Zirconium-containing nitride powder, black UV-curable resin composition, black resin cured product, electronic materials

Abstract

The present invention provides a zirconium-containing nitride powder, a black UV-curable resin composition, a black resin cured product, and an electronic material that are suitable as a black pigment for a black UV-curable resin composition that exhibits excellent visible light shielding properties, exhibits black color, and has excellent UV-curing properties. [Solution] The zirconium-containing nitride powder of the present invention is characterized by containing at least one element, niobium or tantalum, in the zirconium nitride crystal. The black ultraviolet-curable resin composition of the present invention is characterized by containing the zirconium-containing nitride powder of the present invention, a photopolymerizable compound, and a photopolymerization initiator.

Description

Technical Field

[0001] This invention relates to zirconium-containing nitride powder, a black ultraviolet curable resin composition, a cured black resin, and an electronic material.

Background Art

[0002] For example, as a black matrix for a display device (display) composed of liquid crystal, organic EL, etc., a light-shielding material for a C image sensor, a light-shielding material for an optical member, a light-shielding filter, an IR (infrared) cut filter, a coverlay film, a light-shielding film for an electronic member, a black film, etc., a black resin composition containing an insulating black pigment is used. Here, as a method for curing a black resin composition, a photolithography method using an ultraviolet curable resin is widely known. For the insulating black pigment used in this photolithography method using an ultraviolet curable resin, ultraviolet transmittance is required.

[0003] For example, in Patent Document 1, for the purpose of improving the transmittance in the ultraviolet region, a coloring composition for a light-shielding film combining inorganic particles containing titanium and an organic pigment as a pigment has been proposed. Further, in Patent Document 2, an ultraviolet curable black composition using zirconium nitride particles as a black pigment is known.

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Patent Document 2

Summary of the Invention

Problems to be Solved by the Invention

[0005] However, in the colored composition for light-shielding films disclosed in Patent Document 1, the absorption of ultraviolet light by inorganic particles containing titanium is significant, which may result in insufficient transmission of ultraviolet light and inadequate curing by ultraviolet light. Furthermore, in the UV-curable black composition disclosed in Patent Document 2, zirconium nitride particles are used as the black pigment, but the peak of light absorption is located around a wavelength of 600-700 nm, and although it is black, it sometimes exhibits a slight bluish tint. If the content of the black pigment is increased in order to make it even blacker, the transmission of ultraviolet light becomes insufficient, and the UV-curable resin cannot be cured efficiently.

[0006] This invention has been made in view of the circumstances described above, and aims to provide a zirconium-containing nitride powder, a black ultraviolet-curable resin composition, a black resin cured product, and an electronic material that are suitable as a black pigment for a black ultraviolet-curable resin composition that exhibits excellent visible light shielding properties, exhibits black color, and has excellent photocurability properties by ultraviolet light. [Means for solving the problem]

[0007] In order to solve the above problems, the inventors of this invention conducted diligent research and obtained the following findings. It was found that by adding appropriate amounts of niobium or tantalum to zirconium nitride powder, which can be used as a black powder, the absorption peak of visible light is shifted to the shorter wavelength side, and by absorbing visible light sufficiently, the blackness is increased without exhibiting a blue color.

[0008] The zirconium-containing nitride powder of Embodiment 1 of the present invention is based on the above-mentioned findings and is characterized by having a structure in which at least one element, niobium or tantalum, is contained in the crystal of the zirconium nitride. According to the zirconium-containing nitride powder of embodiment 1 of the present invention, the zirconium nitride crystal has a structure in which at least one element, niobium or tantalum, is contained, so the absorption peak of visible light is shifted to the shorter wavelength side, and the blackness can be increased without exhibiting a blue color by sufficiently absorbing visible light.

[0009] The zirconium-containing nitride powder of embodiment 2 of the present invention is characterized in that, in the zirconium-containing nitride powder of embodiment 1 of the present invention, the ratio α(550) / α(365) of the extinction coefficient of ultraviolet light at a wavelength of 365 nm to the extinction coefficient of visible light at a wavelength of 550 nm, measured using a dispersion obtained by dispersing the zirconium-containing nitride powder in butyl carbitol acetate at a concentration of 50 mass sppm, is 1.2 or more. According to the zirconium-containing nitride powder of embodiment 2 of the present invention, the ratio α(550) / α(365) of the extinction coefficient α(365) of ultraviolet light at a wavelength of 365 nm to the extinction coefficient α(550) of visible light at a wavelength of 550 nm in the above-mentioned dispersion is 1.2 or more, so it can sufficiently absorb visible light and has excellent ultraviolet light transmittance.

[0010] The zirconium-containing nitride powder of embodiment 3 of the present invention is a zirconium-containing nitride powder of embodiment 1 or embodiment 2 of the present invention, wherein the extinction coefficient α(550) of visible light at a wavelength of 550 nm, measured using a dispersion obtained by dispersing the zirconium-containing nitride powder in butyl carbitol acetate at a concentration of 50 mass sppm, is 80 m -1 The above is its defining characteristic. According to the zirconium-containing nitride powder of embodiment 3 of the present invention, the extinction coefficient α(550) of visible light at a wavelength of 550 nm in the above-mentioned dispersion is 80 nm. -1 As such, it can absorb visible light sufficiently and increase the blackness.

[0011] The black ultraviolet-curable resin composition of aspect 4 of the present invention is characterized by containing a zirconium-containing nitride powder according to any one of aspects 1 to 3 of the present invention, a photopolymerizable compound, and a photopolymerization initiator. According to the black ultraviolet-curable resin composition of aspect 4 of the present invention, since it contains a zirconium-containing nitride powder of any one of aspects 1 to 3 of the present invention, it has a high visible light absorption rate and excellent ultraviolet light transmittance, making it possible to cure it efficiently with ultraviolet light.

[0012] The cured black resin of Embodiment 5 of the present invention is characterized in that it is a cured product of the black ultraviolet curable resin composition of Embodiment 4 of the present invention. According to the cured black resin of Embodiment 5 of the present invention, since it is a cured product of the black ultraviolet curable resin composition of Embodiment 4 of the present invention, it has a high blackness degree and can sufficiently block visible light.

[0013] The electronic material of Embodiment 6 of the present invention is characterized by containing the black ultraviolet curable resin composition of Embodiment 4 of the present invention. According to the electronic material of Embodiment 6 of the present invention, since it contains the black ultraviolet curable resin composition of Embodiment 4 of the present invention, it has a high blackness degree, can sufficiently block visible light, and is excellent in various properties.

Advantages of the Invention

[0014] According to the present invention, it is possible to provide a zirconium-containing nitride powder suitable as a black pigment of a black ultraviolet curable resin composition excellent in visible light shielding property, exhibiting black color, and excellent in photocurability by ultraviolet rays, a black ultraviolet curable resin composition, a cured black resin, and an electronic material.

Brief Description of the Drawings

[0015] [Figure 1] It is an explanatory diagram showing the light absorption spectrum in an example of the present invention.

Modes for Carrying Out the Invention

[0016] Hereinafter, embodiments of the present invention will be described. Each of the embodiments shown below is specifically described to better understand the gist of the invention, and unless otherwise specified, does not limit the present invention.

[0017] The zirconium-containing nitride powder according to the present embodiment is used as an insulating black pigment, and has a structure in which at least one element of niobium or tantalum is contained in the crystal of zirconium nitride. In the zirconium-containing nitride powder according to this embodiment, it is confirmed by X-ray diffraction that it has the same crystal structure as zirconium nitride, and it is specified by analysis with a scanning electron microscope equipped with an EDS that it contains niobium (Nb) or tantalum (Ta).

[0018] Thus, by having a structure in which at least one of niobium or tantalum is contained in the crystal of zirconium nitride, the wavelength of the absorption peak of visible light is shifted to the short wavelength side, and the visible light is sufficiently absorbed.

[0019] Here, in the zirconium-containing nitride powder according to this embodiment, the total content of niobium or tantalum is preferably 0.5 atomic % or more and 20 atomic % or less. When the total content of niobium or tantalum is 0.5 atomic % or more, the wavelength of the absorption peak of visible light will surely shift to the short wavelength side. On the other hand, when the total content of niobium or tantalum is 20 atomic % or less, the characteristics as zirconium nitride can surely be maintained. In addition, the total content of niobium or tantalum is more preferably 1 atomic % or more and even more preferably 5 atomic % or more. Also, the total content of niobium or tantalum is more preferably 15 atomic % or less and even more preferably 10 atomic % or less.

[0020] Further, in the zirconium-containing nitride powder according to this embodiment, hafnium and oxygen may be contained as impurity elements other than nitrogen, zirconium, niobium, and tantalum. Note that the total content of these impurity elements is preferably 10 mass % or less and preferably 5 mass % or less.

[0021] Further, in the zirconium-containing nitride powder according to this embodiment, the average particle diameter is preferably in the range of 5 nm or more and 150 nm or less. Furthermore, the average particle size of the zirconium-containing nitride powder is more preferably 8 nm or larger, and even more preferably 10 nm or larger. In addition, the average particle size of the zirconium-containing nitride powder is more preferably 100 nm or smaller, and even more preferably 80 nm or smaller.

[0022] Furthermore, in the zirconium-containing nitride powder of this embodiment, it is preferable that the ratio α(550) / α(365) of the extinction coefficient of ultraviolet light at a wavelength of 365 nm and the extinction coefficient of visible light at a wavelength of 550 nm, measured using a dispersion solution in which the zirconium-containing nitride powder is dispersed in butyl carbitol acetate to a concentration of 50 mass sppm, is 1.2 or higher. As mentioned above, the α(550) / α(365) ratio being 1.2 or higher allows for efficient absorption of visible light while ensuring ultraviolet light transmission. Here, the above-mentioned α(550) / α(365) is more preferably 1.3 or greater, and even more preferably 1.4 or greater. There is no particular upper limit to α(550) / α(365), but it is practically 12 or less.

[0023] The extinction coefficient α mentioned above can be measured as follows. As described above, a dispersion of zirconium-containing nitride powder, which is the basis of this embodiment, in butyl carbitol acetate is placed in a cell with a path length d (unit: m). Light is shone into the cell containing the dispersion, and the transmitted light intensity of the light that passes through the cell is measured. The path length d, the incident light intensity I0 of the light shone into the cell, and the transmitted light intensity I of the light that passes through the cell are substituted into the following equation (1) to calculate α as the extinction coefficient of the light shone into the cell. I = I0 exp(-α × d) ... (1)

[0024] Furthermore, in the zirconium-containing nitride powder of this embodiment, the extinction coefficient α(550) of visible light at a wavelength of 550 nm, measured using a dispersion solution in which the powder is dispersed in butyl carbitol acetate at a concentration of 50 mass sppm, is 80 m -1 It is preferable that the above conditions are met. The above α(550) is 80m -1 As a result of the above, visible light can be absorbed efficiently. Here, the above-mentioned α(550) is 90m -1 It is more preferable that it be greater than or equal to 100m -1 It is even more preferable that the above is true. Note that there is no particular upper limit to α(550), but practically speaking, 1200m is preferable. -1 The results are as follows:

[0025] Next, a method for producing the zirconium-containing nitride powder according to this embodiment will be described. The zirconium-containing nitride powder of this embodiment can be produced using a thermal plasma apparatus such as a high-frequency induction thermal plasma nanoparticle synthesis apparatus. The thermal plasma apparatus comprises a raw material supply machine that supplies raw materials to a plasma torch, a plasma torch connected to the raw material supply machine that synthesizes and nitrides the raw materials by the thermal plasma method, an induction coil wound around the outer circumference of the plasma torch, a high-frequency power supply electrically connected to the induction coil that supplies high-frequency power to the induction coil, a chamber connected to the plasma torch through which a cooling gas such as N2 gas or Ar gas flows, and a bag filter connected to the chamber that recovers the zirconium-containing nitride powder.

[0026] To produce zirconium-containing nitride powder using the above-described thermal plasma apparatus, first, raw material powder containing zirconium, niobium, and tantalum is supplied to the raw material feeder. The zirconium, niobium, and tantalum contained in the raw materials may be metal powders, nitride powders, or oxide powders.

[0027] Next, the raw material powder supplied to the raw material feeder is introduced into the plasma torch along with a carrier gas such as N2 gas or Ar gas. The plasma torch may have an N2 gas atmosphere, a mixed gas atmosphere of N2 and H2, a mixed gas atmosphere of N2 and Ar, or a mixed gas atmosphere of N2 and NH3. These N2-containing gases generate thermal plasma of N2 gas, thermal plasma of a mixed gas of N2 and H2, thermal plasma of a mixed gas of N2 and Ar, or thermal plasma (plasma flame) of a mixed gas of N2 and NH3 by supplying high-frequency power from a high-frequency power supply to an induction coil. The raw material metal powder introduced into the plasma torch then volatilizes and gasifies due to the high-temperature thermal plasma of N2 gas, etc., generated in the plasma torch at several thousand degrees Celsius, that is, it undergoes a synthetic nitriding reaction by the thermal plasma method.

[0028] Next, the gasified raw material metal is rapidly cooled in a chamber through which a cooling gas such as N2 gas or Ar gas flows. That is, it is instantaneously cooled and condensed by a cooling gas such as N2 gas or Ar gas in a chamber below the plasma torch, thereby generating zirconium-containing nitride powder. The generated zirconium-containing nitride powder is recovered by a bag filter. In this way, the zirconium-containing nitride powder of this embodiment is produced.

[0029] Next, the black ultraviolet-curable resin composition according to this embodiment will be described. The black ultraviolet-curable resin composition according to this embodiment contains the zirconium-containing nitride powder according to this embodiment, a photopolymerizable compound, and a photopolymerization initiator.

[0030] The zirconium-containing nitride powder according to this embodiment is included as an insulating black pigment. In addition, the zirconium-containing nitride powder content in the black UV-curable resin composition according to this embodiment is preferably in the range of 0.1 parts by mass or more and 60 parts by mass or less per 100 parts by mass of the black UV-curable resin composition.

[0031] The photopolymerizable compound included in the black UV-curable resin composition according to this embodiment can be a radical polymerizable compound, a cationic polymerizable compound, or an anionic polymerizable compound. For example, as the radical polymerizable compound, an oligomer having an ethylenically unsaturated bond or a polyfunctional monomer having three or more ethylenically unsaturated bonds can be used. The oligomer having an ethylenically unsaturated bond may be an acrylic oligomer having two or more (meth)acryloyl groups. The acrylic oligomer is a low molecular weight polymer obtained by polymerizing acrylic monofunctional monomers. Examples of acrylic oligomers include acrylic (meth)acrylate, urethane (meth)acrylate, epoxy (meth)acrylate, and polyester (meth)acrylate. The molecular weight of the acrylic oligomer may be, for example, in the range of 1,000 to 10,000 in number average molecular weight.

[0032] The (meth)acrylate monomers and oligomers described above can be used individually or in combination of two or more. Furthermore, the acrylic oligomers are not limited to those described above, and commonly available oligomers can be used. The polyfunctional monomer having an ethylenically unsaturated bond may be an acrylic polyfunctional monomer having three or more (meth)acryloyl groups. Examples of acrylic polyfunctional monomers include pentaerythritol tri(meth)acrylate, pentaerythritol tetra(meth)acrylate, and trimethylolpropane tri(meth)acrylate.

[0033] Examples of cationic polymerizable compounds include epoxy compounds and oxetane compounds. Epoxy compounds are not particularly limited as long as they have a reactive epoxy group, and examples include bisphenol A type epoxy, bisphenol F type epoxy, biphenyl type epoxy, biphenyl mixed type epoxy, naphthalene type epoxy, cresol novolac type epoxy, dicyclopentadiene type epoxy, trisphenolethane type epoxy, tetraphenolethane type epoxy, aliphatic epoxy, and alicyclic epoxy. Oxetane compounds include the aforementioned oxetane compounds and oligomers obtained by partially polymerizing them. The content of the photopolymerizable compound is preferably in the range of 5 parts by mass or more and 99 parts by mass or less per 100 parts by mass of the black ultraviolet-curable resin composition.

[0034] In this embodiment, the photopolymerizable compound is preferably a structure having a carboxyl group in the repeating unit within the molecule. By using a photopolymerizable compound containing a carboxyl group within the molecule, the dispersibility of the particles is improved.

[0035] The photopolymerization initiator included in the black UV-curable resin composition according to this embodiment is preferably a compound that absorbs ultraviolet light, specifically light with a wavelength of 100 to 400 nm, and can initiate a polymerization reaction. The amount of photopolymerization initiator should be, for example, within the range of 0.5 parts by mass to 15 parts by mass per 100 parts by mass of UV-curable organic matter.

[0036] The photopolymerization initiator contained in the black UV-curable resin composition according to this embodiment may be, for example, a radical generator or a photoacid generator. Examples of UV curing agents include acetophenone compounds, benzophenone compounds, benzoin ether compounds, triazine compounds, phosphine oxide compounds, sulfonium compounds, iodonium compounds, and organic peroxides.

[0037] Examples of acetophenone compounds include acetophenone, dimethylacetophenone, and 2-hydroxy-2-methylpropiophenone. Examples of benzophenone compounds include benzophenone and 2-chlorobenzophenone. Examples of benzoin ether compounds include benzoin and benzoin methyl ether. Examples of phosphine oxide compounds include bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide and 2,4,6-trimethylbenzoyl-diphenylphosphine oxide. Examples of sulfonium compounds include triphenylsulfonium tetrafluoroborate, tri-p-tolylsulfonium trifluoromethanesulfonate, diphenyl[4-(phenylthio)phenyl]sulfonium hexafluoroantimonate, and diphenyl[4-(phenylthio)phenyl]sulfonium hexafluorophosphate. Examples of iodonium compounds include bis(4-tert-butylphenyl)iodonium hexafluorophosphate and diphenyliodonium hexafluorophosphate. Examples of organic peroxides include benzoyl peroxide and cumene peroxide.

[0038] In the black ultraviolet-curable resin composition according to this embodiment, in addition to the photopolymerizable compound, photopolymerization initiator, and zirconium-containing nitride powder (black pigment), it may also contain plasticizers and other additives (surfactants, leveling agents, etc.).

[0039] Examples of plasticizers that can be used include phosphate ester plasticizers, phthalate ester plasticizers, aliphatic-basic ester plasticizers, aliphatic dibasic acid ester plasticizers, dihydric alcohol ester plasticizers, and oxyacid ester plasticizers. Examples of phosphate ester plasticizers include tributyl phosphate and 2-ethylhexyl phosphate. Examples of phthalate ester plasticizers include dimethyl phthalate and dibutyl phthalate. Examples of aliphatic-basic ester plasticizers include butyl oleate and glycerol monooleate. Examples of aliphatic dibasic acid ester plasticizers include dibutyl adipate and di-2-ethylhexyl sebacate. Examples of dihydric alcohol ester plasticizers include diethylene glycol dibenzoate and triethylene glycol di-2-ethylbutyrate. Examples of oxyacid ester plasticizers include methyl acetylricinoleate and tributyl acetylcitrate.

[0040] Next, a method for producing the black ultraviolet-curable resin composition according to this embodiment will be described. First, a black dispersion is prepared by dispersing zirconium-containing nitride powder (black pigment) in a solvent. As the solvent, monomers with reactive functional groups in their molecules, water, and organic solvents can be used. Examples of monomers having reactive functional groups within the molecule include (meth)acrylic monomers having a (meth)acryloyl group, epoxy monomers having an oxirane ring such as an epoxy group or a glycidyl group, vinyl monomers having a vinyl group or a vinyl ether group, and oxetane monomers having an oxetanyl group. Examples of organic solvents include ethyl carbitol acetate, ethyl carbitol acetate, butyl carbitol, methyl cellosolve, ethyl cellosolve, diethylene glycol ethyl methyl ether, propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate (PGMEA), propylene glycol monoethyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, triethylene glycol monomethyl ether, triethylene glycol monoethyl ether, and other glycol ethers, as well as α-terpineol, methyl ethyl ketone (MEK), ethyl acetate, butyl acetate, n-propanol, isopropanol, methanol, ethanol, and toluene. Furthermore, from the viewpoint of improving the dispersion efficiency of the zirconium-containing nitride powder (black pigment), it is preferable to use a low-viscosity solvent with a viscosity of 100 Pa·s or less at 25°C.

[0041] Here, the black dispersion may contain a dispersant. As this dispersant, for example, an organic substance having a group that has affinity for zirconium-containing nitride powder (black pigment) can be used. Examples of groups that have affinity for zirconium-containing nitride powder (black pigment) include secondary amine groups, tertiary amine groups, carboxylic acid groups, phosphate groups, and phosphate ester groups. Dispersants that can be used include polymeric dispersants with molecular weights ranging from several thousand to tens of thousands, silane coupling agents such as organotriethoxysilane and organotrimethoxysilane, and titanate coupling agents.

[0042] The black dispersion obtained as described above is mixed with the photopolymerizable compound and the photopolymerization initiator. There are no particular restrictions on the mixing method; for example, mixing equipment such as a planetary agitator, a three-roll mill, or a kneader can be used. In this way, the black ultraviolet-curable resin composition of this embodiment is manufactured.

[0043] The black dispersion obtained as described above is mixed with the photopolymerizable compound and the photopolymerization initiator. There are no particular restrictions on the mixing method; for example, mixing equipment such as a planetary agitator, a three-roll mill, or a kneader can be used. In this way, the black ultraviolet-curable resin composition of this embodiment is manufactured.

[0044] The black resin cured product of this embodiment is obtained by curing the black ultraviolet-curable resin composition of this embodiment described above. In this embodiment, the cured black resin is formed by, for example, applying the black UV-curable resin composition of this embodiment onto a substrate to form a coating film. Next, the coating film is irradiated with ultraviolet light to polymerize the photopolymerizable compound. As the ultraviolet light source, halogen lamps, metal halide lamps, UV-LEDs, etc., can be used, and the light source is not particularly limited as long as it has a wavelength that matches the absorption wavelength of the photopolymerization initiator.

[0045] The electronic material of this embodiment includes the black ultraviolet-curable resin composition of this embodiment. Specific examples of electronic materials include, for instance, black matrices and black column spacers for color filters, CMOS camera modules, sealing materials for liquid crystal display elements, partition materials for micro-LEDs, semiconductor encapsulants, underfill materials, black paste for circuit concealment, light-shielding solder resist, black UV-curing inks, and optical adhesives.

[0046] According to the zirconium-containing nitride powder of this embodiment, which has the above configuration, the zirconium nitride crystal contains at least one element, niobium or tantalum. As a result, the absorption peak of visible light is shifted to the shorter wavelength side, and by sufficiently absorbing visible light, the blackness increases without exhibiting a blue color, thereby improving the light-shielding properties of visible light.

[0047] In the zirconium-containing nitride powder of this embodiment, if the ratio α(550) / α(365) of the extinction coefficient of ultraviolet light at a wavelength of 365 nm to the extinction coefficient of visible light at a wavelength of 550 nm, measured using a dispersion obtained by dispersing the zirconium-containing nitride powder in butyl carbitol acetate at a concentration of 50 mass sppm, is 1.2 or higher, then it can sufficiently absorb visible light and has excellent ultraviolet transmittance.

[0048] In this embodiment of the zirconium-containing nitride powder, the extinction coefficient α(550) of visible light at a wavelength of 550 nm, measured using a dispersion obtained by dispersing the zirconium-containing nitride powder in butyl carbitol acetate at a concentration of 50 mass sppm, is 80 m -1 In the above cases, sufficient absorption of visible light increases the blackness without exhibiting a blue color, thereby improving the light-blocking properties of visible light.

[0049] According to the black UV-curable resin composition of this embodiment, since the zirconium-containing nitride powder of this embodiment is contained as a black pigment, it has a high visible light absorption rate and excellent UV transmittance, allowing for efficient curing by ultraviolet light and forming a black resin cured product with excellent visible light shielding properties.

[0050] According to this embodiment, the cured black resin product is a cured product of the black ultraviolet-curable resin composition of this embodiment, and therefore has a high degree of blackness, can sufficiently block visible light, and is particularly suitable as a light-shielding member. The electronic material of this embodiment contains the black ultraviolet-curable resin composition of this embodiment, and therefore has high blackness, can sufficiently block visible light, and has excellent various properties.

[0051] Although one embodiment of the present invention has been described above, the present invention is not limited thereto and can be modified as appropriate without departing from the technical spirit of the invention. [Examples]

[0052] The verification experiments conducted to confirm the effectiveness of the present invention will be described.

[0053] Zirconium-containing nitride powder was prepared using a high-frequency induction thermal plasma system JHS-35M (manufactured by JEOL Ltd.). First, raw material metal powders, including zirconium nitride powder, metallic niobium powder, and metallic tantalum powder, were supplied to the raw material feeder. The raw materials used were zirconium nitride powder (Nippon Shin Kinzoku, purity 97 mass%, average particle size 1 μm), metallic niobium powder (High Purity Chemicals, purity 99 mass%, average particle size 20 μm), and metallic tantalum powder (High Purity Chemicals, purity 99.9 mass%, average particle size 45 μm).

[0054] Next, the raw material powder supplied to the raw material feeder was introduced into the plasma torch along with an N2 gas carrier gas. The inside of the plasma torch was kept in an N2 gas atmosphere, and a thermal plasma of N2 gas was generated. The raw material powder introduced into the plasma torch was vaporized and gasified by the thermal plasma of N2 gas at several thousand degrees Celsius generated inside the plasma torch, and the synthetic nitriding reaction proceeded using the thermal plasma method. Next, the gasified raw material metal was instantaneously cooled and condensed by N2 gas (cooling gas) in a chamber below the plasma torch, thereby generating zirconium-containing nitride powder.

[0055] As described above, as examples of the present invention, zirconium-containing nitride powder containing 5 atomic percent of niobium (Nb), zirconium-containing nitride powder containing 10 atomic percent of niobium (Nb), zirconium-containing nitride powder containing 5 atomic percent of tantalum (Ta), and zirconium-containing nitride powder containing 10 atomic percent of tantalum (Ta) were prepared (Examples 1-4). Furthermore, as a comparative example, zirconium-containing zirconium nitride powder was prepared using only zirconium nitride powder (Nippon Shinkinzoku, purity 97 mass%, average particle size 1 μm) as the raw material, and manufactured using a plasma apparatus in the same manner.

[0056] The absorption spectra of these samples were examined. A dispersion of butyl carbitol acetate with a black pigment dispersed at 50 mass sppm was packed into a quartz cell with a path length of 10 mm. Using a spectrophotometer (Hitachi High-Tech Fielding Co., Ltd. UH-4150), transmitted light from wavelengths of 300 nm to 1300 nm was measured. The path length d, the incident light intensity I0 of the light irradiated onto the cell, and the transmitted light intensity I of the light that passed through the cell were substituted into equation (1) above to calculate α as the extinction coefficient of the light irradiated onto the cell. The measurement results are shown in Figure 1. The values ​​of α(365), α(550), and α(550) / α(365) are shown in Table 1.

[0057] [Table 1]

[0058] In both zirconium nitride powders containing niobium (Nb) and zirconium nitride powders containing tantalum (Ta), the absorption peaks were found to be shifted to shorter wavelengths compared to zirconium nitride powder. Furthermore, the shift was larger in zirconium nitride powders containing 10 atomic percent niobium and tantalum than in zirconium nitride powders containing 5 atomic percent niobium and tantalum.

[0059] As described above, it has been confirmed that the present invention provides a zirconium-containing nitride powder suitable as a black pigment for a black UV-curable resin composition that exhibits excellent visible light shielding properties, exhibits black color, and has excellent UV-curing properties. [Industrial applicability]

[0060] The black ultraviolet-curable resin composition containing the zirconium-containing nitride powder of the present invention as a black pigment can be suitably used, for example, as a material for forming black patterns in black resists and black inks for inkjet printers. Furthermore, the cured black resin product of the black ultraviolet-curable resin composition of the present invention can be used as a black matrix in image forming elements used in display devices such as liquid crystal displays and organic EL displays, or as a light-shielding material in image sensors such as CMOS sensors. Furthermore, the black resin cured product of the present invention can also be used as a material for sealing materials for liquid crystal display elements, black column spacers, partition materials for micro-LEDs, semiconductor encapsulants, underfill materials, black pastes for concealing circuits, light-shielding solder resists, black UV-curing inks, and optical adhesives.

Claims

1. A zirconium-containing nitride powder characterized by containing at least one element, niobium or tantalum, in the zirconium nitride crystal.

2. The zirconium-containing nitride powder according to claim 1, characterized in that the ratio α(550) / α(365) of the extinction coefficient of ultraviolet light at a wavelength of 365 nm to the extinction coefficient of visible light at a wavelength of 550 nm, measured using a dispersion obtained by dispersing the zirconium-containing nitride powder in butyl carbitol acetate at a concentration of 50 mass ppm, is 1.2 or more.

3. The extinction coefficient α(550) of visible light at a wavelength of 550 nm, measured using a dispersion obtained by dispersing the zirconium-containing nitride powder in butyl carbitol acetate at a concentration of 50 mass ppm, was 80 m －１ The zirconium-containing nitride powder according to claim 1, characterized in that it is as described above.

4. A black ultraviolet-curable resin composition characterized by containing a zirconium-containing nitride powder according to any one of claims 1 to 3, a photopolymerizable compound, and a photopolymerization initiator.

5. A cured black resin product characterized by being a cured product of the black ultraviolet-curable resin composition described in claim 4.

6. An electronic material characterized by comprising the black ultraviolet-curable resin composition described in claim 4.

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