する不純物が混入しないよう注意が必要である。
以下の実験例における観察はすべて、大気中で20~25℃の室温下で行った。
顕微鏡の倍率および励起光の照射範囲は、サンプル基板上に励起光が当たる範囲がすべてCCDカメラに取り込めるよう、適時設定した。また、半導体ナノ粒子を励起するレーザー光の強度は、サンプル基板に対し、単位面積当たりの励起エネルギーが100~250W/cm2の範囲内に収まるよう出力を調整した。
顕微鏡と分光器に間にセットしたスリットを介して数個の半導体ナノ粒子のスペクトル像のみがCCDカメラに取り込まれる状態で、観察されるスペクトル像を1.0秒間隔(1Hz)で100点(100秒間)記録した。
得られたスペクトル画像において、波長については、予め波長が分かっているリファレンス光のスペクトル画像と比較することで算出し、また、強度については、粒子のない部分の強度をバックグランドとして全体の強度から差し引くといった補正を行い、個々の半導体ナノ粒子の波長と強度のデータ点を求め、更に、これを適宜のグラフソフトを用いてガウスフィットさせることで、個々の半導体ナノ粒子の発光スペクトル(λ2)、発光スペクトル(λ2)のピーク波長(λ2 MAX)、発光スペクトル(λ2)の半値幅(FWHM2)を数値化した。
なお、本実施例において上記数値化は、取り込んだ全ての画像からランダムに40粒子の半導体ナノ粒子を選択し、各粒子毎にランダムに選択した5点のスペクトルに対して行った。こうして得られた計200個の測定データに基づくことにより、半値幅(FWHM2)の平均値、ピーク波長(λ2 MAX)の標準偏差(SD1)、半値幅(FWHM2)の標準偏差(SD2)を得た。表2に当該分析結果を併記した。
製造に用いた原材料の組成比を変更した以外は、実験例1と同様にして半導体ナノ粒子を作製した後、実験例1と同様に分析を行った結果を表1及び表2に併記した。
コア粒子の製造時における加熱の昇温速度が毎分3℃であること、及び製造に用いた原材料の組成比を変更したこと以外は、実験例1と同様にして半導体ナノ粒子を作製した後、実験例1と同様に分析を行った結果を表1及び表2に併記した。
3、103 液晶
7、8 QDパターニング
9 拡散層
11 コア
12 シェル
102 QDフィルム
104 カラーフィルター(R)
105 カラーフィルター(G)
106 カラーフィルター(B)
Claims (12)
- In及びPを含有するコアと1層以上のシェルとを有するコア/シェル型半導体ナノ粒子の集合である半導体ナノ粒子集合体であって、
前記半導体ナノ粒子集合体を分散媒中に分散させた状態で450nmの励起光で励起させたときの発光スペクトル(λ1)のピーク波長(λ1 MAX)が605~655nmの間にあり、前記発光スペクトル(λ1)の半値幅(FWHM1)が43nm以下であり、
前記半導体ナノ粒子集合体を構成する半導体ナノ粒子を、445nmの励起光で励起させて得られる1粒子毎の発光スペクトル(λ2)が、以下の要件(1)~(3):
(1)発光スペクトル(λ2)の半値幅(FWHM2)の平均値が28nm以下であること、
(2)発光スペクトル(λ2)のピーク波長(λ2 MAX)の標準偏差(SD1)が10nm以上30nm以下であること、
(3)発光スペクトル(λ2)の半値幅(FWHM2)の標準偏差(SD2)が12nm以下であること、
の全てを満たすことを特徴とする半導体ナノ粒子集合体。 - 前記半値幅(FWHM1)が38nm以下であることを特徴とする請求項1に記載の半導体ナノ粒子集合体。
- 前記半値幅(FWHM2)の平均値が25nm以下であることを特徴とする請求項1又は2に記載の半導体ナノ粒子集合体。
- 前記標準偏差(SD2)が7nm以下であることを特徴とする請求項1~3の何れか一項に記載の半導体ナノ粒子集合体。
- 前記半値幅(FWHM1)が35nm以下であり、前記半値幅(FWHM2)の平均値が24nm以下であり、前記標準偏差(SD2)が6nm以下であることを特徴とする請求項1~4の何れか一項に記載の半導体ナノ粒子集合体。
- 前記半導体ナノ粒子集合体の量子効率(QY)が80%以上であることを特徴とする請求項1~5の何れか一項に記載の半導体ナノ粒子集合体。
- 前記半導体ナノ粒子集合体の量子効率(QY)が85%以上であることを特徴とする請求項6に記載の半導体ナノ粒子集合体。
- 前記半導体ナノ粒子集合体の量子効率(QY)が90%以上であることを特徴とする請求項7に記載の半導体ナノ粒子集合体。
- 前記半導体ナノ粒子が少なくともIn、P、Zn、Se及びハロゲンを含有し、
前記半導体ナノ粒子において、原子換算で、Inに対するP、Zn、Se及びハロゲンの各モル比が、P:0.20~0.95、Zn:11.00~50.00、Se:7.00~25.00、ハロゲン:0.80~15.00であること、
を特徴とする請求項1~8の何れか一項に記載の半導体ナノ粒子集合体。 - 請求項1~9の何れか一項に記載の半導体ナノ粒子集合体が、有機分散媒に分散した半導体ナノ粒子集合体分散液。
- 請求項1~9の何れか一項に記載の半導体ナノ粒子集合体が、モノマーまたはプレポリマーに分散した半導体ナノ粒子集合体組成物。
- 請求項1~9の何れか一項に記載の半導体ナノ粒子集合体が、高分子マトリクス中に分散した半導体ナノ粒子集合体硬化膜。
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