JPH06183733A - Electric conductive white powder and it production - Google Patents
Electric conductive white powder and it productionInfo
- Publication number
- JPH06183733A JPH06183733A JP35368792A JP35368792A JPH06183733A JP H06183733 A JPH06183733 A JP H06183733A JP 35368792 A JP35368792 A JP 35368792A JP 35368792 A JP35368792 A JP 35368792A JP H06183733 A JPH06183733 A JP H06183733A
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- Prior art keywords
- antimony
- tin
- compound
- oxide
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は改良された酸化アンチモ
ン含有酸化錫白色導電性微粉末とその製造方法に関す
る。更に詳しくは、色味の無い無色透明な導電性塗布膜
を形成する充填材としての酸化アンチモン含有酸化錫微
粉末の製造方法に関する。酸化アンチモン含有酸化錫粉
末に酸化アンチモンがドープされたセラミックは１〜７
０Ω・ｃｍの比抵抗の良好な導電性を有し、特に湿度の
影響を受けない性質のある導電性粉末として広く実用さ
れている。中でも樹脂の中に充填されて成形体や塗布膜
に導電性を付与し、記録フィルムや光磁気ディスク用の
帯電防止透明膜、半導体クリーンルームパネル等とし
て、利用され、その他触媒、センサー等にも利用されて
いる。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an improved antimony oxide-containing tin oxide white conductive fine powder and a method for producing the same. More specifically, it relates to a method for producing tin oxide fine powder containing antimony oxide as a filler for forming a colorless and transparent conductive coating film having no tint. Ceramics in which antimony oxide-doped tin oxide powder is doped with antimony oxide are 1 to 7
It is widely used as a conductive powder having good conductivity with a specific resistance of 0 Ω · cm and not being affected by humidity. Among them, it is filled in resin to give conductivity to molded products and coating films, and is used as antistatic transparent film for recording films and magneto-optical disks, semiconductor clean room panels, etc., and also used for catalysts, sensors, etc. Has been done.
【０００２】[0002]
【従来技術および問題点】酸化アンチモン含有酸化錫粉
末を充填材として透明導電性シートとするときは、１〜
５μｍの薄い皮膜に形成するので、粒径は可視光の波長
の半分の０．２μｍ以下（好ましくは０．１μｍ以下）
の球形の形状であり、微細かつ均一で分散性と導電性に
優れていなければならない。また一般に、酸化錫に良い
導電性を付与するために、酸化アンチモンを添加（ドー
プ）するのであるが、添加量は概ね酸化アンチモンとし
て１〜３０ｗｔ％、望ましくは５〜２０ｗｔ％の範囲に
ある。しかしながら、ドープ量が増加するに従い、粉末
の色味に青味が増加する傾向にあり、透明性導電性シー
トの使用特性および外観からも色味を抑制し、無色化
（白色化）もしくはそれに近い物である事が望ましい。2. Description of the Related Art When using a tin oxide powder containing antimony oxide as a filler to form a transparent conductive sheet,
Since it forms a thin film of 5 μm, the particle size is 0.2 μm or less (preferably 0.1 μm or less), which is half the wavelength of visible light.
It must be fine, uniform, and excellent in dispersibility and conductivity. Further, generally, in order to impart good conductivity to tin oxide, antimony oxide is added (doped), but the addition amount is generally in the range of 1 to 30% by weight, preferably 5 to 20% by weight as antimony oxide. However, as the amount of dope increases, the tint of the powder tends to increase, and the tint is suppressed from the viewpoint of the use characteristics and appearance of the transparent conductive sheet, and it becomes colorless (whitened) or close to it. It is desirable to be a thing.
【０００３】その製造は、Ｓｎ（IV）イオンおよびＳｂ
（III）イオンを含む水溶液、一般的には塩化第二錫
（ＳｎＣｌ4）と塩化第一アンチモン（ＳｂＣｌ3）の塩
酸酸性溶液から、アルカリ溶液の添加により中和して共
沈して得られる水酸化物沈殿を水で洗浄した後、固液を
分離し、乾燥、焼成する方法によっている。乾燥、焼成
は沈殿物をトレーに移してバッチ式加熱炉内で加熱する
か、コンベアに載せて連続加熱装置により加熱する。冷
却後粉砕して粉末とし、フルイ分けするのが一般に行わ
れている。The production of Sn (IV) ions and Sb
(III) Ion-containing aqueous solution, generally obtained by neutralizing and coprecipitating from an acidic hydrochloric acid solution of stannic chloride (SnCl 4 ) and stannous antimony (SbCl 3 ) by adding an alkaline solution After washing the hydroxide precipitate with water, the solid-liquid is separated, dried and fired. For drying and firing, the precipitate is transferred to a tray and heated in a batch type heating furnace, or placed on a conveyor and heated by a continuous heating device. After cooling, it is generally pulverized into powder and then sifted.
【０００４】色味を抑えた酸化錫系微粉末の製造方法と
して例えば特公昭62-1574 には、ｐＨ１０以上のアルカ
リ水溶液を６５℃以上に保ちながら、この溶液に塩化錫
溶液を加えて沈殿を生成させ、最終的にｐＨ５〜１に保
つ事によって微細な沈殿を得て、これを洗浄、乾燥後還
元性雰囲気または不活性雰囲気中で、３５０〜７００℃
の温度で焼成する事からなる低電気抵抗酸化錫微粉末の
製造方法が開示されている。しかし、この方法によって
製造された酸化錫微粉末は色味はよいが、導電性におい
て１００Ω・ｃｍ以下の低抵抗粉体は得ることが困難で
しかも、還元の度合いによっては酸化安定性に欠けると
いう問題があった。As a method for producing tin oxide fine powder with suppressed tint, for example, in Japanese Examined Patent Publication No. 62-1574, a tin chloride solution is added to this solution while keeping an alkaline aqueous solution having a pH of 10 or more at 65 ° C. or more to cause precipitation. A fine precipitate is obtained by finally producing it and maintaining it at pH 5 to 1, washing it, drying it, and then 350 to 700 ° C. in a reducing atmosphere or an inert atmosphere.
There is disclosed a method for producing a tin oxide fine powder having a low electric resistance, which comprises firing at a temperature of. However, although the tin oxide fine powder produced by this method has a good tint, it is difficult to obtain a low resistance powder having an electrical conductivity of 100 Ω · cm or less, and further, it lacks oxidative stability depending on the degree of reduction. There was a problem.
【０００５】[0005]
【課題解決の手段】本発明は前記した従来技術の問題点
を解消し、白色度が高く、色味を抑えた、しかも分散良
好な導電性微粉末を提供することを目的としている。上
記目的を達成するため、鋭意研究を行った結果、本発明
者等は酸化アンチモンドープ酸化錫へ第３元素としてア
ルミニウム、リン、モリブデン、タングステンを含有さ
せる事で問題が解決する事を見出した。SUMMARY OF THE INVENTION It is an object of the present invention to solve the above-mentioned problems of the prior art, and to provide a conductive fine powder having high whiteness, suppressed tint and good dispersion. As a result of earnest studies to achieve the above object, the present inventors have found that the problem can be solved by adding aluminum, phosphorus, molybdenum, and tungsten as the third element to antimony oxide-doped tin oxide.
【０００６】[0006]
【発明の構成及び限定理由】本発明はアルミニウム、リ
ン、モリブデン、タングステンを合計で、０．１〜７ｗ
ｔ％、酸化アンチモンを３〜３０ｗｔ％含有し、残りが
酸化錫である粒径０．２μｍ以下の白色導電性粉末を提
供する。Structure of the invention and reason for limitation In the present invention, the total amount of aluminum, phosphorus, molybdenum and tungsten is 0.1 to 7 w.
Provided is a white conductive powder containing t%, antimony oxide in an amount of 3 to 30 wt%, and the balance being tin oxide and having a particle size of 0.2 μm or less.
【０００７】本発明はまた、水溶性の錫化合物とアンチ
モン化合物の共存する混合水溶液とアルカリ水溶液とを
混和し、中和して水酸化物を沈殿させる製造方法におい
て、水溶性のアルミニウム化合物、リン化合物、モリブ
デン化合物、タングステン化合物の１種を混和し水酸化
物を沈殿させた後、該水酸化物を洗浄、乾燥、焼成、粉
砕し０．２μｍ以下の平均粒径を有する酸化アンチモン
含有酸化錫微粉末の製造方法を提供する。The present invention also provides a water-soluble aluminum compound, a phosphorus compound, in a production method of mixing a water-soluble tin compound and an antimony compound coexisting mixed aqueous solution and an alkaline aqueous solution to neutralize and precipitate a hydroxide. A compound, a molybdenum compound, or a tungsten compound, which is mixed to precipitate a hydroxide, and the hydroxide is washed, dried, fired, and pulverized to obtain an antimony oxide-containing tin oxide having an average particle diameter of 0.2 μm or less. A method for producing a fine powder is provided.
【０００８】本発明において水溶性化合物とは、金属の
塩および金属を酸根部に含む酸素酸またはその塩を意味
する。酸化アンチモンの添加量は１〜３０ｗｔ％で、１
ｗｔ％未満であると色味は低下するが、導電性は不足す
る。また３０ｗｔ％を越えても導電性は変らず、青味が
増加する。第３元素として添加されるアルミニウム、リ
ン、モリブデン、タングステンは酸化物として０．１〜
７ｗｔ％で、好ましくは０．３〜３ｗｔ％で、０．１ｗ
ｔ％未満では色味、白色度の改善は見られず、７ｗｔ％
を超えても導電性は低下しない。第３元素を添加する方
法としてはアルミニウム、リン、モリブデン、タングス
テンの化合物を錫アンチモン混合塩酸酸性水溶液もしく
はアルカリ水溶液に溶解させる。錫アンチモン混合塩酸
酸性水溶液へ添加する化合物の例は塩化アルミニウムの
溶解は塩化アルミニウム、硝酸アルミニウム、硫酸アル
ミニウム、燐酸、モリブデン酸、五塩化モリブデン、タ
ングストリン酸、六塩化タングステン等が挙げられる。
またアルカリ水溶液へ添加する化合物の例はアルミン酸
塩（アルミン酸ナトリウム）、リン酸塩（ヘキサメタリ
ン酸ナトリウム等）、モリブデン酸塩（モリブデン酸ナ
トリウム等）、タングステン酸塩（タングステン酸ナト
リウム等）が挙げられる。これらの化合物を含む溶液を
加水分解させ第３元素を含むアンチモン錫水和物を得
る。酸化錫、酸化アンチモンの原料としては塩化物、有
機化合物（アルコキシド）等があるが、塩化物が望まし
い。In the present invention, the water-soluble compound means a salt of a metal and an oxyacid containing a metal in an acid radical or a salt thereof. The amount of antimony oxide added is 1 to 30 wt% and is 1
If it is less than wt%, the tint is reduced, but the conductivity is insufficient. Further, even if it exceeds 30 wt%, the conductivity does not change and the blue tint increases. Aluminum, phosphorus, molybdenum, and tungsten added as the third element are 0.1 to 0.1 as oxides.
7 wt%, preferably 0.3 to 3 wt%, 0.1 w
If it is less than t%, no improvement in color and whiteness is observed, and 7 wt%
Even if it exceeds, the conductivity does not decrease. As a method of adding the third element, a compound of aluminum, phosphorus, molybdenum and tungsten is dissolved in a tin-antimony mixed hydrochloric acid acidic aqueous solution or an alkaline aqueous solution. Examples of the compound added to the tin-antimony mixed hydrochloric acid aqueous solution include aluminum chloride, aluminum nitrate, aluminum sulfate, phosphoric acid, molybdic acid, molybdenum pentachloride, tungstophosphoric acid, and tungsten hexachloride.
Examples of compounds added to the alkaline aqueous solution include aluminate (sodium aluminate), phosphate (sodium hexametaphosphate, etc.), molybdate (sodium molybdate, etc.), and tungstate (sodium tungstate, etc.). To be The solution containing these compounds is hydrolyzed to obtain antimony tin hydrate containing the third element. As a raw material of tin oxide and antimony oxide, there are chlorides, organic compounds (alkoxides) and the like, but chlorides are preferable.
【０００９】具体的に言えば、本発明方法は、塩化錫、
塩化アンチモンの混合塩酸水溶液とアルカリ水溶液とを
反応させ、アンチモン水和物を含む錫水和沈殿物を得る
際に予め錫アンチモン混合塩酸水溶液もしくはアルカリ
水溶液にアルミニウム化合物、リン化合物、モリブデン
化合物、タングステン化合物の少なくとも１種類以上溶
解させて加水分解反応させてこれを水洗、濾別、乾燥
し、導電性を得るために焼成（３００℃〜７００℃好ま
しくは４５０℃〜６５０℃）することからなる。加水分
解に使用するアルカリ水溶液としては、水酸化ナトリウ
ム、水酸化カリウム、炭酸ナトリウム、炭酸カリウム等
のアルカリ金属水酸化物、炭酸塩やアンモニア等が挙げ
られる。Specifically, the method of the present invention comprises tin chloride,
When a tin hydrate precipitate containing antimony hydrate is obtained by reacting a mixed hydrochloric acid aqueous solution of antimony chloride with an alkaline aqueous solution, an aluminum compound, a phosphorus compound, a molybdenum compound, or a tungsten compound is previously added to the tin antimony mixed hydrochloric acid aqueous solution or the alkaline aqueous solution. Of at least one of them is dissolved and hydrolyzed, washed with water, separated by filtration, dried, and fired (300 ° C. to 700 ° C., preferably 450 ° C. to 650 ° C.) to obtain conductivity. Examples of the alkaline aqueous solution used for hydrolysis include alkali metal hydroxides such as sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate, carbonates and ammonia.
【発明の具体的開示】以下、本発明を具体的実施例によ
って具体的に説明する。DETAILED DESCRIPTION OF THE INVENTION The present invention will be specifically described below with reference to specific examples.
【００１０】[0010]
【実施例１】水２ｌを攪拌しながら９０℃に保持し、こ
れに塩化第二錫９０ｇと三塩化アンチモン８ｇとを含む
塩酸酸性水溶液２００ｍｌとヘキサメタリン酸ナトリウ
ム２ｇを溶解した水酸化ナトリウム水溶液（５００ｇ／
ｌ）２００ｍｌとを３０分にわたって同時に滴下し、リ
ンを含むアンチモン錫水和物を得た。水洗、濾別、乾燥
（１００℃）を行った後焼成（６００℃、１ｈｒ）し
た。得られた５８ｇの粉末（酸化アンチモン１０ｗｔ
％、リン１ｗｔ％）は比表面積７６ｍ2／ｇ（平均粒径
０．０２μｍ）で、色調を測定したところＬ値６５、ａ
−２．０、ｂ −２．３（スガ試験機(株)製カラーコン
ピュータ）、体積抵抗値５Ω・ｃｍ（１００ｋｇ／ｃｍ
2 加圧粉体）であった。Example 1 2 l of water was stirred and kept at 90 ° C., and 200 ml of an acidic hydrochloric acid aqueous solution containing 90 g of stannic chloride and 8 g of antimony trichloride and 2 g of sodium hexametaphosphate were dissolved in the sodium hydroxide aqueous solution (500 g /
l) 200 ml was simultaneously added dropwise over 30 minutes to obtain antimony tin hydrate containing phosphorus. It was washed with water, filtered, dried (100 ° C.), and then baked (600 ° C., 1 hr). Obtained 58 g of powder (antimony oxide 10 wt
%, Phosphorus 1 wt%) has a specific surface area of 76 m 2 / g (average particle size 0.02 μm), and the color tone was measured to find an L value of 65, a
-2.0, b-2.3 (color computer manufactured by Suga Test Instruments Co., Ltd.), volume resistance value 5 Ω · cm (100 kg / cm
2 pressurized powder).
【実施例２】アルミン酸ナトリウム１．４ｇを水酸化ナ
トリウム水溶液に溶解させ、実施例１と同様な方法で導
電性微粉末を合成した。得られた５７ｇの粉末（酸化ア
ンチモン１０ｗｔ％、アルミニウム０．８ｗｔ％）は比
表面積９１ｍ2／ｇ（平均粒径０．０１５μｍ）、色調
Ｌ値６０、ａ −３．１、ｂ −２．６、体積抵抗値６Ω
・ｃｍであった。Example 2 1.4 g of sodium aluminate was dissolved in an aqueous sodium hydroxide solution, and conductive fine powder was synthesized in the same manner as in Example 1. The obtained 57 g of powder (antimony oxide 10 wt%, aluminum 0.8 wt%) has a specific surface area of 91 m 2 / g (average particle size 0.015 μm), color tone L value of 60, a-3.1, b-2.6. , Volume resistance value 6Ω
・ It was cm.
【実施例３】モリブデン酸ナトリウム３．７ｇを水酸化
ナトリウム水溶液に溶解させ、実施例１と同様な方法で
導電性微粉末を合成した。得られた５７ｇの粉末（酸化
アンチモン１０ｗｔ％、モリブデン２．５ｗｔ％、比表
面積１０９ｍ2／ｇ（平均粒径０．０１５μｍ）、色調
Ｌ値６１、ａ −２．１、ｂ −０．８、体積抵抗値２Ω
・ｃｍであった。Example 3 3.7 g of sodium molybdate was dissolved in an aqueous sodium hydroxide solution, and conductive fine powder was synthesized in the same manner as in Example 1. The obtained 57 g of powder (antimony oxide 10 wt%, molybdenum 2.5 wt%, specific surface area 109 m 2 / g (average particle size 0.015 μm), color tone L value 61, a −2.1, b −0.8, Volume resistance value 2Ω
・ It was cm.
【比較例１】第３元素を添加しないで実施例１と同様な
方法で導電性粉末を合成した。得られた５７ｇの粉末
（酸化アンチモン１０ｗｔ％）は比表面積６０ｍ2／ｇ
（平均粒径０．０２μｍ）、色調Ｌ値３８、ａ −４．
６、ｂ −８．３、体積抵抗値２Ω・ｃｍであった。Comparative Example 1 A conductive powder was synthesized in the same manner as in Example 1 without adding the third element. The obtained 57 g of powder (antimony oxide 10 wt%) has a specific surface area of 60 m 2 / g.
(Average particle size 0.02 μm), color tone L value 38, a −4.
6, b-8.3, and the volume resistance value was 2 Ω · cm.
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【手続補正書】[Procedure amendment]
【提出日】平成５年１０月１３日[Submission date] October 13, 1993
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】発明の名称[Name of item to be amended] Title of invention
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【発明の名称】 導電性白色粉末とその製造方法Title: Conductive white powder and method for producing the same
Claims (2)
グステンを合計で、０．１〜７ｗｔ％、酸化アンチモン
を３〜３０ｗｔ％含有し、残りが酸化錫である平均粒径
０．２μｍ以下の白色導電性粉末。1. A white electroconductive material containing 0.1 to 7 wt% of aluminum, phosphorus, molybdenum, and tungsten in total, 3 to 30 wt% of antimony oxide, and the balance being tin oxide, having an average particle size of 0.2 μm or less. Powder.
物の共存する混合水溶液とアルカリ水溶液とを混和して
中和し水酸化物を沈殿させる製造方法において、水溶性
のアルミニウム化合物、リン化合物、モリブデン化合
物、タングステン化合物の少なくとも１種を混和し水酸
化物を沈殿させた後、該水酸化物を洗浄、乾燥、焼成、
粉砕して０．２μｍ以下の平均粒径を有する酸化アンチ
モン含有酸化錫微粉末を得る白色導電性粉末の製造方
法。2. A water-soluble aluminum compound, phosphorus compound, molybdenum, which is used in a production method in which a mixed aqueous solution in which a water-soluble tin compound and a water-soluble antimony compound coexist and an alkaline aqueous solution are mixed and neutralized to precipitate a hydroxide. After mixing at least one of the compound and the tungsten compound to precipitate the hydroxide, the hydroxide is washed, dried, and calcined,
A method for producing a white conductive powder, which is pulverized to obtain a tin oxide fine powder containing antimony oxide having an average particle diameter of 0.2 μm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35368792A JPH06183733A (en) | 1992-12-15 | 1992-12-15 | Electric conductive white powder and it production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35368792A JPH06183733A (en) | 1992-12-15 | 1992-12-15 | Electric conductive white powder and it production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06183733A true JPH06183733A (en) | 1994-07-05 |
Family
ID=18432540
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35368792A Pending JPH06183733A (en) | 1992-12-15 | 1992-12-15 | Electric conductive white powder and it production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06183733A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6897001B2 (en) | 2001-09-28 | 2005-05-24 | Canon Kabushiki Kaisha | Toner and image forming method |
| CN102496401A (en) * | 2011-12-09 | 2012-06-13 | 陕西理工学院 | Light-color electric conduction powder with good thermal insulation and not apt to agglomerate and preparing method |
| WO2013105646A1 (en) * | 2012-01-11 | 2013-07-18 | 三菱マテリアル株式会社 | Infrared cut material, infrared cut material dispersion liquid, composition for forming infrared cut film, and infrared cut film |
| JP2015129856A (en) * | 2014-01-08 | 2015-07-16 | 三菱マテリアル株式会社 | Material for controlling optical performance and conductive performance, and liquid composition for forming coating film comprising the material |
| US20180175398A1 (en) * | 2015-08-04 | 2018-06-21 | Mitsui Mining & Smelting Co., Ltd. | Tin oxide, electrode catalyst for fuel cells, membrane electrode assembly, and solid polymer fuel cell |
-
1992
- 1992-12-15 JP JP35368792A patent/JPH06183733A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6897001B2 (en) | 2001-09-28 | 2005-05-24 | Canon Kabushiki Kaisha | Toner and image forming method |
| CN102496401A (en) * | 2011-12-09 | 2012-06-13 | 陕西理工学院 | Light-color electric conduction powder with good thermal insulation and not apt to agglomerate and preparing method |
| WO2013105646A1 (en) * | 2012-01-11 | 2013-07-18 | 三菱マテリアル株式会社 | Infrared cut material, infrared cut material dispersion liquid, composition for forming infrared cut film, and infrared cut film |
| JP2013163634A (en) * | 2012-01-11 | 2013-08-22 | Mitsubishi Materials Corp | Infrared cut material, infrared cut material dispersion liquid, composition for forming infrared cut film, and infrared cut film |
| US8927067B2 (en) | 2012-01-11 | 2015-01-06 | Mitsubishi Materials Corporation | Infrared ray cut-off material, dispersion of infrared ray cut-off material, infrared ray cut-off film-forming composition, and infrared ray cut-off film |
| JP2015129856A (en) * | 2014-01-08 | 2015-07-16 | 三菱マテリアル株式会社 | Material for controlling optical performance and conductive performance, and liquid composition for forming coating film comprising the material |
| US20180175398A1 (en) * | 2015-08-04 | 2018-06-21 | Mitsui Mining & Smelting Co., Ltd. | Tin oxide, electrode catalyst for fuel cells, membrane electrode assembly, and solid polymer fuel cell |
| EP3333127A4 (en) * | 2015-08-04 | 2019-04-10 | Mitsui Mining and Smelting Co., Ltd. | Tin oxide, electrode catalyst for fuel cells, membrane electrode assembly, and solid polymer fuel cell |
| US10615425B2 (en) | 2015-08-04 | 2020-04-07 | Mitsui Mining & Smelting Co., Ltd. | Tin oxide, electrode catalyst for fuel cells, membrane electrode assembly, and solid polymer fuel cell |
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