JPH02197014A - Preparation of conductive tin oxide powder - Google Patents
Preparation of conductive tin oxide powderInfo
- Publication number
- JPH02197014A JPH02197014A JP1719689A JP1719689A JPH02197014A JP H02197014 A JPH02197014 A JP H02197014A JP 1719689 A JP1719689 A JP 1719689A JP 1719689 A JP1719689 A JP 1719689A JP H02197014 A JPH02197014 A JP H02197014A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- fluorine
- tin oxide
- gas
- oxide powder
- 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.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 39
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910001887 tin oxide Inorganic materials 0.000 title claims description 23
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 26
- 239000011737 fluorine Substances 0.000 claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 abstract description 22
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000011261 inert gas Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910000792 Monel Inorganic materials 0.000 description 1
- 235000010582 Pisum sativum Nutrition 0.000 description 1
- 240000004713 Pisum sativum Species 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- YWMMBLROIUSLBV-UHFFFAOYSA-N dimethylstannanylidene(dimethyl)tin Chemical compound C[Sn](C)=[Sn](C)C YWMMBLROIUSLBV-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- VXKWYPOMXBVZSJ-UHFFFAOYSA-N tetramethyltin Chemical compound C[Sn](C)(C)C VXKWYPOMXBVZSJ-UHFFFAOYSA-N 0.000 description 1
- 238000009849 vacuum degassing Methods 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
Landscapes
- Conductive Materials (AREA)
Abstract
Description
【発明の詳細な説明】
(産業上の利用分野)
本発明は酸化スズ(S n Ot )粉末をフッ素ガ
ス処理することによるフッ素ドープした導電性酸化スズ
粉末の製造法に関する。酸化スズ粉末は、低抵抗化する
ことで導電性粉体として用いられている。この導電性粉
体としては通常SbドープしたS n O!が低電気抵
抗体として知られているが、sbの毒性の問題があり、
Sbを含まないものが望まれている。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing fluorine-doped conductive tin oxide powder by treating tin oxide (S n Ot ) powder with fluorine gas. Tin oxide powder is used as a conductive powder due to its low resistance. This conductive powder is usually Sb-doped SnO! is known as a low electrical resistance material, but there is a problem with the toxicity of sb.
A material that does not contain Sb is desired.
(従来技術とその問題点)
導電性酸化スズ粉末の製造法としては、次の方法が知ら
れている。(Prior art and its problems) The following method is known as a method for producing conductive tin oxide powder.
(1)塩化アンチモノと塩化スズの加水分解によりSb
をドープする方法。(1) Sb by hydrolysis of antimonochloride and tin chloride
How to dope.
(2)SnOlなH8のような還元性雰囲気下にて突成
することにより、Snugの−PAt全Atズに還元し
、このSnをドープする方法。(2) A method in which Snug is reduced to -PAt all At by forming SnOl in a reducing atmosphere such as H8, and this Sn is doped.
111の方法で優られた導電性Sn0g粉末は灰青色を
呈することと、sbの毒性VC問題がある。また、(2
)の方法で侮られた導電性SnO,粉末は色が黒くなる
ことと安定性がなく経時変化な伴うことに問題がある。The conductive Sn0g powder obtained by the method of No. 111 exhibits a gray-blue color and has the problem of sb toxicity VC. Also, (2
The conductive SnO powder used in the method (2) has problems in that it becomes black in color, is unstable, and does not change over time.
酸化スズにフッ素をドープする方法としては、酸化スズ
粉末のフッ素ドープは知られていないが、スズ暎の場合
に次の如き例がある。As a method of doping tin oxide with fluorine, doping of tin oxide powder with fluorine is not known, but the following example is available in the case of tin oxide.
fi+ スプレー法
塩化スズの溶液とフッ化アンモニウム等の溶液(または
その混合物)を同時に高@に加熱した基板上に吹きつけ
ることにより、基板上で酸化堆積する醇化スズにフッ素
を取り込ませる方法である。fi+ Spray method This is a method in which fluorine is incorporated into tin infusate that is oxidized and deposited on the substrate by simultaneously spraying a solution of tin chloride and ammonium fluoride (or a mixture thereof) onto a highly heated substrate. .
酸化スズ膜にフッ素が取り込まれる効率は非常に悪く、
大部分のフッ素は飛散してしまうという欠点がある。The efficiency with which fluorine is incorporated into the tin oxide film is very low.
The drawback is that most of the fluorine scatters.
+21 CVD法(化学蒸着法)
有機スズ(テトラメチルスズ)と有機フッ化物(CF
s B r ) k原料とした化学M惰性である。+21 CVD method (chemical vapor deposition method) Organic tin (tetramethyltin) and organic fluoride (CF
s B r ) K is the chemical M inertia used as the raw material.
CVD法は量産性に優れているが、原料となるテトラメ
チルスズが高価であるといつデメリットがある。フッ素
添加のcvD@では比抵抗が3X10″″4Ω儒の膜が
得られている。フッ素の添加量はスズに対して数粂程度
である。Although the CVD method is excellent in mass production, it has a disadvantage in that the raw material, tetramethyltin, is expensive. In fluorine-doped cvD@, a film with a specific resistance of 3×10″″4Ωf was obtained. The amount of fluorine added is about several peas per tin.
以上のように、フッ素’t S n O!中に導入する
ことにより、導電性が出ることが知られているが、粉末
でフッ素ドープしたS n O!は知られていない。こ
れはSnO@粉末にフッ素をドープすることが難しいた
めであった。As mentioned above, Fluorine't SnO! It is known that conductivity can be achieved by introducing fluorine-doped powder into S n O! is not known. This was because it was difficult to dope SnO@ powder with fluorine.
(発明の目的)
本発明者等は、5nO1粉末にフッ素?ドープして導電
性な付与する方法な!!!供すべく、研究?電ねた結果
、不活性雰囲気下で5nO1粉末を7ツ累処理すること
により、目的を達成しうろことな見出し、本発明に到達
した。(Purpose of the invention) The present inventors have discovered that 5nO1 powder contains fluorine. There is a way to make it conductive by doping it! ! ! Research to serve? As a result of our research, we achieved the objective by processing 5nO1 powder seven times under an inert atmosphere, and arrived at the present invention.
(発明の構成)
すなわち、本発明によれば、酸化スズ粉末を、不活性ガ
ス雰囲気下にて10〜40 vol %のフッ素ガスと
接触させることにより、DflR化スズにフッ素をドー
プして導電性を付与することを特徴とする導電性酸化ス
ズ粉末の與造法、が遵られる。(Structure of the Invention) That is, according to the present invention, tin oxide powder is brought into contact with 10 to 40 vol % fluorine gas in an inert gas atmosphere, thereby doping tin DflR with fluorine to make it conductive. A method for producing conductive tin oxide powder is followed, which is characterized by imparting a conductive tin oxide powder.
本発明方法におけるNl、Ar等の不活性ガス雰囲気下
におけるフッ素ガス濃度は10〜40vol%の範囲で
ある。フッflL濃度が10vol%未満ではフッ素が
入りに<<、導電性が低い。40vol−を越えると、
反応が激しくなり、酸化スズ粉末は黒色となり、不適で
ある。例えばF、10vol慢−N黛90vol慢処理
の場合には、ノンドープの酸化スズの比抵抗値は1G’
Ω・1オーダーであるのに対し、1G4Ω・αオーダー
の25fi性酸化スズ粉末が舟られる。また、酸化スズ
粉末とフッ素ガスとの接触時の温度は、室温でもフッ素
ドープは可能であるが、24電性が低いので、好ましく
は300〜600℃の範囲である。600℃?越えると
、反応が激しく、酸化スズ粉末は黒色となる。In the method of the present invention, the fluorine gas concentration in an atmosphere of an inert gas such as Nl or Ar is in the range of 10 to 40 vol%. When the fluorine concentration is less than 10 vol %, fluorine is present and the conductivity is low. When it exceeds 40 vol-,
The reaction becomes violent and the tin oxide powder turns black, which is unsuitable. For example, in the case of F, 10 vol.-N, 90 vol. treatment, the specific resistance value of undoped tin oxide is 1G'
While it is on the order of Ω・1, 25fi tin oxide powder on the order of 1G4Ω・α is used. Further, the temperature at which the tin oxide powder and the fluorine gas are brought into contact is preferably in the range of 300 to 600° C., although fluorine doping is possible even at room temperature, since the 24-electrification is low. 600℃? If this value is exceeded, the reaction will be violent and the tin oxide powder will turn black.
本発明方法で得られた導電性酸化スズ粉末で白色に近い
ものは1紙、&I脂、繊維等の帯電防止剤として使用で
きる。また可視光の波長(0,4〜0.8μ7?り以下
の粒子によることにより、透明性が出てくるため、塗料
中に混入し、帯電防止塗料とすることもできる。この塗
料に+ia布した塗膜は透明帯酸防止フィルムになるば
かりでなく、@電圧を1811釧するための感光機用酢
嗅ともなる。The nearly white conductive tin oxide powder obtained by the method of the present invention can be used as an antistatic agent for paper, &I oil, fibers, etc. In addition, particles with a wavelength of visible light (0.4 to 0.8 microns or less) provide transparency, so they can be mixed into paints and used as antistatic paints. The resulting coating film not only becomes a transparent anti-acid film, but also serves as a vinegar filter for photosensitive machines to adjust the voltage.
次に、本発明を実施11H,I VCより具体的に説明
するが、これら実施例は本発明の範囲k 1tllJ定
するものではない。又実施例においては、vol釜?俤
にて示す。Next, the present invention will be explained in detail using Examples 11H and IVC, but these Examples do not define the scope of the present invention. Also, in the embodiment, vol pot? Indicated by a circle.
央#I声Jl
モネル製の円筒模型(60cm長×6cWLグ)の反応
容器に5n02粉末8.5yを入れたモネル裂14aa
長のボートを入れ、真ツ脱気10分後、N8ガスパージ
し、室温でF、10%−N!90%の混合気体を140
cc/IIJAの流速で40分導入した後sJガスで
10分間パージし、真空脱気10分後、またN、ガスパ
ージし、サンプルケ取り出した。Flガス@埋したSn
0g粉末をxookg/dにて加圧した圧粉体の形にし
、比低抗値k ma1定したところ、5.0X10’Ω
・(7)となった。Central #I voice Jl Monel fissure 14aa containing 8.5y of 5n02 powder in a reactor of a Monel cylindrical model (60cm length x 6cWL)
After putting in a long boat and degassing for 10 minutes, purge with N8 gas, and at room temperature F, 10%-N! 90% mixed gas at 140%
After introducing at a flow rate of cc/IIJA for 40 minutes, it was purged with sJ gas for 10 minutes, and after vacuum degassing for 10 minutes, it was purged again with N gas and the sample was taken out. Fl gas @ buried Sn
0g powder was pressed at xookg/d to form a green compact, and the specific resistance value kma1 was determined to be 5.0X10'Ω.
・It became (7).
実施例2
実施例1と同様の実験装置、牛脂で、F1ガス処理を行
った。ただF、10%−N、90%の混合気体な導入す
る際、反応管をマントルヒーターで300℃に加熱した
。こうしてF、ガス処理した5nOt粉末の比低抗値は
6.5X10”Ω・傭であった。Example 2 F1 gas treatment was performed using the same experimental equipment and beef tallow as in Example 1. However, when introducing a mixed gas of F, 10%-N, and 90%, the reaction tube was heated to 300° C. with a mantle heater. The specific resistance value of the 5nOt powder thus treated with F gas was 6.5×10”Ω·m.
実施例3
実験方法はW施例1,2に従い、F、10チーN、90
俤の混合気体を導入し77[]熱り温度を600℃にし
て5not粉末をF、ガス処理したところ、Sn0g粉
末の比抵抗値は2.4X10”Ω・□□□どなった。Example 3 The experimental method was according to W Examples 1 and 2, F, 10 Chi N, 90
When the 5not powder was treated with F gas by introducing a mixed gas of 77[] and heating temperature to 600°C, the specific resistance value of the Sn0g powder was 2.4×10”Ω·□□□.
実施例4
実験方法は上記実施例に従い、F、40%−Nx60%
の混合気体を導入し、それぞれ40分。Example 4 The experimental method was as per the above example, F, 40%-Nx60%
A mixture of gases was introduced for 40 minutes each.
300℃及び40分、600℃でF、ガス処理したとこ
ろ、得られた5nO1粉末の比抵抗値はそれぞれ7.5
XIO”Ω・濡及び1.8X10”Ω・ぼであった。When treated with F and gas at 300°C and 600°C for 40 minutes, the specific resistance value of the obtained 5nO1 powder was 7.5.
The test results were 1.8×10”Ω and 1.8×10”Ω.
比較例1
実施例1と同様の実験装置、手順で、F、5s−N、9
5−の混合気体な導入し、40へ300℃でF、ガス処
理したところ、得られた5n01粉末の比抵抗値は1.
0X10’Ω・αであった。Comparative Example 1 Using the same experimental equipment and procedure as in Example 1, F, 5s-N, 9
When a mixed gas of 5N01 was introduced and gas treated with F at 300°C, the specific resistance value of the obtained 5N01 powder was 1.
It was 0×10'Ω·α.
比較例2
実施例1と同様の実験装置、手順で、F250%−N、
50%の混合気体を導入し、40分、300℃でF、ガ
ス処理したところ、得られた5nO1粉末は黒色の粉末
となり、安定性がなかった。Comparative Example 2 Using the same experimental equipment and procedure as in Example 1, F250%-N,
When a 50% mixed gas was introduced and F gas treatment was performed at 300° C. for 40 minutes, the obtained 5nO1 powder became a black powder and was unstable.
Claims (2)
40vol%のフッ素ガスと接触させることにより,該
酸化スズにフッ素をドープして導電性を付与することを
特徴とする導電性酸化スズ粉末の製造法。(1) Add tin oxide powder to 10~
A method for producing conductive tin oxide powder, which comprises doping the tin oxide with fluorine to impart conductivity to the tin oxide by contacting it with 40 vol% fluorine gas.
法であって、該フッ素ガスとの接触時の温度を300〜
600℃の範囲とすることを特徴とする該製造法。(2) The method for producing the conductive tin oxide powder according to claim (1), wherein the temperature at the time of contact with the fluorine gas is 300-300°C.
The manufacturing method is characterized in that the temperature is in the range of 600°C.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1719689A JP2605855B2 (en) | 1989-01-26 | 1989-01-26 | Method for producing conductive tin oxide powder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1719689A JP2605855B2 (en) | 1989-01-26 | 1989-01-26 | Method for producing conductive tin oxide powder |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH02197014A true JPH02197014A (en) | 1990-08-03 |
JP2605855B2 JP2605855B2 (en) | 1997-04-30 |
Family
ID=11937182
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP1719689A Expired - Lifetime JP2605855B2 (en) | 1989-01-26 | 1989-01-26 | Method for producing conductive tin oxide powder |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2605855B2 (en) |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5238674A (en) * | 1990-02-05 | 1993-08-24 | Oce-Nederland B.V. | Process for preparing a fluorine-doped tin oxide powder |
WO1995004700A1 (en) * | 1993-08-11 | 1995-02-16 | Sumitomo Chemical Company, Limited | Metal oxide powder and process for producing the same |
EP0849337A3 (en) * | 1996-12-19 | 1999-04-21 | Showa Denko Kabushiki Kaisha | Surface-fluorinated metal oxide particulates, process for manufacturing the same and use of the same |
US6245140B1 (en) | 1996-12-19 | 2001-06-12 | Showa Denko K.K. | Surface-fluorinated metal oxide particulates, process for manufacturing the same, and use of the same |
DE102008030486A1 (en) | 2008-06-26 | 2009-12-31 | Binnewies, Michael, Prof. Dr. rer. nat. | Preparing substituted tin(IV)-oxide particle, useful e.g. in solar cell, comprises providing precursor compound, introducing compound suitable for substitution, and converting precursor compound with oxygen/a compound that releases oxygen |
EP2851908A1 (en) | 2013-09-19 | 2015-03-25 | Titan Kogyo Kabushiki Kaisha | Fluorinated phosphorus-doped electroconductive tin oxide powder, method of producing the powder and film using the powder |
US9269472B2 (en) | 2011-03-16 | 2016-02-23 | Mitsui Mining & Smelting Co., Ltd. | Fluorine-doped tin-oxide particles and manufacturing method therefor |
CN105540648A (en) * | 2016-01-21 | 2016-05-04 | 山东科技大学 | Preparation method of stannic oxide mesoporous spheres |
US9372419B2 (en) | 2012-08-30 | 2016-06-21 | Canon Kabushiki Kaisha | Electrophotographic photosensitive member, process cartridge, and electrophotographic apparatus |
US9470989B2 (en) | 2014-02-24 | 2016-10-18 | Canon Kabushiki Kaisha | Electrophotographic photosensitive member, process cartridge, and electrophotographic apparatus |
US10329161B2 (en) | 2014-12-19 | 2019-06-25 | Mitsui Mining & Smelting Co., Ltd. | Halogen-containing tin oxide particles and production method thereof |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5062520B2 (en) * | 2007-01-31 | 2012-10-31 | 三菱マテリアル株式会社 | Transparent tin oxide powder |
-
1989
- 1989-01-26 JP JP1719689A patent/JP2605855B2/en not_active Expired - Lifetime
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5238674A (en) * | 1990-02-05 | 1993-08-24 | Oce-Nederland B.V. | Process for preparing a fluorine-doped tin oxide powder |
JPH0769633A (en) * | 1990-02-05 | 1995-03-14 | Oce Nederland Bv | Preparation of fluorine dope oxidation tin powder |
WO1995004700A1 (en) * | 1993-08-11 | 1995-02-16 | Sumitomo Chemical Company, Limited | Metal oxide powder and process for producing the same |
US6303091B1 (en) * | 1993-08-11 | 2001-10-16 | Sumitomo Chemical Company, Limited | Metal oxide powder and method for the production of the same |
EP0849337A3 (en) * | 1996-12-19 | 1999-04-21 | Showa Denko Kabushiki Kaisha | Surface-fluorinated metal oxide particulates, process for manufacturing the same and use of the same |
US6245140B1 (en) | 1996-12-19 | 2001-06-12 | Showa Denko K.K. | Surface-fluorinated metal oxide particulates, process for manufacturing the same, and use of the same |
DE102008030486A1 (en) | 2008-06-26 | 2009-12-31 | Binnewies, Michael, Prof. Dr. rer. nat. | Preparing substituted tin(IV)-oxide particle, useful e.g. in solar cell, comprises providing precursor compound, introducing compound suitable for substitution, and converting precursor compound with oxygen/a compound that releases oxygen |
US9269472B2 (en) | 2011-03-16 | 2016-02-23 | Mitsui Mining & Smelting Co., Ltd. | Fluorine-doped tin-oxide particles and manufacturing method therefor |
US9372419B2 (en) | 2012-08-30 | 2016-06-21 | Canon Kabushiki Kaisha | Electrophotographic photosensitive member, process cartridge, and electrophotographic apparatus |
EP2851908A1 (en) | 2013-09-19 | 2015-03-25 | Titan Kogyo Kabushiki Kaisha | Fluorinated phosphorus-doped electroconductive tin oxide powder, method of producing the powder and film using the powder |
US9470989B2 (en) | 2014-02-24 | 2016-10-18 | Canon Kabushiki Kaisha | Electrophotographic photosensitive member, process cartridge, and electrophotographic apparatus |
US10329161B2 (en) | 2014-12-19 | 2019-06-25 | Mitsui Mining & Smelting Co., Ltd. | Halogen-containing tin oxide particles and production method thereof |
CN105540648A (en) * | 2016-01-21 | 2016-05-04 | 山东科技大学 | Preparation method of stannic oxide mesoporous spheres |
Also Published As
Publication number | Publication date |
---|---|
JP2605855B2 (en) | 1997-04-30 |
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