TW200809876A - Conductive particle, conductive powder consisting thereof, process for producing the same, and conductive ink obtained using the conductive powder - Google Patents
Conductive particle, conductive powder consisting thereof, process for producing the same, and conductive ink obtained using the conductive powder Download PDFInfo
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- TW200809876A TW200809876A TW96122328A TW96122328A TW200809876A TW 200809876 A TW200809876 A TW 200809876A TW 96122328 A TW96122328 A TW 96122328A TW 96122328 A TW96122328 A TW 96122328A TW 200809876 A TW200809876 A TW 200809876A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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Abstract
Description
200809876 九、發明說明: 【發明所屬之技術領域】 本發明係有關於導電性粒子與該導電性粒子所構成之 ‘電性粉體、並勢4太 、#希, ” 1 &方法以及利用該導電性粉體所製出的 ¥电ί生墨水。且特別有關於使用氧化鈦於導電性粒子 =造導電性墨水等之際,即使花費較長的分散時間:; 月b 所得到的導電膜的電阻之變動的導電性粒子。 【先前技術】 於塑膠薄膜或塗裝的領域’在要求遮蔽性的用途方 因應明色的情形則氧化鈦等作為填料 電性=碳黑㈣^ 能形=:==_僅在必要的部分 以推廣開來。使用㈣好’而期待今後的用途得 然而’騎與導電性的 黑色,其使时… $而使用奴黑…則塗膜成為 原料的代表之氧化叙# 色的遮敝用 在導電性方面1 、·,右以此氧化鈦作為填料來使用,則 在⑷生方面就會有所不足。因此,作為改 i 形之技術’於專利文獻1( 广 10-Π7729號公報)中福·,/、專利申明書特開平 氧化鋁等作A %卩*母、二氧化矽、氧化鈦、 乳化料作為原料的血小板㈣針狀的基質上, 及/或组來進行摻雜_ 、 ^鎚 的導電性顏料。另方:的氧化錫或二氧化欽作為導電層 面,諸位本發明者已完成申請以二 2213-8940-PF;Ahddub 5 200809876 • 氧化鈦作為心材並塗布氧化錫的導電性粒子。 % tj» ^ ^ ^ a 元成申請的發明中,藉由設置在芯材的表面使 用氧化錫之莫, 、電a ’仍維持著明色而具有遮蔽性與導電性 的導電性粒子,並使用此導電性粒子所得到的塗膜顯示 1 · 0x10 Ω /□上下的表面電阻。然而,在使用該導電性粒 子於塗料等之際,欲得到均勻的混合狀態,或強力授拌、 或包括反覆的攪拌之長時間授拌,則其後所得到的導電 _ ',原本應得到的電阻值卻上昇了,而有無法得到所預期 的效果之問題。因此,對於可使用於抑制電阻值變動的導 電性塗料或導電性墨水之導電性粉體’有其需求存在著。200809876 IX. Description of the Invention: [Technical Field of the Invention] The present invention relates to an electro-powder composed of conductive particles and the electroconductive particles, and a method of utilizing the electric powder, the potential 4, and the #1, and the method and utilization thereof The electric current produced by the conductive powder is particularly useful in the case of using titanium oxide in the case of conductive particles = conductive ink, etc., even if a long dispersion time is required: Conductive particles in which the resistance of the film fluctuates. [Prior Art] In the field of plastic film or coating, in the case of applications requiring shielding properties, titanium oxide or the like is used as a filler. Electrical properties = carbon black (4) =:==_ Only in the necessary parts to promote. Use (four) good 'and look forward to future use, however, 'riding with conductive black, which makes time... $ and use slave black... then the film becomes raw material The representative of the oxidized ## color concealer used in the electrical conductivity 1 , ·, right using this titanium oxide as a filler, there will be some disadvantages in (4) health. Therefore, as a technology to change the shape of the i- Document 1 (Guang 10-Π7729号Report) Zhongfu·, /, patent declaration special open alumina, etc. as A*卩* mother, cerium oxide, titanium oxide, emulsified material as raw material platelets (four) needle-like substrate, and / or group to do Conductive pigments of miscellaneous _, ^ hammer. Others: tin oxide or dioxygen as a conductive layer, the inventors have completed the application to 2213-8940-PF; Ahddub 5 200809876 • titanium oxide as a heart material and coated oxidation Conductive particles of tin. % tj» ^ ^ ^ a In the invention of the application, by using tin oxide on the surface of the core material, the electric a ' remains bright and has shielding and conductivity. The conductive film and the coating film obtained by using the conductive particles exhibit a surface resistance of 1 · 0x10 Ω / □. However, when the conductive particles are used in a paint or the like, a uniform mixed state is desired, or Strong mixing, or long-time mixing with repeated stirring, then the resulting conductivity _ ', the resistance value originally obtained should rise, and there is a problem that the expected effect cannot be obtained. Used to suppress electricity Value change of conductive ink or conductive coating of conductive powder 'there have their needs.
因此’諸位本申請者,再一次有關於導電性粒子,姑 專心致志研究,而查明前述電阻值的上昇係起因於芯材: 導電層之間的剝離現象。亦即,㈣層容易由芯材剝離,、 再藉由以同樣的厚度形成導電層,則完成了由導電性^ 所得到的導電膜為穩定的而能夠確保導電性的導電:粒 更且,有關本發明的導 藉由調整導電層的組成而能 值’又因形狀為粒狀故分散 且平滑的導電膜。 電性粒子同時具有以下特徵: 夠凋整所得到的導電膜的電阻 性優異,而容易獲得凝聚較少 子 體 所構成之導電性粉體、其製造方法以及利用該導屬 2213-8940-PF;Ahddub 6 200809876 所製出的導電性墨水加以說明。 有關本發明的導電性粒子: 係於芯材粒子表面且有 / x明的導電性粒子 /、百V私層的粒狀導雷 在於:前述芯材粒f # τ 〃子,其特徵 河祖子係Τ102,於該粒 1^〇2導電層。 衣面具有摻入鈮的 於有關本發明的導電性粒子, 2ηπι〜15nm較佳。 J述蜍电層的厚度係 又㈤述導電層的鈮含有 T · Λ曰 右將導電性粒子令邱的Therefore, the applicants once again studied conductive particles and studied it with enthusiasm, and found that the rise in the resistance value was caused by the peeling phenomenon between the core materials: the conductive layers. In other words, the (four) layer is easily peeled off from the core material, and by forming the conductive layer with the same thickness, the conductive film obtained by the conductivity is stable and the conductivity can be ensured: the grain is further The conductive film of the present invention which is dispersed and smoothed by adjusting the composition of the conductive layer and having an energy value 'is also a granular shape. The electric particles have the following characteristics: the conductive film obtained by the entanglement is excellent in electrical resistance, and the conductive powder composed of a small number of aggregates is easily obtained, the manufacturing method thereof, and the use of the derivative 2213-8940-PF ; Conductive ink made by Ahddub 6 200809876 is explained. The conductive particles according to the present invention: the conductive particles of the surface of the core material particles and having /x bright, and the granular guide of the hundred V private layer are: the core material particles f # τ 〃子, the characteristic of the ancestors The sub-system 102 is on the conductive layer of the granules. The coating surface has conductive particles to which the ruthenium is incorporated in the present invention, and 2 η π 〜 15 nm is preferable. J describes the thickness of the electrical layer. (5) The conductive layer contains T T 右 right and the conductive particles make Qiu
Ti〇2菫設為100重量%時,則係〇 〇5重旦 ° 有關本發明的導電性於體.古里❶重較佳。 係以前述導電性粒子所構成的導電性粉體,其特徵在於體 别料電性粒子的初級粒徑係G. G 5心1、m。When Ti〇2菫 is set to 100% by weight, it is preferable that the conductivity of the present invention is relatively high. The conductive powder composed of the conductive particles is characterized in that the primary particle diameter of the bulk electrical particles is G. G 5 core 1, m.
前述導電性粉體的中位徑D 較佳。 以體和基準係以下 前述導電性粉體的比# % , 2 一 "的比表面積係ImVg〜22mVg較佳。 前述導電性粉體中芯材粒 _ γ 丁的比表面積與所得到的導 電性粒子的比表面積之比〔(導 伃到的ν 电性粒子的比表面 材粒子的比表面積)〕係1.0〜2.0更佳。 、〜 有關本發明的導電性粉體之製造方法發 導電性粉體之製造方法,其特徵 的 牡孓具有以下的步驟Α〜Ε。 A :將Ti〇2粉末分散於水中 驟。 w"1〇2懸浮液的步 B:添加鈦鹽與鈮鹽於前述71〇2懸浮液中,並加以溶 解而得到反應用液的步驟。 2213~8940~PF;Ahddub 7 200809876 c將别述反應用液調製於中性〜驗性範圍,而得到含 有摻入鈮的Ti〇2前驅物塗布之Ti〇2粒子的懸浮液之步驟。 D:對前述懸浮液施行固液分離,並將分取的摻入鈮的 Ti(h前驅物塗布之Ti〇2粉末加以乾燥,而得到摻入鈮的 Ti(h前驅物塗布之Ti〇2粉餅之步驟。 E:將藉由乾燥而假固化的摻入㈣η〇2前驅物塗布 之Ti〇2粉餅加以粉碎之後,施行培燒而得到導電性粉體之 步驟。The median diameter D of the conductive powder is preferred. The specific surface area of the ratio of the above-mentioned conductive powders of the above-mentioned conductive powder is preferably in the range of ImVg to 22 mVg. The ratio of the specific surface area of the core material _ γ butyl to the specific surface area of the obtained conductive particles in the conductive powder [(the specific surface area of the specific surface material particles of the ν electric particles) is 1.0~ 2.0 is better. The method for producing a conductive powder according to the present invention is a method for producing a conductive powder, characterized in that the oyster has the following steps. A: Disperse the Ti〇2 powder in water. w"1〇2 suspension step B: A step of adding a titanium salt and a cerium salt to the above 71 〇 2 suspension and dissolving it to obtain a reaction liquid. 2213~8940~PF; Ahddub 7 200809876 c The reaction liquid is prepared in a neutral to the range of the test, and a step of containing a suspension of Ti〇2 particles coated with a ruthenium-doped Ti〇2 precursor is obtained. D: The solid suspension is subjected to solid-liquid separation, and the Ti (h precursor-coated Ti〇2 powder) doped with cerium is dried to obtain Ti (h precursor-coated Ti〇2). Step of the powder cake E: A step of pulverizing the Ti〇2 powder cake coated with the (tetra) η〇2 precursor by dry curing and then pulverizing the mixture to obtain a conductive powder.
於前述步驟A所使用的Ti〇2粉末之粒徑為〇 〇5# m〜1.0/^,懸浮液中的Ti〇2濃度為2〇g/L〜5〇〇g/L較佳。 於前述步驟B的鈦鹽係由水溶性鈦鹽的硫酸鈦醯、四 氯化鈦1酸鈦、四1化鈦之中所選擇的i種或2種以上, 鈦濃度為1重量%〜3 〇重量%較佳。 五氯化鈮、五氟化鈮、五碘 以上’銳濃度為0.02莫耳 於前述步驟B的鈮鹽係由 化鈮之中所選擇的1種或2種 /L〜0· 5莫耳/L較佳。The particle size of the Ti〇2 powder used in the above step A is 〇5#m~1.0/^, and the concentration of Ti〇2 in the suspension is preferably 2〇g/L to 5〇〇g/L. The titanium salt in the above step B is one or more selected from the group consisting of titanium titanate, titanium tetrachloride titanate and titanium tetraoxide of a water-soluble titanium salt, and the titanium concentration is 1% by weight to 3 〇% by weight is preferred. Antimony pentachloride, antimony pentafluoride, pentadium iodide or higher 'The sharp concentration is 0.02 mol. The barium salt of the above step B is one or two selected from the plutonium / L / 0 · 5 mol / L is preferred.
於前述步驟C的調整後的H p係7〜11的中性〜鹼性範 圍,而使用由NaOH、Κ0Η、Na2C〇3、今—山 風之中所選擇的1種或 2種以上於pH調整為較佳。 ’ 於前述步驟E的焙燒環境係 八虱%境為較佳。 有關本發明的導電性墨水: β關本發明的導電性墨水 係使用前述導電性粉體作為顏料者。 有關本發明的導電膜··有關 +、、酋十从電ρ 本备明的導電膜係使用前 述導電性墨水而得到者。 2213-8940-PF;Ahddub 8 200809876 發明效果: 有關本魚明的導電性粒子,作為怒材與導電層的共同 原料係使用τ1〇2,藉此而使芯材與導電層之間的界線顯得 !清楚’因此能夠防止芯材與導電層之間的剝離。更且, 藉由形成同樣厚度的導 一 的V弘層,則由使用此種導電性粒子的 導電塗料所传到的導電膜呈現穩定的導電性。並且,利 用凋正鈮摻入1’則表面電阻值亦可作到目標的範圍内。 又由於導電性粒子録狀,故在塗料中的分散性相當優 異’因政聚較少,%可得到平滑的導電膜。使用如此施行 所製出的導電性粉體來作為填料之塗膜或塑膠,外觀依然 維持著明色並具有導電性,巾導電性則依其用途來設定於 最適範圍。In the neutral to alkaline range of the adjusted H p series 7 to 11 in the above step C, one or two or more selected from the group consisting of NaOH, Κ0Η, Na2C〇3, and present-mountain wind are used for pH adjustment. It is better. The calcination environment in the above step E is preferably 80%. The conductive ink of the present invention: β is a conductive ink of the present invention, and the conductive powder is used as a pigment. The conductive film of the present invention is obtained by using the conductive ink described above in relation to the conductive film of the present invention. 2213-8940-PF; Ahddub 8 200809876 Effect of the invention: The conductive particles of the fish body use τ1〇2 as a common raw material of the anger material and the conductive layer, thereby making the boundary between the core material and the conductive layer appear Clear! Therefore, peeling between the core material and the conductive layer can be prevented. Further, by forming the V-layer of the same thickness of the conductive layer, the conductive film which is transferred by the conductive paint using such conductive particles exhibits stable conductivity. Moreover, the surface resistance value can be made into the target range by incorporating the positive electrode with 1'. Further, since the conductive particles are recorded, the dispersibility in the coating material is quite excellent. ” Because of less political aggregation, a smooth conductive film can be obtained. The coating film or the plastic which is used as the filler by using the conductive powder thus produced maintains a bright color and has an electrical conductivity, and the conductivity of the towel is set to an optimum range depending on the application.
【實施方式】 有關本發明的導電性粒子的實施例:有關本發明的導 電性:子係於芯材粒子表面具有導電層的粒狀導電性粒 子,可述芯材粒子係、Ti〇2,於該粒子表面具有摻人錕的Ti^ 導電層者。 關於本專利申請案,使用鈮作為對Ti〇2的摻入材料雖 可得到良好的導電性’但存在於導電層内的鈮的形態並不 明瞭。而係在週期表上與鈮接近的元素的鉅的氧化物亦習 知與鈮的氧化物同樣顯示良好的導電性。因而,一般認為 使用组來代替鈮亦可獲得同等的效果。 並且’本發明中由於使用粒狀的τ i 〇2作為芯材,故所 2213-8940-PF;Ahddub 9 200809876[Embodiment] The conductive particles of the present invention are related to the conductive particles of the present invention: the particulate conductive particles having a conductive layer on the surface of the core material particles, and the core material particles, Ti〇2, On the surface of the particle, there is a Ti^ conductive layer doped with germanium. With regard to this patent application, the use of ruthenium as a material for doping Ti 2 can provide good conductivity, but the form of ruthenium present in the conductive layer is not clear. The giant oxides of the elements which are close to the ruthenium on the periodic table are also known to exhibit good electrical conductivity as well as the oxides of ruthenium. Therefore, it is generally considered that the use of a group instead of 铌 can also achieve the same effect. And in the present invention, since granular τ i 〇 2 is used as the core material, 2213-8940-PF; Ahddub 9 200809876
付到的導電性粒子也成為粒狀,因係以摻入鈮的Ti〇2來構 f導電層’故該導電層與芯材粒子之間的界面顯得不清 =:可明特徵之—°導電層與&材之間的界面顯得不清 疋的W係、因使用共同的Ti〇2於芯材與導電層的原料之 故如刖述,雖係在大氣中對換入銳的咖前驅物塗布之 二他粒子施予焙燒而得到導電性粒子,但利用焙燒使咖 河驅物變成Τ1〇2的燒結狀態,致芯材與導電層之間的黏附 變得很堅固,此因界面不明之故。因此,一般認為於培燒 :施行對形成導電層的陶入鈮,則藉由此銳擴散於芯 材的T i 〇2側而完成由莫φ Μ 成甶V電層至芯材層的鈮的濃度梯度。 於有關本發明的導電性粒子,前述導電層的厚度係 2mn〜15nm較佳’前述導電層的鈮含有率,若將導電性粒子 内的T1〇2量設為1〇〇重量%時,則係、〇〇5重量重量% 此處雖說是導電層的厚度,然有關本發明的導電性 粒子,由於芯材與導電層之間的界面不清楚,故以導電性 ^子的質量與使用於形成此導電性粒子的芯材用Τι〇2的質 置以及掺:的鈮量作為計算基礎,利用比表面積算出。、 要喪2導電層的厚度及組成雖藉由最後形成的導電膜所 ..凡成,但由於一般的要求範圍 :面電阻值為丨·。购/□左右〜“购/□左右,故 :成上述範圍為較佳。而將製造的難易度等列入考量的導 :層的厚度係一為更佳;銳含有率係將導電性粒: =^102量設為1〇0重量%時,則重重量% 22l3-8940-PF;Ahddub 10 200809876 有關本發明的導雷# ψν # &每^ , t , 净包性叔體的貫施例··有關本發明的導 電性粉體係以前述導雷桩私工^ ^ . 义¥电性拉子所構成的導電性粉體,前述The conductive particles are also granulated, because the conductive layer is formed by the inclusion of lanthanum Ti〇2, so the interface between the conductive layer and the core particles is unclear =: the characteristic is -° The W system in which the interface between the conductive layer and the & material is unclear, and the use of the common Ti〇2 in the core material and the conductive layer is described in detail, although it is in the atmosphere. The precursor coated with the other particles is calcined to obtain conductive particles, but the calcination is changed to a sintered state of Τ1〇2 by baking, and the adhesion between the core material and the conductive layer becomes strong, and the interface is strong. Unknown reasons. Therefore, it is generally considered that the argon-forming enthalpy of the formation of the conductive layer is performed by sharply diffusing on the side of the T i 〇 2 of the core material to complete the 电V electrical layer from the φ 甶 电 to the core layer. Concentration gradient. In the conductive particles according to the present invention, the thickness of the conductive layer is preferably 2 nm to 15 nm, and the content of the conductive layer is preferably 〇〇. 〇〇, 〇〇 5 wt% Here, although the thickness of the conductive layer, the conductive particles of the present invention, because the interface between the core material and the conductive layer is unclear, the quality and use of the conductivity The core material forming the conductive particles was calculated using the specific surface area by using the mass of the Τι 2 and the amount of enthalpy. The thickness and composition of the conductive layer are to be formed by the last formed conductive film. However, due to the general requirements: the surface resistance value is 丨·. Buy / □ around ~ "purchase / □ around, so: the above range is better. And the ease of manufacture, etc. in the consideration of the layer: the thickness of the layer is better; the sharp content is the conductive particles When the amount of ==102 is set to 1〇0% by weight, then the weight is 22l3-8940-PF; Ahddub 10 200809876 The guide ################################################################################### In the conductive powder system of the present invention, the conductive powder composed of the above-mentioned conductive piles
導電性粒子的初級粒徑俦0 R 、 杬係0.05#m〜i.0/^。有關本發明的 導電性粉體的用途’對於以導電性墨水為首的有機絕緣 體、例如塗料或塑膠薄膜等賦與導電性,若以此為目的的 話,則均勾分散性與導電性能夠並存的實施例受到要求。 而且’若由此要求特性來研究粉體的形狀,則對於導電性, 製成如專利文獻1所揭露的鱗片狀的薄片為較佳。然而, 由於缚片欠缺均勻分散松 从4 放性故右應用基於強力攪拌或長時 間攪拌的強力分散處理,則會 j曰引起v电層的剝離或薄片本 身的破壞,其結果用以得到所期待的特性之步驟設計合有 所困難。 "男 並且為了改善分散性,粒子^彡n n 言,製成呈球形、似玻开彡笙夂A门 ^ 似 &球形專各向同性的球形者為較佳。相 對於此,使形狀為非粒狀的鳞片 狀的一片狀或針狀的粒子分散之墨 水或塗料,調配成相同含量 、 里的^形,則黏度會上昇,難以 獲知塗膜的均勻性。& # i ^ 、 甘、 由此减點,導電性粒子的形狀係粒狀, 其初級粒徑比〇.〇5em還大較 ,, 、八罕乂彳土因此,導電性粒子的 =粒徑:超過U㈣’則無論形狀如何為粒狀,導電膜的 :面千=變差’同時粒子間的間隙變大,即使為了得到 、 千彳-也必須考慮塗膜厚度。又 ¥笔性粒子的初級粒徑為U心〇.‘更佳。 並且,前述導電性粉體的中位徑m。以體積基準係以 爪以下為較佳。不能'忽視如前述粒徑賦與墨水或塗料的黏 11 2213-8940-PF;Ahddub 200809876 此亦::不僅是粒徑範圍,而且也必須考慮粒捏的 求甚殷的導ϋ此觀點’特別是對於塗膜厚度的管理要 …更:墨水用途,則中位徑一積基準係〇,2 為心戶電性粉體的比表面積係im2/g〜22m2/g較佳。作 :利用後辻用# Tl°2係原來比表面積較大的原料,因此對 反的本發明的製造方法來形成導電層係採用液相 所二的·。所得到的導電性粒子的特性,受到作為芯材 有關本二的粒度或表面狀態报大的影響。因而, =的導電性粒子與導電性粉體由於發揮穩 的範l:t g〜22mVg較佳。而比表面積… 、〜17m/g ’又更佳的範圍係、7mVg〜i5mVg。 ;刖述導電性粉體,芯材粒 導電性粒子的的比表面積與所得到的 ^ )/(^ 又貝t 〔(導電性粒子的比表面 :;二材粒子的比表面積)〕係1〇〜2.〇更佳。如前述, 對於利用本發明的製造方法來 應。因而,若顯微地觀察表面,雖;;=有係、採用液相反 P战為具有凹凸形狀去, t為=揮導電性,還是需要儘可能保持平滑的表面狀 ^ u ’芯材粒子的比表面積與所得到的導電性粒子的 之比〔(導電性粒子的比表面積)/(芯材粒子的比 表面知)〕若為i.。〜2.0’則能夠確保穩定的導電性。 有關本發明的導電性粉體之製造例:有 電性粉體之製造方法,具有以下的步驟^步㈣。 步驟A係將T i 〇2粉末分散於水中 τ,而得到Ti〇2懸浮液 2213-8940-PF;Ahddub 12 200809876 的步驟,发曰 /、曰的在於消除芯材的凝聚,而使均勻地分散。 因此’此處所使用的Ti〇2粉末之粒徑係0· 05# m〜:L 〇// m, 雖浮:液中沾 心 的Ti〇2濃度係20g/L〜500g/L為較佳。所形成的 導電芦的晰旦 曰、貝夏相較於芯材的質量雖非較小,但若考慮導電 ^ 乂成於比表面積較大的芯材之外層,則作為粒徑的增加 來加以_iL曰The primary particle diameter of the conductive particles is 俦0 R and 杬 is 0.05#m~i.0/^. The use of the conductive powder of the present invention is to impart conductivity to an organic insulator such as a conductive ink, such as a paint or a plastic film. If this is the purpose, both the hook-and-scatter property and the conductivity can coexist. Embodiments are required. Further, when the shape of the powder is studied by the characteristics, it is preferable to form the scaly sheet as disclosed in Patent Document 1 for the conductivity. However, due to the lack of uniform dispersion of the tabs, the strong dispersion treatment based on strong agitation or long-time agitation may cause the peeling of the v-electrode layer or the destruction of the flakes themselves, and the result is used to obtain The design of the expected feature steps is difficult. "Men and in order to improve the dispersibility, the particles are made into a spherical shape, which is similar to the sphere of the sphere and the spherical isotropic isotropic. On the other hand, when the ink or the coating material in which the scaly-like one-piece or needle-shaped particles having a non-granular shape is dispersed is blended into the same content or in the shape of the inside, the viscosity is increased, and it is difficult to know the uniformity of the coating film. . &# i ^ , Gan, and thus the point of reduction, the shape of the conductive particles is granular, and its primary particle size is larger than that of 〇.〇5em, and, as is the case of Bahanan, the conductive particles = Diameter: Exceeding U(four)', no matter how the shape is granular, the surface of the conductive film: surface is reduced, and the gap between the particles becomes large. Even in order to obtain, the thickness of the coating film must be considered. Also ¥ The primary particle size of the pen particles is U heart 〇. ‘More. Further, the median diameter m of the conductive powder. Preferably, the volume is based on the following jaws. Can't neglect the adhesion of ink or paint as mentioned above. 11 2213-8940-PF; Ahddub 200809876 This is also: not only the particle size range, but also must be considered in the opinion of the grain pinch. It is for the management of the thickness of the coating film. Further, for the ink application, the median diameter is a reference system, and the specific surface area of the electro-mechanical powder is preferably im2/g to 22 m2/g. For the use of #Tl°2, the raw material having a large specific surface area is used. Therefore, in the production method of the present invention, the conductive layer is formed by using a liquid phase. The properties of the obtained conductive particles are affected by the particle size or surface state of the core material. Therefore, it is preferable that the conductive particles of = and the conductive powder exhibit a stable range of 1: t g to 22 mVg. The specific surface area..., ~17 m/g ′ is more preferably in the range of 7 mVg to i5 mVg. Describing the conductive powder, the specific surface area of the core particle conductive particles and the obtained ^ ) / (^ t t ( [(specific surface of the conductive particles: specific surface area of the two particles)] Preferably, as described above, the manufacturing method according to the present invention is applied. Therefore, if the surface is observed microscopically, there is a system, and the liquid is opposite to the P-type having a concave-convex shape, t is = Conductivity, or need to maintain a smooth surface as much as possible ^ u 'The ratio of the specific surface area of the core particles to the obtained conductive particles [(specific surface area of conductive particles) / (specific surface area of core particles) In the case of the conductive powder of the present invention, the method for producing the conductive powder of the present invention has the following steps (4). The T i 〇 2 powder is dispersed in water τ to obtain a Ti 〇 2 suspension 2213-8940-PF; Ahddub 12 200809876, the enthalpy / enthalpy is to eliminate the aggregation of the core material, and to uniformly disperse. Therefore, the particle size of the Ti〇2 powder used here is 0· 05# m~:L 〇// m Although floating: the concentration of Ti〇2 in the liquid is preferably 20g/L~500g/L. The quality of the formed conductive reeds is not small compared to the quality of the core material, but if Considering that the conductive layer is formed on the outer layer of the core material having a larger specific surface area, it is added as an increase in the particle size.
山地考$之必要性甚小,此處所調製的芯材的粒 仅可Μ為大致和導電性粒子的粒徑一樣。因而,芯材的粒 /可大致和作為目的的導電性粒子的粒徑一致。又粒徑的 耗圍係考慮使用前述的導電性粉體所得到的墨水等的黏 度、塗膜的遮蔽性來加以決定。並且,懸浮液中的Ti〇2濃 又(水料/辰度)主要考慮生產性與導電性粒子的特性來加以 、疋例如,右漿料濃度太高,則粒子之間容易凝聚致分 政性變差;若漿料濃度太低,則芯材與導電層之間的黏附 性有減低的趨勢。由此觀點,漿料濃度的幻艮靠《5〇〇g/L 車乂 k、更佳的上限濃度係3〇〇g/L。艮㈤2〇Μ也是能 夠維持工業的生產性之漿料濃度。 / Μ Ί丁到日q g』…一心q队τ雄刀口銥鹽盥 錕鹽’並加以溶解來準備反應用液之步驟,係對芯材表面 所形成的導電膜的膜厚及銳摻入量加以設定的步驟… 而言,所使用的鈦鹽係由水溶抖 一版 印扒岭性鈦鹽的硫酸鈦醯、四氯化 鈦、硫酸鈦、四氟化鈦等之中 、 予您中所迭擇的1種或2種以上, 將鈦濃度調配成1重量%〜3 〇會吾。/兔鈐 刊重里/。為較佳。此鈦鹽的 量,相對於漿料濃度,為了達丨 — 1違到所s又疋者,以重量%來管理 較佳。此處所使用的鈦鹽若9 k α ^ -右疋水溶性,則可為任何—種, 2213-8940-PF;Ahddub 13 200809876 可使用硫酸㈣、^化鈦、硫酸鈦 濃度係將芯材表面所形成的導電層厚度設定於最適的产 度。亦即在形成厚導電層的情形可調配成高濃度 ’辰 成薄導電層的情形可調配成低濃度。 人 形 選擇的^種或2種以上,峨可調配成二^The necessity of the mountain test is very small, and the particles of the core material prepared here can only be roughly the same as the particle size of the conductive particles. Therefore, the particle/core of the core material can substantially coincide with the particle diameter of the intended conductive particle. The consumption of the particle size is determined in consideration of the viscosity of the ink or the like obtained by using the conductive powder described above and the shielding property of the coating film. Moreover, the concentration of Ti〇2 in the suspension (water/density) is mainly considered in consideration of the properties of the productive and conductive particles, for example, if the concentration of the right slurry is too high, the particles are easily condensed to cause division. The property is poor; if the slurry concentration is too low, the adhesion between the core material and the conductive layer tends to decrease. From this point of view, the illusion of the slurry concentration depends on "5 〇〇 g / L 乂 k, a better upper limit concentration of 3 〇〇 g / L.艮(5)2〇Μ is also a slurry concentration that can maintain industrial productivity. / Μ 到 到 to the day qg 』... One heart q team τ 刀 刀 铱 铱 salt salt ' salt and dissolved to prepare the reaction liquid step, the film thickness and sharp incorporation of the conductive film formed on the surface of the core material Steps to be set... In terms of the titanium salt, the titanium salt of titanium sulfate, titanium tetrachloride, titanium sulfate, titanium tetrafluoride, etc. One or two or more kinds of the selected ones, and the titanium concentration is adjusted to 1% by weight to 3 〇. / Rabbit 钤 重 重 /. It is better. The amount of the titanium salt, relative to the concentration of the slurry, is preferably managed in a weight % in order to achieve a 丨-1 violation. The titanium salt used herein may be any type if it is water-soluble, and may be any type, 2213-8940-PF; Ahddub 13 200809876 may use a sulfuric acid (tetra), titanium oxide, titanium sulfate concentration system to coat the surface of the core material. The thickness of the formed conductive layer is set to an optimum yield. That is, in the case where a thick conductive layer is formed, a high concentration of a thin conductive layer can be adjusted to a low concentration. Human form Selecting 2 species or more, 峨 can be adjusted into two ^
'耳。此處所使用的鈮鹽若是與鈦鹽同樣的水溶性 可為任何-種,可使用五氯化銳、五氟化錕、五硬化、 而銳濃度係對芯材表面所形成的導電層之摻人量設定於田 適的浪度。亦即在摻人量多的情形可調配成高濃度、而在 摻入量少的情形可調配成低濃度。 —步驟C係將步驟Β所準備的反應麵周整於中性〜鹼性 :圍’使摻入銳的Ti〇2前驅物(主要係氯氧化物)析出,而 侍到包含摻入鈮的Ti〇2前驅物塗布之Μ粒子的懸浮液之 步驟’係於芯材的Ti〇2表面形成均勻的摻入鈮的Ti〇2前驅 物的析出膜之牛_ θ — " 艇之步驟。具體而言,為了將調製後的ΡΗ調成 7〜11的中性〜驗性範圍,則可使用由、K0H、Na2C〇3或 心強驗之中作選擇的i種或2種以上來調整pH。由於此 步驟成為懸浮液的形態之反應,故加上攪拌操作為較佳。 此步驟C要注意至完成鹼的添加為止所需的時間,具 體而言,設為1。分鐘〜90分鐘較佳。後述的實施例需;〇 分鐘。例如,作為簡明的例子,料進行步驟β與步驟c 的狀況亦即右於使芯材分散的懸浮液中,同時添加欽鹽、 、里及鹼,則在反應液中的鈦鹽或鈮鹽與鹼的接觸狀態下 2213-8940-PF;Ahddub 14 200809876 會產生斑點,欲形成均句的Tl〇2前驅物是有所困難。 又若於使芯材分散的懸浮液中先添加鹼之後,再添加 欽鹽、铌鹽,則係於芯材I面形成的㈣層之㈣前驅物’ 形成多孔的狀態而成為脆弱的物質,則使用導電性粉末於 導電性塗料時,會成為導電性不良的塗料。 步驟D係對步驟f/ 斤仔到的懸洋液施行固液分離,並 將刀取的摻人鈮的了1〇2前驅物塗布之Ti()2|末加以乾燥,'ear. The cerium salt used herein may be any water-soluble salt of the same type as the titanium salt, and may be used as a pentachloride, a lanthanum pentafluoride or a five-hardening, and a sharp concentration is added to the conductive layer formed on the surface of the core material. The amount of people is set in the wave of Tian Shi. That is to say, in the case of a large amount of people, it can be adjusted to a high concentration, and in the case of a small amount of incorporation, it can be adjusted to a low concentration. - Step C is to complete the reaction surface prepared in step 于 to neutral ~ alkaline: surrounding 'precipitate the incorporation of sharp Ti 〇 2 precursor (mainly oxychloride), and serve to contain bismuth The step of suspending the ruthenium particles coated with the Ti〇2 precursor is carried out on the surface of Ti〇2 of the core material to form a uniform precipitate of the ruthenium-doped Ti〇2 precursor. Specifically, in order to adjust the adjusted enthalpy to a neutral-to-experimental range of 7 to 11, it is possible to adjust by using one or two or more types selected from K0H, Na2C〇3, or cardiac strength test. pH. Since this step becomes a reaction of the form of the suspension, it is preferred to add a stirring operation. In this step C, attention is paid to the time required to complete the addition of the base, and specifically, it is set to 1. Minutes ~ 90 minutes are preferred. The embodiment described later is required; 〇 minutes. For example, as a concise example, the conditions of step β and step c are carried out, that is, in the suspension which is dispersed in the core material, and the salt or strontium salt in the reaction liquid is added at the same time. 2213-8940-PF in contact with alkali; Ahddub 14 200809876 will produce spots, and it is difficult to form a Tl〇2 precursor of a uniform sentence. Further, when a base is added to the suspension in which the core material is dispersed, and then a salt or a cerium salt is added, the (four) precursor of the (four) layer formed on the surface of the core material forms a porous state and becomes a fragile substance. When a conductive powder is used for a conductive coating material, it becomes a coating material with poor conductivity. Step D is to perform solid-liquid separation on the suspension liquid of step f/jin, and dry the Ti()2| coated with the ruthenium-doped precursor of the ruthenium.
而得到摻入銳的Tl〇2前驅物塗布之Μ粉末的步驟,可施 行通用的方法之清洗、_ H /驟Ε係將步驟D所得到的摻人铌的TiG2前驅物塗布 之Μ粉餅加以粉碎之後,於大氣環境下施行培燒而得到 導電性粉體之步驟,係將步驟Β所形成的摻入銳的Tl〇2前 驅物層作成氧化物之步、驟。於此步驟中銳被換入於下他, 而毛揮預期的4寸性。對於粉體的粉碎可使用加壓 統方法的粉碎設備。而在户声 4傳 隹大口垸之除的裱境,本發明係設為 孔::'。-般認為此係Ti〇2前驅物層的主成分為氫氧化 進仃基於加熱的脫水反應,則可發揮充分的效果。 有關本叙明的導電性墨水的實施例 電性墨水係傕用俞、^ ^ V 昭 使“述導電性粉體作為顏料者,係黏度亦依 :取適切的調製者。此處所得到的導電性墨水由於 性粉體的情形相較, _ 、衣成墨水的導電性粒子的固體成分較 :水二',即使所欲形成的導電膜厚度相同,然所使用的 基於有機溶劑等對環境的影響也會減低。 2213-8940^PF;Ahddub ^ 200809876 有關本u的導電性粉體之用途並不限於導電性墨水, 亦能夠使用於前述的導電性塗料或對塑膠賦與導電性之目 的0 以下雖顯示實施例與比較例,但本發明並不受這些例 子所限定、解釋。有關以實施例與比較例所調製的導電性 粕體或V包性墨水之調製方法,係利用以下所述的實施例 二比車又例來個別加以說明,並將導電性墨水的分散時間和The step of obtaining the ruthenium powder coated with the sharp Tl〇2 precursor can be carried out by a general method of cleaning, and the ruthenium-doped TiG2 precursor-coated glutinous powder cake obtained in the step D is used. After the pulverization, the step of performing calcination in an atmosphere to obtain a conductive powder is a step of forming an oxide by forming a sharp T1〇2 precursor layer formed by the step Β. In this step, Rui was replaced by the next one, and the hair was expected to be 4 inches. For the pulverization of the powder, a pulverizing apparatus using a pressurization method can be used. In the dilemma of the division of the household voice, the invention is set to the hole::'. It is generally considered that the main component of the Ti〇2 precursor layer is hydrogen hydroxide. The heating-based dehydration reaction can exert a sufficient effect. Regarding the conductive ink system of the present embodiment, the electric ink system is used for the purpose of "the conductive powder is used as the pigment, and the viscosity is also dependent on: the appropriate modulation is obtained. The conductivity obtained here. The ink of the conductive ink is compared with the case of the powder, and the solid content of the conductive particles of the ink is better than that of the water: even if the thickness of the conductive film to be formed is the same, the organic solvent or the like is used for the environment. The effect is also reduced. 2213-8940^PF;Ahddub ^ 200809876 The use of the conductive powder of this u is not limited to conductive ink, and can also be used for the above-mentioned conductive paint or for the purpose of imparting conductivity to plastics. Although the examples and the comparative examples are shown below, the present invention is not limited by these examples, and the method for preparing the conductive quinone or V-encapsulated ink prepared by the examples and the comparative examples is as follows. The second embodiment is described separately from the vehicle, and the dispersion time of the conductive ink is
導電膜的表面電阻數據的結果表示於第i表。f 1圖係將 运些數據作成圖表。第丨表係揭冑,以使用基於本發明所 形成的導電性粉體所製成的導電膜作為實施例1;而比較 用者係以使用氧化錫來形成導電層、並使用以此導電層所 形成的導電性粉體而製成的導電膜作為比較例J。 第1表The results of the surface resistance data of the conductive film are shown in the i-th table. The f 1 map will be used to chart these data. The third embodiment discloses that a conductive film made of the conductive powder formed based on the present invention is used as the embodiment 1; and the comparative user uses tin oxide to form a conductive layer and uses the conductive layer. A conductive film made of the formed conductive powder was used as Comparative Example J. Table 1
〔導電性粉體的調製〕 1 ·使用樂品的調整 鈦鹽溶液··使用硫酸鈦醯,調整至5重量%作為鈦份 銳鹽溶液:溶解五氯化銳3g於1 OOmL的濃鹽酸中加以 調整 PH調整用溶液:氫氧化鈉25重量%的水溶液 2 ·導電層的形成 2213~8940-PF;Ahddub 16 200809876[Preparation of conductive powder] 1 - Adjusting the titanium salt solution using the music product · Using titanium sulphate, adjust to 5% by weight as a titanium salt solution: Dissolve 5 g of pentachloride in 100 mL of concentrated hydrochloric acid Adjust the pH adjustment solution: 25 wt% aqueous solution of sodium hydroxide 2 · Formation of conductive layer 2213~8940-PF; Ahddub 16 200809876
- 添加初級粒徑^^^^的Ti〇2粉末100g於純水15L 中,而得到Ti〇2粉末分散的懸浮液。添加鈦鹽溶液4〇〇g 與鈮鹽溶液2〇ffiL於此懸浮液,調製成反應用液。將如此施 行所製出的反應用液昇溫至6(TC,經7〇分鐘添加pH調整 用溶液350mL。將此處所得到的懸浮液再攪拌3〇分鐘維持 後利用再製漿法,施予清洗,最後使用吸據器進行吸引 過濾,分取固體成分並加以乾燥,而得到假固化的粉體。 _ 3.導電性粉體的形成 其次,使用加壓磨機將乾燥而假固化的粉體加以粉 碎,於70(TC的大氣環境中培燒!小時,而得到形成⑽ 導電層的導電性粉體,此Ti〇2導電層係在Ti〇2粉末中摻入 鈮。 4·導電性粉體的評估 粒徑· 0. 15 μ m(由倍率60, 〇〇〇倍的SEM—掃描式電子 顯微鏡觀察像之中任意選擇的50點之粒徑的平均) • 2〇〇mL的試樣容器中稱取試樣約〇.lg, 混合0· 2g/L的六偏磷酸鈉i〇mL之後添加純水9〇mL,使用 超音波分散機〔日本精機(股份)製us—3〇〇τ〕並分散ι〇 分鐘,以調製試樣懸浮液。利用(股份)堀場製造廠製Μ — 920、藉由激光繞射散射法對該試樣懸浮液所求得的累積體 積達到50%的時點之粒徑} 比表面積:芯材係10· 0mVg、導電性粉末係 11.6m2/g(以BET—布·埃·泰方法加以測定) L值:96.9 {以色差測定器〔K〇NICA min〇lta 2213-8940-PF;Ahddub 17 200809876 ftOUUNGsC股份)製⑽―35〇〇d〕來測定色調) 其二欠’導電層的厚度係利用以下的步驟以計算求得。 a) 由所得到的導電性粉末的質量與所使用的芯材的質 量來求得塗膜部分的質量。 b) 藉由將塗膜質量除以氧化鈦的密度,再除以上述所 付到的芯材的表面積,以求得塗膜厚度(導電層厚度:nm)。 c) 由$電性粉末所包含的鈮的分析值來求得鈮摻入量 U)。 此結果係導電層厚度約為8nm,相對於導電性粒子全 部的Tl02量1〇0重量%,則導電層的質量厚度係25重量% ; 將導電性粒子全部的Ti〇2量設& 1〇〇重量%時,則銳換入 ΐ係〇·2重量% ;將導電層的量設為1〇〇重量%時,則 鈮摻入量係〇 · 8重量%。 〔導電性墨水的調製〕 1. 於容量5〇cc的容器中加入導電性粉末74ig與丙稀 •酸樹脂〔MITSUBISHIRAY0NC0·,ltd.(股份礓似隐⑶ -167〕6.41g、並使用甲苯—丁醇混合液作為溶劑,加以 混合使導電膜形成後的導電粒子含有率成為7〇%。 2. 其次,添加玻璃珠粒料於前述混合物中,使用塗料 振動器施行1小時、2小時、3小時、4小時、以及5小時 的分散處理,而得到導電性墨水丨〜導電性墨水5。 〔塗膜的形成〕 利用刮條塗布 使用上述導電性墨水〗〜導電性墨水 機(# 10)於PET薄膜上形成塗膜。 2213-8940-PF;Ahddub 18 200809876 • 〔評估結果〕 將前述塗膜以設定於80它的熱風循環式烘箱乾燥3〇 分鐘後,使用〔三菱化學(股份)製HIRESTA IP來進行表面 %阻的評話。結果如第1表所示。使用分散時間設為5小 時的導電性墨水5所形成的導電膜的表面電阻值,不過是 使用分散時間1小時的導電性墨水i所形成的導電膜的表 面電阻值之33倍,分散時間的長時間化的影響小,甚為良 •好。 θ " 【比較例1】 〔導電性粉體的調製〕 1 ·導電層的形成 添加與在實施例1所使用者相同的Ti〇2粉末9〇〇g於 純水5L中,而得到τi〇2粉末分散的懸浮液。於此懸浮液 中添加錫酸鈉三水合鹽930g,並添加純水使全部的液量成 為8L。將如此施行所製出的反應用液昇溫至7〇<t,維持 鲁60分鐘後,經90分鐘添加20%硫酸1_6L。將此處所得到 的懸浮液再攪拌30分鐘維持後,利用再製漿法,施予清 洗,最後使用吸濾器進行吸引過濾,分取固體成分並加以 乾燥,而得到在Ti〇2上塗布Sn〇2的粉體。 2·導電性粉體的形成 其次,使用加壓磨機將乾燥而假固化的粉體加以粉 碎,對此粉體於700°C的還原環境(2%H2— I)中焙燒1小時。 3 ·導電性粉體的評估 對於以下的項目,使用與實施例1同樣的評估方法。 2213-8940-pp;Ahddub 19 200809876 粒徑·· 〇· 15μ m ^50 · 〇. 8 // m 比表面積:芯材係1〇 〇mVg、導電性粉末係25 imVg L 值:85· 3 /、-人,導電層的厚度係利用以下的計算而求得。 曰 A戶斤得到的$電性粉末的質量與芯材所使用的了」& 置來求得導電層的質量厚度。 ^藉由將塗膜貝里除以氧化錫的密度,再除以上述所 亍】的心材的表面積,以求得塗膜厚度(導電層厚度··⑽)。 〇將導電性粉末中的錫等級換算為Sn〇2質量,以求得 Sn〇2塗膜部分的質量厚度(%)。 此結果係導電層厚度約為8隨,相對於換算為⑽之 =生粒子全部的了1()2量i⑽重量%,則導電 度係35重量%。 、i + 〔導電性墨水的調製〕 利用與實施例1同樣的摔 作以鈿仃分散處理,而得到 V電性墨水Γ〜導電性墨水5,。 〔塗膜的形成〕 與實施例1同樣地施行。 〔評估結果〕 與實施例1同樣地施行# Η、繁】本邮-電阻的評估。結果如第1 圖、弟1表所不。使用分散時 /, 间σ又為5小時的墨水5,所 形成的導電膜的表面電阻值, η 上幵至使用分散時間彳小卑 的墨水Γ所形成的導電膜的* ^ 的表面電阻值之120,000倍, 2213-8940-PF;Ahddub 20- 100 g of Ti〇2 powder having a primary particle size of ^^^^ was added to 15 L of pure water to obtain a suspension in which Ti〇2 powder was dispersed. 4 〇〇g of a titanium salt solution and 2 〇ffi of a cerium salt solution were added to prepare a reaction liquid. The reaction solution prepared in this manner was heated to 6 (TC, and 350 mL of the pH adjustment solution was added over 7 minutes. The suspension obtained here was stirred for further 3 minutes, and then washed by a repulping method. Finally, the suction filter is used for suction filtration, and the solid component is separated and dried to obtain a pseudo-cured powder. _ 3. Formation of conductive powder Next, dry and pseudo-cured powder is used using a pressure mill. It is pulverized and fired in an atmosphere of 70 (TC) for an hour to obtain a conductive powder which forms a (10) conductive layer which is doped with lanthanum in the Ti〇2 powder. Evaluation of particle size · 0. 15 μ m (average of 50-point particle size of arbitrarily selected image by SEM-scanning electron microscope with magnification of 60, 〇〇〇) • Sample of 2〇〇mL Weigh the sample about 〇.lg in the container, mix 0·2g/L sodium hexametaphosphate i〇mL, add 9〇mL of pure water, and use ultrasonic dispersion machine [Japan Seiki (share) system us-3〇〇 τ] and disperse 〇 〇 minutes to prepare the sample suspension. Use (share) market manufacturing plant — 920. Particle size at a time when the cumulative volume of the sample suspension is 50% by laser diffraction scattering method} Specific surface area: core material 10·0 mVg, conductive powder system 11.6 m2/g ( Measured by the BET-Beauty method) L value: 96.9 {Measured by color difference measuring device [K〇NICA min〇lta 2213-8940-PF; Ahddub 17 200809876 ftOUUNGsC shares) (10)-35〇〇d] Hue) The thickness of the two underlying conductive layers was calculated by the following procedure. a) The mass of the coating film portion was determined from the mass of the obtained conductive powder and the mass of the core material used. b) The coating film thickness (conductive layer thickness: nm) was determined by dividing the coating film mass by the density of titanium oxide and dividing by the surface area of the above-mentioned core material. c) The amount of cerium incorporation is determined from the analytical value of cerium contained in the electrical powder. The result is that the thickness of the conductive layer is about 8 nm, and the mass thickness of the conductive layer is 25% by weight with respect to the total amount of T1O2 of the conductive particles, and the mass thickness of the conductive layer is 25% by weight. When the weight is 5%, the enthalpy is 2% by weight, and when the amount of the conductive layer is 1% by weight, the amount of cerium is 8% by weight. [Preparation of Conductive Ink] 1. Add conductive powder 74ig and acrylic acid resin (MITSUBISHIRAY0NC0·,ltd.) to 6.41g of a container with a capacity of 5〇cc and use toluene. The butanol mixture was mixed as a solvent, and the content of the conductive particles after the formation of the conductive film was 7%. 2. Next, glass beads were added to the mixture, and the paint shaker was used for 1 hour, 2 hours, and 3 hours. The conductive ink 丨 to the conductive ink 5 were obtained by dispersion treatment in an hour, 4 hours, and 5 hours. [Formation of Coating Film] The above-mentioned conductive ink 〖to conductive ink machine (# 10) was applied by a bar coating. A coating film was formed on the PET film. 2213-8940-PF; Ahddub 18 200809876 • [Evaluation Result] The coating film was dried in a hot air circulating oven set at 80 for 3 minutes, and then used [MITSUBISHI Chemical Co., Ltd.) IP was used to evaluate the surface % resistance. The results are shown in Table 1. The surface resistance value of the conductive film formed by using the conductive ink 5 having a dispersion time of 5 hours was used, but the dispersion time was 1 hour. The surface resistivity of the conductive film formed by the conductive ink i is 33 times, and the influence of the long-term dispersion time is small, which is good and good. θ " [Comparative Example 1] [Modulation of conductive powder] 1 - Formation of a conductive layer: 9 〇〇g of the same Ti〇2 powder as in the user of Example 1 was added to 5 L of pure water to obtain a suspension in which τi〇2 powder was dispersed. Sodium stannate was added to the suspension. 930 g of trihydrate salt was added, and pure water was added to make the total amount of liquid 8 L. The reaction liquid prepared in this manner was heated to 7 Torr < t, and after maintaining for 60 minutes, 20% sulfuric acid 1-6 L was added over 90 minutes. After the suspension obtained here was further stirred for 30 minutes, it was subjected to washing by a repulping method, and finally suction filtration was carried out using a suction filter, and the solid component was separated and dried to obtain a coating of Sn on Ti〇2. Powder of 2. 2. Formation of conductive powder Next, the dried and pseudo-cured powder was pulverized using a pressure mill, and the powder was in a reducing environment (2% H 2 - I) at 700 ° C. Roasting for 1 hour. 3 · Evaluation of conductive powder for the following items The same evaluation method as in Example 1. 2213-8940-pp; Ahddub 19 200809876 Particle size · · 〇 · 15μ m ^50 · 〇. 8 // m Specific surface area: core material 1〇〇mVg, conductive powder system 25 imVg L value: 85·3 /, - person, the thickness of the conductive layer is obtained by the following calculation. 曰A household weight of the electric powder and the core material used "& The thickness of the conductive layer was determined. The coating film thickness (the thickness of the conductive layer (10)) was determined by dividing the coating film by the density of tin oxide and dividing the surface area of the above-mentioned core material. 〇 The tin level in the conductive powder was converted to Sn 〇 2 mass to determine the mass thickness (%) of the Sn 〇 2 coating film portion. As a result, the thickness of the conductive layer was about 8 and the conductivity was 35% by weight with respect to (10) = the total amount of 1 () 2 i (10)% by weight of the green particles. i + [Preparation of Conductive Ink] The V-electric ink Γ to the conductive ink 5 were obtained by the same treatment as in Example 1 by the enthalpy dispersion treatment. [Formation of Coating Film] The same procedure as in Example 1 was carried out. [Evaluation Result] In the same manner as in the first embodiment, the evaluation of the mail-resistance was carried out. The results are as shown in Figure 1 and Table 1. When the ink 5 which is dispersed/, and the interval σ is 5 hours, the surface resistance value of the formed conductive film, η is increased to the surface resistance value of the conductive film formed by the ink enthalpy of the dispersion time. 120,000 times, 2213-8940-PF; Ahddub 20
200809876 相較於使用實施例所得到的墨水 5倍。 所形成的導電膜,約為 〔200809876 is 5 times better than the ink obtained using the examples. The formed conductive film is about [
實施例與比較例的對 一邊參照第1表, 各種數據,來進行實 比〕 邊參照以實施例舆比較例所得到 施例與比較例的對比。 +由第1表可瞭解,使用以有關本發明的實施例1的導 “生拉子所構成的導電性粉體所得到的導電性墨水,相對 2比較例卜分散時間的影#較小,而得料電 結果。 〜旧 產業上可利用性: 有關本發明的導電性粒子之凝聚體,使用係此種凝聚 體的導電性粉體作為填料的導電性墨水、導電㈣ 與導電性的塑冑’係-方面具明色一方面具遮蔽性,並且 有穩定的導電性者。 /、 【圖式簡單說明】 所得到的導 第1圖係表示改變導電性墨水的分散時間 電膜的表面電阻之圖。 【主要元件符號說明】 益 〇 0、Λ 2213-8940-PF;Ahddub 21The comparison between the examples and the comparative examples was made with reference to the first table and various data, and the comparison between the examples obtained in the comparative examples and the comparative examples was made. + It is understood from the first table that the conductive ink obtained by using the conductive powder composed of the raw material of the first embodiment of the present invention is smaller than the dispersion time of the comparative example. In the case of the aggregate of the conductive particles of the present invention, the conductive powder using the conductive powder of the aggregate as a filler, the conductive ink, the conductive (four), and the conductive plastic are used.胄 ' Department - aspect has a clear color on the one hand, and has a stable conductivity. /, [Simple diagram of the diagram] The obtained diagram 1 shows the surface of the electro-film that changes the dispersion time of the conductive ink. Diagram of resistance. [Key component symbol description] 益〇0, Λ 2213-8940-PF; Ahddub 21
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