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Black titanium oxynitride pigment, method for producing the same, and resin compound for encapsulating semiconductor using black titanium oxynitride pigment

A technology of titanium oxynitride and manufacturing method, which is applied in the direction of titanium oxide/hydroxide, nitrogen compound, semiconductor devices, etc., to achieve the effect of improving covering, high electrical insulation, and high α-ray shielding

Active Publication Date: 2017-12-01
MITSUBISHI MATERIALS ELECTRONICS CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, black titanium oxynitride pigments may generate α-rays due to impurities (particularly lead) contained in ilmenite (the raw material of titanium oxide that becomes the raw material of black titanium oxynitride)

Method used

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  • Black titanium oxynitride pigment, method for producing the same, and resin compound for encapsulating semiconductor using black titanium oxynitride pigment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0035] Next, examples of the present invention will be described in detail together with comparative examples.

[0036]

[0037] First, titanium chloride is treated by distillation (impurity reduction method) at a temperature range of 130 to 140° C. to reduce uranium content and thorium content in titanium chloride, respectively. Next, 45 moles of isopropanol (alcohol) was added to 10 moles of distilled titanium chloride, and titanium chloride and isopropanol (alcohol) were reacted to produce titanium tetraisopropoxide (titanium alkoxide). . Furthermore, titanium tetraisopropoxide was distilled for 5 hours by vacuum distillation (temperature 130-150° C., pressure 10-20 Pa) to reduce the content of uranium and thorium in titanium tetraisopropoxide. Next, the distilled titanium tetraisopropoxide was hydrolyzed to produce a white titanium oxide pigment (TiO 2 ). And, utilize the ammonia gas of flow rate 10 liters / min to above-mentioned white titanium oxide pigment (TiO 2 ) ...

Embodiment 2

[0039] Utilize ammonia gas to the white titanium oxide pigment (TiO2) used in embodiment 1 2 ) is reduced to obtain a black titanium oxynitride pigment, but the ammonia flow rate and the reaction time during this reduction are each set as half of that of Example 1. Ethanol was added as alcohol to the black titanium oxynitride pigment, the black titanium oxynitride pigment was dispersed in ethanol, and wet pulverized by a bead mill to obtain a black titanium oxynitride pigment dispersion with an average primary particle size of 140 nm. The black titanium oxynitride pigment is composed of the chemical formula: TiN X o Y (wherein, X=0.2, Y=0.8). Furthermore, the above-mentioned dispersion liquid was subjected to solid-liquid separation and dried to obtain a black titanium oxynitride pigment. This black titanium oxynitride pigment was referred to as Example 2.

Embodiment 3

[0041] A black titanium oxynitride pigment was obtained in the same manner as in Example 1 except that the temperature during vacuum distillation of tetraisopropoxytitanium was 180°C. This black titanium oxynitride pigment was referred to as Example 3.

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Abstract

The alpha ray emission of the black titanium oxynitride pigment of the present invention is 0.1 cph / cm2 or less. In addition, the black titanium oxynitride pigment preferably has a uranium content of 1 mass ppb or less and a thorium content of 5 mass ppb or less.

Description

technical field [0001] The present invention relates to a black titanium oxynitride pigment with reduced uranium content and thorium content, a method for producing the black titanium oxynitride pigment, and a semiconductor sealing resin compound using the black titanium oxynitride pigment. In addition, this international application claims priority based on Japanese Patent Application No. 064922 (Japanese Patent Application No. 2014-064922) filed on Mar. 27, 2014, and uses all the contents of Japanese Patent Application No. 2014-064922 in this international application. Background technique [0002] In the past, a carbon black colorant for semiconductor sealing materials has been disclosed, which is filtered through a filter with a pore size of 5 μm or less after wet oxidation treatment of carbon black, and then the carbon black content is concentrated and adjusted to 3-3 μm. 50% by mass of carbon black slurry is obtained by spray-drying. The carbon black colorant for semic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/04C08K3/00C08K3/28C08L63/00H01L23/29H01L23/31
CPCC01B21/0821C08K3/28H01L23/295C01P2004/64C09C1/36C01P2006/62H01L2924/0002C08K3/013H01L2924/00C08L63/00C08K3/00
Inventor 影山谦介石黑茂树
Owner MITSUBISHI MATERIALS ELECTRONICS CHEM CO LTD
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