发明名称 Fine metal particles and fine metal oxide particles in dry powder form, and use thereof
摘要 The present invention provides a process for simply and easily producing fine metal particles or fine metal oxide particles in the form of a dry powder which can be used as extremely fine particles in a good dispersion state without causing coagulation for a long time even if not stored in a dispersion solvent. Fine metal particles or fine metal oxide particles in the form of a dry powder are prepared using a dispersion in which fine metal particles or fine oxide metal particles having a surface oxidation film are dispersed in an organic solvent in a stable state, while once covering the particle surface with covering agent molecules containing, at a terminal, a functional group having an oxygen atom, a nitrogen atom, or a sulfur atom as a group capable of forming a coordinative bond with metal, and by removing the dispersion solvent, washing and removing excess covering agent molecules with a polar solvent without damaging the covering agent molecule layer covering the fine particle surface, finally evaporating the polar solvent used for washing and drying.
申请公布号 US9233420(B2) 申请公布日期 2016.01.12
申请号 US201414158620 申请日期 2014.01.17
申请人 HARIMA CHEMICALS, INC. 发明人 Itoh Daisuke;Ueda Masayuki;Hata Noriaki;Matsuba Yorishige
分类号 B22F1/02;B22F1/00;B82Y30/00;C04B35/626;C04B35/628;C04B35/632;C09C1/62;H05K3/12 主分类号 B22F1/02
代理机构 Knobbe Martens Olson & Bear LLP 代理人 Knobbe Martens Olson & Bear LLP
主权项 1. A process for preparing fine metal particles in the form of a dry powder, characterized in that the fine metal particles in the form of a dry powder are free from any solvent, an average particle size of the fine metal particles themselves are selected in the range of 1 to 20 nm, the surface of the fine metal particles themselves is covered with one or more compounds selected from the group consisting of diamine compounds having an alkyl substituent on one of two amino groups, hydroxyamine compounds having an O-alkyl substituent, and monoamines containing a branched alkyl group, which diamine compounds, hydroxyamine compounds and monoamines have a boiling point of from 150° C. to 300° C., a covering amount of said one or more compounds is adjusted by selecting the total of said one or more compounds in the range of 5 to 35 parts by mass based on 100 parts by mass of the fine metal particles themselves, and thus, the fine metal particles in the form of a dry powder are composed of the fine metal particles themselves and the one or more compounds; and as for the step of adjustment of the covering amount, the process comprises the steps of: beforehand bringing said one or more compounds into contact with the surface of the fine metal particles themselves having an average particle size selected in the range of 1 to 20 nm, thereby once applying said one or more compounds through a coordinative bond with a metal element contained in the fine metal particles in an amount greater than the aimed covering amount in total of said one or more compounds based on 100 parts by mass of the fine metal particles themselves to form a covering layer thereof, and preparing, as a starting material, a dispersion in which the fine metal particles having a covering layer of said one or more compounds are dispersed in a dispersion solvent comprising one or more organic solvents, removing the organic solvent contained in the dispersion as a dispersion solvent under reduced pressure, thereby concentrating the dispersion, adding, to the dispersion subjected to the treatment for concentration, one or more polar solvents in which said one or more compounds exhibit a higher solubility at room temperature than that in the organic solvent, thereby dissolving excess of one or more compounds in said one or more polar solvents, and then separating fine metal particles in which the adjustment of the covering amount is attained by removing the excess of one or more compounds, as a solid phase component, from the obtained dispersion by filtration, and performing the treatment of evaporating the remaining one or more polar solvents at a temperature of 100° C. or lower to dry up, wherein a thickness of the covering layer formed with the adjusted covering amount is at least 0.5 nm or thicker, and selected in the range of 2/10 to 8/10 of the average particle size of the fine metal particles, and the one or more polar solvents are selected from the group consisting of alcohol solvents having a low boiling point of 80° C. or lower, ketone solvents having a low boiling point of 80° C. or lower and acetonitrile.
地址 Kakogawa-Shi JP