公开(公告)号：JP2009102716A

公开(公告)日：2009-05-14

申请号：JP2007277135

申请日：2007-10-25

Applicant: Dowa Electronics Materials Co Ltd ,  Dowaエレクトロニクス株式会社

Inventor： SATO KIMITAKA ,  OKANO TAKU

IPC: B22F9/24 ,  H01B13/00

Abstract: PROBLEM TO BE SOLVED: To provide a new synthesis method for silver nanoparticles by which reaction time can be more shortened, the using amount of a reducing agent can be more reduced, reaction temperature can be more lowered than a conventionally well-known alcoholic reduction method.
SOLUTION: In the method for producing silver nanoparticles, a solution, in which a silver compound is dissolved in a primary amine (X) with a molecular weight of 200 to 400 having an unsaturated bond, is held within the temperature region of 60 to 200°C and also below the boiling point of each amine composing the amine(s) (Y) in a state where one or more alcohol amines (Y) are mixed, thus the silver particles are precipitated by utilizing the reducing power of the amine(s) (Y). As the amine(s) (Y), for example, one or more among monoethanol amine, diethanol amine and triethanol amine can be selected. As the amine (X), foe example, oleylamine (C
9 H
18 =C
9 H
17 -NH
2 ; and molecular weight, 267.4) is exemplified as a suitable object.
COPYRIGHT: (C)2009,JPO&INPIT

Abstract translation: 要解决的问题：为了提供银纳米颗粒的新合成方法，其可以更短时间地反应时间，还原剂的使用量可以进一步降低，反应温度可以比常规公知的更低 酒精还原法 解决方案：在制备银纳米颗粒的方法中，将银化合物溶解在具有不饱和键的分子量为200-400的伯胺（X）中的溶液保持在 在混合一种或多种醇胺（Y）的状态下，在构成所述胺（Y）的各种胺的沸点为60〜200℃，低于沸点的情况下，通过利用 胺（Y）。 作为胺（Y），例如可以选择单乙醇胺，二乙醇胺和三乙醇胺中的一种或多种。 作为胺（X），作为实施例，油胺（C 8 S 9 SB 17） NH 2 ;分子量267.4）作为合适的目的被列举。 版权所有（C）2009，JPO＆INPIT

公开(公告)号：JP2007258677A

公开(公告)日：2007-10-04

申请号：JP2007001310

申请日：2007-01-09

Applicant: Dowa Electronics Materials Co Ltd ,  Dowaエレクトロニクス株式会社

Inventor： SATO KIMITAKA ,  KUEDA MINORU ,  OKANO TAKU ,  OGI KOZO

IPC: H01L31/04 ,  H01L21/28

CPC classification number: Y02E10/50

Abstract: PROBLEM TO BE SOLVED: To provide a conductive thin film which can be largely formed in a non-vacuum atmosphere and at temperatures lower than 300°C, has a texture structure suitable as a reflective film on the side of a rear electrode of a thin-film solar cell, and has high adhesion with a substrate with a low resistance. SOLUTION: A silver conductive film is a silver thin film formed on a substrate, is made up of a layer including sintered silver particles having an average grain size D TEM of 100 nm or less, has a resistivity of 5 μΩ cm or less, includes not more than three holes/μm 2 in the sintered layer, and has a texture structure with a surface roughness Ra of 10 nm to 100 nm. The silver conductive film having such a texture structure can be manufactured by a manufacturing process including a step of applying a solution of dispersed silver particles to the substrate to form a film, and then sintering the film. The solution is obtained by dispersing silver particles having an average grain size D TEM of 100 nm or less in a liquid organic medium which is nonpolar or has low polarity and boils at 60 to 300°C. COPYRIGHT: (C)2008,JPO&INPIT

Abstract translation: 要解决的问题：为了提供可以在非真空气氛中并且在低于300℃的温度下大部分形成的导电薄膜，具有适合作为背面电极侧的反射膜的织构结构 的薄膜太阳能电池，并且与具有低电阻的基板具有高粘附性。 解决方案：银导电膜是在基板上形成的银薄膜，由包括平均晶粒尺寸D TEM 的烧结银颗粒的层为100nm以下的层构成，具有 5μΩcm以下的电阻率在烧结层中包含不超过三个孔/μm 2 ，并且具有表面粗糙度Ra为10nm至100nm的织构结构。 具有这样的纹理结构的银导电膜可以通过包括以下步骤的制造方法制造：将分散的银粒子的溶液施加到基板上以形成膜，然后烧结该膜。 通过将平均粒径D TEM 的银颗粒分散在非极性或极性低的液体有机介质中并在60〜300℃下沸腾而得到溶液。 版权所有（C）2008，JPO＆INPIT

公开(公告)号：JP2009161808A

公开(公告)日：2009-07-23

申请号：JP2008000220

申请日：2008-01-06

Applicant: Dowa Electronics Materials Co Ltd ,  Dowaエレクトロニクス株式会社

Inventor： SATO KIMITAKA ,  OKANO TAKU ,  NAKANOYA TARO

IPC: B22F1/02 ,  B22F1/00 ,  B22F9/24 ,  B82Y20/00 ,  B82Y30/00 ,  B82Y40/00 ,  B82Y99/00 ,  C09C1/62 ,  C09C3/08 ,  C09D1/00 ,  C09D5/24 ,  C09D7/12 ,  C09D11/00 ,  C09D11/52 ,  C09D201/00 ,  H01B1/22 ,  H01B5/00 ,  H01B13/00

CPC classification number: C09C1/62 ,  B22F1/0018 ,  B22F1/0022 ,  B22F9/24 ,  B22F2998/00 ,  B22F2999/00 ,  B82Y30/00 ,  C01P2002/88 ,  C01P2004/04 ,  C01P2004/64 ,  C01P2006/40 ,  C09D5/24 ,  C09D11/52 ,  H01B1/22 ,  Y10T428/2991 ,  B22F2301/255 ,  B22F2304/054 ,  B22F1/0059

Abstract: PROBLEM TO BE SOLVED: To provide a silver fine powder covered with a protective material which can greatly lower a sintering temperature than a conventional one. SOLUTION: The silver fine powder is formed of silver particles which have an average particle diameter D TEM of 3 to 20 nm or an X-ray crystal grain size D X of 1 to 20 nm, and have hexylamine (C 6 H 13 -NH 2 ) adsorbed on their surfaces. When the silver fine powder is mixed with an organic medium to form a silver paint, the silver paint is applied onto a substrate to form a paint film, and the paint film is baked in the atmosphere at 120°C, the silver fine powder shows properties of being converted into an electroconductive film having a specific resistance of 25 μΩcm or less. Even when the paint film is baked at 100°C, the obtained electroconductive film shows the specific resistance of 25 μΩcm or less. The silver fine powder can be produced by mixing a dispersion liquid of silver particles, in which the silver particles covered with a primary amine (A) having an unsaturated bond and a molecular weight of 200 to 400 are monodispersed in the organic medium, with hexylamine, and holding the mixture at 5 to 80°C in a state of being stirred to form sedimentary particles. COPYRIGHT: (C)2009,JPO&INPIT

Abstract translation: 要解决的问题：提供覆盖有保护材料的银细粉末，其可以大大降低烧结温度，而不是常规的。 解决方案：银细粉末由平均粒径D TEM 为3〜20nm的银颗粒或X射线晶粒尺寸D X 1〜20nm，并且具有吸附在其表面上的己胺（C 6 H 13 -NH SB 2）。 当银粉末与有机介质混合形成银漆时，将银涂料施加到基材上以形成漆膜，并将该漆膜在大气中在120℃下烘烤，银细粉末显示 被转换成电阻率为25μΩcm以下的导电膜的性质。 即使在100℃下烘烤漆膜时，得到的导电膜的电阻率为25μΩcm以下。 通过将银粒子的分散液与己胺分散在单颗分散在有机介质中的具有不饱和键的伯胺（A）和分子量为200〜400的银粒子的分散液，可以制造银细粉末。 ，并在搅拌的状态下将混合物保持在5〜80℃，形成沉积粒子。 版权所有（C）2009，JPO＆INPIT

公开(公告)号：JP2008169453A

公开(公告)日：2008-07-24

申请号：JP2007005756

申请日：2007-01-15

Applicant: Dowa Electronics Materials Co Ltd ,  Dowaエレクトロニクス株式会社

Inventor： OKANO TAKU ,  OGI KOZO ,  SATO KIMITAKA

IPC: B22F9/24 ,  C09D1/00 ,  H01B1/22

Abstract: PROBLEM TO BE SOLVED: To provide a silver particle-dispersed liquid capable of forming a coating film having satisfactory adhesion with a substrate such as a glass substrate and a resin substrate even if being fired at a relatively low temperature of ≤300°C without adding a silane coupling agent and a thermosetting resin and without requiring a complicated heat treatment step, and to provide a method for producing the same.
SOLUTION: In alcohol having a boiling point of 80 to 200°C or polyol having a boiling point of 150 to 300°C as a reactive medium and a reducing agent, silver particles produced by subjecting a silver compound to reducing treatment at 80 to 200°C are dispersed into a liquid organic medium in the coexistence of a fatty acid compound having a boiling point of ≥300°C and an amine compound having a boiling point of 150 to 350°C as an organic protective agent.
COPYRIGHT: (C)2008,JPO&INPIT

Abstract translation: 要解决的问题：即使在相对较低的温度≤300°的温度下进行烧制，也可以提供能够形成与玻璃基板，树脂基板等基板具有良好粘接性的涂膜的银粒子分散液 并且不需要复杂的热处理步骤，并且提供一种制备该硅烷偶联剂的方法。 解决方案：在沸点为80-200℃的醇或沸点为150-300℃的多元醇作为反应介质和还原剂中，通过使银化合物在 将80〜200℃分散在沸点≥300℃的脂肪酸化合物与沸点为150〜350℃的胺化合物共存的液体有机介质中作为有机保护剂。 版权所有（C）2008，JPO＆INPIT

公开(公告)号：JP2010248539A

公开(公告)日：2010-11-04

申请号：JP2009096261

申请日：2009-04-10

Applicant: Dowa Electronics Materials Co Ltd ,  Dowaエレクトロニクス株式会社

Inventor： OKANO TAKU

IPC: B22F9/24 ,  B22F1/00 ,  B22F1/02 ,  B22F9/00 ,  H01B1/00 ,  H01B1/22 ,  H01B5/00 ,  H01B13/00

Abstract: PROBLEM TO BE SOLVED: To provide a method for producing silver nanoparticles each having the property of hardly forming a defective coating film when applied, the silver nanoparticles obtained thereby and a dispersion liquid of the silver nanoparticles.
SOLUTION: The method for producing silver nanoparticles includes the steps of: adding an amine compound having ≥15°C solidifying point and 100-1,000 molecular weight to alcohol having 80-200°C boiling point; and reducing a silver ion in the amine compound-added alcohol to coat the surface of silver with the amine compound and obtain silver powder. The amine compound to be used has preferably ≤83 iodine value. Fig.2 shows an example of a coating film with excellent smoothness having hardly any defects, while Fig.3 shows an example of a defective coating. film in which white spots are present at several places.
COPYRIGHT: (C)2011,JPO&INPIT

Abstract translation: 要解决的问题：提供一种制备银纳米颗粒的方法，其中所述的银纳米颗粒在施加时具有几乎不形成不良涂膜的性质，由此获得的银纳米颗粒和银纳米颗粒的分散液。 解决方案：制备银纳米颗粒的方法包括以下步骤：向具有80-200℃沸点的醇加入具有≥15℃凝固点和100-1,000分子量的胺化合物; 并在加入胺化合物的醇中还原银离子以用胺化合物涂覆银表面，得到银粉。 所使用的胺化合物优选为≤83碘值。 图2示出了几乎没有缺陷的具有优异平滑性的涂膜的实例，而图3显示了有缺陷的涂层的实例。 几个地方存在白点的电影。 版权所有（C）2011，JPO＆INPIT

公开(公告)号：JP2009068053A

公开(公告)日：2009-04-02

申请号：JP2007236037

申请日：2007-09-11

Applicant: Dowa Electronics Materials Co Ltd ,  Dowaエレクトロニクス株式会社

Inventor： OKANO TAKU ,  SATO KIMITAKA

IPC: B22F9/24 ,  B22F1/02 ,  H01B1/22 ,  H01B13/00

Abstract: PROBLEM TO BE SOLVED: To provide silver particles which are as extremely fine as 3 to 7 nm in mean particle diameter D
TEM and are extremely satisfactory in dispersibility in liquid and are adequate for drawing of fine wiring by an ink jet method in particular.
SOLUTION: The method for manufacturing the silver particles includes a step of dissolving a silver compound using primary amine (for example, oleylamine) of a molecular weight ≥200 having an unsaturated bond as a solvent, and a step of compositing the silver particles of 3 to 7 nm in mean particle diameter D
TEM covered on the amine by heating and holding the solvent in a temperature area of ≥95°C and where the silver compound does not thermally decompose. The silver particles obtained in the manner described above have a grain size distribution of ≤15% in CV value expressed by the standard deviation [standard deviation δD of particle diameter]/D
TEM x100 and the degree of single crystallization expressed by D
TEM /D
X is, for example, ≤2.0.
COPYRIGHT: (C)2009,JPO&INPIT

Abstract translation: 要解决的问题：为了提供平均粒径D 为3〜7nm极细的银颗粒，并且在液体中的分散性非常令人满意并且足以拉伸细 特别是通过喷墨法进行布线。 解决方案：用于制造银颗粒的方法包括使用具有不饱和键的分子量≥200的伯胺（例如油胺）作为溶剂溶解银化合物的步骤，以及将银 通过加热并保持溶剂在≥95℃的温度区域并且银化合物不热分解而在胺上覆盖3至7nm的平均粒径D TEM 的颗粒。 以上述方式得到的银粒子，以标准偏差[粒径的标准偏差δD] / D ×100表示​​的CV值的晶粒度分布≤15％，单位面积 由D / D X 表示的结晶例如为≤2.0。 版权所有（C）2009，JPO＆INPIT

公开(公告)号：JP2009091634A

公开(公告)日：2009-04-30

申请号：JP2007264598

申请日：2007-10-10

Applicant: Dowa Electronics Materials Co Ltd ,  Dowaエレクトロニクス株式会社

Inventor： SATO KIMITAKA ,  OKANO TAKU

IPC: B22F9/24 ,  H01B13/00

Abstract: PROBLEM TO BE SOLVED: To provide a technique which can obtain silver fine powder in which only silver nanoparticles having extremely high dispersibility are sorted at a high yield without adding a reduction auxiliary agent.
SOLUTION: Disclosed is a method for producing silver fine powders comprising: a process A where a solution in which a silver compound is dissolved into a mixed solvent of primary amine X with a molecular weight of 200 to 400 having an unsaturated bond and 2-octanol is held at 130 to 180°C, thus, utilizing the reduction force of the 2-octanol, silver particles are precipitated, so as to obtain slurry in which silver particles coated with an organic substance (protective material) are present; a process B where the slurry is subjected to solid-liquid separation, so as to recover a solid content; and a process C where the solid content is cleaned, and is thereafter subjected to solid-liquid separation, so as to recover the cleaned solid content.
COPYRIGHT: (C)2009,JPO&INPIT

Abstract translation: 解决的问题：提供一种可以获得银微粉末的技术，其中仅添加非常高分散性的银纳米粒子以高产率分选而不添加还原助剂。 解决方案：公开了一种生产银细粉末的方法，其包括：方法A，其中将银化合物溶解在具有不饱和键的分子量为200-400的伯胺X的混合溶剂中， 2-辛醇保持在130〜180℃，因此利用2-辛醇的还原力，沉淀出银粒子，得到其中存在有有机物质（保护材料）的银粒子的浆料; 将浆料进行固液分离的方法B，以回收固体成分; 和清洁固体成分的方法C，然后进行固液分离，以回收清洁的固体成分。 版权所有（C）2009，JPO＆INPIT

公开(公告)号：JP2008190025A

公开(公告)日：2008-08-21

申请号：JP2007173732

申请日：2007-07-02

Applicant: Dowa Electronics Materials Co Ltd ,  Dowaエレクトロニクス株式会社

Inventor： SATO KIMITAKA ,  OKANO TAKU

IPC: B22F1/02 ,  B22F9/24 ,  B82Y30/00 ,  B82Y40/00 ,  C09D11/00 ,  C09D11/38 ,  C09D11/52

CPC classification number: B22F9/24 ,  B22F1/0007 ,  B22F1/0022 ,  B22F1/0062 ,  B82Y30/00 ,  C09D11/30 ,  C09D11/36 ,  C09D11/52 ,  H01B1/02 ,  H01B1/22 ,  H05K1/097 ,  H05K2201/0224 ,  Y10T428/2982 ,  Y10T428/2991 ,  Y10T428/2998

Abstract: PROBLEM TO BE SOLVED: To provide silver nanoink in which the concentration of silver is remarkably increased while satisfactorily maintaining the dispersibility of silver fine powder. SOLUTION: A silver fine powder composed of silver particles having an average particle diameter of not more than 20 nm is disclosed, each of which particles has an organic protection material on the surface. The presence ratio of the organic protection material to the total of the silver particle and the organic protection material is 0.05 to 25% by mass. An amine compound having a molecular weight of 100 to 1,000 is suitably used for the organic protection material, and such as compound having one or more unsaturated bonds in a molecule is particularly suitable. In the silver fine powder, the crystallite diameter on the (111) crystal face of the silver particle is not more than 20 nm. An ink having a viscosity of not more than 50 mPa s is also disclosed, which is obtained by dispersing the silver powder in an organic solvent so that the silver concentration is not less than 10% by mass. COPYRIGHT: (C)2008,JPO&INPIT

Abstract translation: 要解决的问题：提供银纳米颗粒，其中银的浓度显着增加，同时令人满意地保持银细粉的分散性。 解决方案：公开了由平均粒径不大于20nm的银颗粒构成的银细粉末，其中每个颗粒在表面上具有有机保护材料。 有机保护材料与银粒子和有机保护材料的总量的存在比为0.05〜25质量％。 分子量为100〜1000的胺化合物适用于有机保护材料，分子中具有一个以上不饱和键的化合物特别合适。 在银细粉末中，银颗粒（111）晶面上的微晶直径不超过20nm。 还公开了粘度不大于50mPa·s的油墨，其通过将银粉分散在有机溶剂中而使银浓度不小于10质量％得到。 版权所有（C）2008，JPO＆INPIT

公开(公告)号：JP2008084620A

公开(公告)日：2008-04-10

申请号：JP2006261526

申请日：2006-09-26

Applicant: Dowa Electronics Materials Co Ltd ,  Dowaエレクトロニクス株式会社

Inventor： OGI KOZO ,  OKANO TAKU

IPC: H01B5/00 ,  B22F1/00 ,  B22F9/24 ,  H01B1/22 ,  H01B5/14 ,  H01B13/00

CPC classification number: B82Y30/00 ,  B22F1/0022 ,  B22F1/0062 ,  B22F9/24 ,  B22F2998/00 ,  H01B1/02 ,  H01B1/22 ,  H05K1/097 ,  H05K2201/0224 ,  H05K2201/0266 ,  H05K2203/1131

Abstract: PROBLEM TO BE SOLVED: To improve adhesiveness to a glass substrate, polyimide film substrate, or the like at low temperature baking of 300°C or lower, without addition of silane coupling agent or thermosetting resin at electrode or circuit formation using silver particle powder dispersion liquid. SOLUTION: The powder of silver particle containing an organic protective film is featured by a broad granularity distribution in which CV value calculated with a following expression (1) is 40% or higher, using the particle size measured by TEM (transmission type electron microscope) observation. The organic protective film is constituted of, for example, fatty acid (oleic acid) of molecular weight 100-1,000 and amine compound of molecular weight 100-1,000. At least either the fatty acid or amine compound comprises at least one unsaturated bonding in a single molecule. The expression (1): CV value=100×[standard deviation σ D of particle size]/[average particle size D TEM ]. COPYRIGHT: (C)2008,JPO&INPIT

Abstract translation: 要解决的问题：为了提高在300℃以下的低温烘烤下对玻璃基板，聚酰亚胺膜基板等的粘附性，在电极上添加硅烷偶联剂或热固性树脂或使用银的电路形成 颗粒粉末分散液。 解决方案：使用通过TEM测定的粒径（透射型），以下述式（1）计算出的CV值为40％以上的宽粒度分布，具有含有有机保护膜的银粒子的粉末 电子显微镜）观察。 有机保护膜由例如分子量为100-1,000的脂肪酸（油酸）和分子量为100-1,000的胺化合物构成。 脂肪酸或胺化合物中的至少一种在单个分子中包含至少一个不饱和键。 表达式（1）：CV值= 100×[标准偏差σ D 粒径] / [平均粒径D TEM ]。 版权所有（C）2008，JPO＆INPIT

公开(公告)号：EP1983528A4

公开(公告)日：2015-07-29

申请号：EP07706716

申请日：2007-01-09

Applicant: DOWA ELECTRONICS MATERIALS CO

Inventor： SATO KIMITAKA ,  HISAEDA YUTAKA ,  OKANO TAKU ,  OGI KOZO

IPC: H01B5/14 ,  C23C18/08 ,  H01B13/00 ,  H01L31/0224 ,  H01L31/0392

CPC classification number: H01L31/022425 ,  C23C18/08 ,  H01L31/0392 ,  Y02E10/50 ,  Y10T428/24413