JPH0351657B2 - - Google Patents
Info
- Publication number
- JPH0351657B2 JPH0351657B2 JP59138571A JP13857184A JPH0351657B2 JP H0351657 B2 JPH0351657 B2 JP H0351657B2 JP 59138571 A JP59138571 A JP 59138571A JP 13857184 A JP13857184 A JP 13857184A JP H0351657 B2 JPH0351657 B2 JP H0351657B2
- Authority
- JP
- Japan
- Prior art keywords
- tin
- oxide
- stannic oxide
- conductivity
- metal
- 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.)
- Expired - Lifetime
Links
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 52
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 18
- 239000000835 fiber Substances 0.000 claims description 16
- 229910001128 Sn alloy Inorganic materials 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 229910001887 tin oxide Inorganic materials 0.000 claims description 10
- 229910044991 metal oxide Inorganic materials 0.000 claims description 9
- 150000004706 metal oxides Chemical class 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000004020 conductor Substances 0.000 claims 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 6
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- GZCWPZJOEIAXRU-UHFFFAOYSA-N tin zinc Chemical compound [Zn].[Sn] GZCWPZJOEIAXRU-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Description
【発明の詳細な説明】
産業上の利用分野
本発明は繊維状導電性酸化第二錫の製造法に関
する。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for producing fibrous conductive stannic oxide.
酸化第二錫は酸、アルカリに対して非常に耐久
性を有し、また熱に対しても安定であるので、こ
れを導電性の優れた繊維にすることができれば耐
薬品、耐熱性で、かつ電気伝導性の繊維として有
用に利用し得られる。 Since stannic oxide is extremely durable against acids and alkalis, and is also stable against heat, if it can be made into a fiber with excellent conductivity, it will be resistant to chemicals and heat. Moreover, it can be usefully used as an electrically conductive fiber.
従来技術
従来、繊維状導電性酸化錫を多量に製造する方
法は知られていない。Prior Art Conventionally, there is no known method for producing a large amount of fibrous conductive tin oxide.
発明の目的
本発明の目的は酸化第二錫の細かな均一径で、
且つ導電性の優れた繊維を製造する方法を提供す
るにある。Purpose of the invention The purpose of the present invention is to produce a fine uniform diameter of stannic oxide,
Another object of the present invention is to provide a method for producing fibers with excellent conductivity.
発明の構成
本発明者らはさきに酸化第二錫に銅を加えた混
合物を不活性ガス雰囲気下で溶融し、該溶融物か
ら酸化第二錫を蒸発させ、蒸発物を低温部に導い
て析出成長させると、酸化第二錫繊維が得られる
ことを発明した。（特願昭58−164764号）。更に研
究を重ねた結果、前記方法における銅に代え、錫
または錫の融点を増減させる錫合金を使用して
も、同様にして酸化第二錫繊維が製造し得られる
ことが分つた。そして、酸化第二錫にこれに導電
性を増加させる金属またはその金属酸化物及び錫
または錫の融点を増減させた錫合金を混合し、該
混合物を不活性ガス雰囲気下または錫、錫合金が
酸化されない酸素分圧のガス雰囲気下で溶融して
前記導電性を増加させる金属または金属酸化物を
含んだ酸化錫を蒸発させ、この蒸発物を低温部に
導き析出成長させると、導電性のよい酸化第二錫
繊維が得られることを究明し得た。この知見に基
いて本発明を完成した。Structure of the Invention The present inventors first melted a mixture of tinned oxide and copper in an inert gas atmosphere, evaporated the tinned oxide from the melt, and led the evaporated product to a low temperature section. The inventors have discovered that stannic oxide fibers can be obtained by precipitation growth. (Special Application No. 164764, 1982). As a result of further research, it was found that stannic oxide fibers could be produced in the same manner by using tin or a tin alloy that increases or decreases the melting point of tin in place of copper in the above method. Then, the stannic oxide is mixed with a metal that increases conductivity or its metal oxide, and tin or a tin alloy that increases or decreases the melting point of tin. Tin oxide containing a metal or metal oxide that increases the conductivity by melting in a gas atmosphere with a non-oxidizing oxygen partial pressure is evaporated, and this evaporated product is led to a low-temperature area to precipitate and grow. It has been found that stannic oxide fibers can be obtained. The present invention was completed based on this knowledge.
本発明の要旨は、酸化第二錫と、酸化第二錫に
導電性を増加させるアンチモンまたはイリジウム
またはその金属酸化物と、錫または錫の融点を増
減させた錫合金とを、不活性ガス雰囲気下または
錫、錫合金が酸化されない酸素分圧のガス雰囲気
下で混合融合し、該溶融物から前記導電性を増加
させる金属または金属酸化物を含んだ酸化錫を蒸
発させ、蒸発物を低温部に導いて酸化第二錫繊維
を析出成長させることを特徴とする繊維状導電性
酸化第二錫の製造法にある。 The gist of the present invention is to prepare stannic oxide, antimony or iridium or its metal oxide that increases the electrical conductivity of the stannic oxide, and tin or a tin alloy in which the melting point of tin is increased or decreased in an inert gas atmosphere. The tin or tin alloy is mixed and fused under a gas atmosphere with an oxygen partial pressure in which it is not oxidized, the tin oxide containing the metal or metal oxide that increases the conductivity is evaporated from the melt, and the evaporated product is transferred to a low temperature section. The present invention provides a method for producing fibrous conductive stannic oxide, which is characterized by depositing and growing stannic oxide fibers.
酸化第二錫に導電性を増加させる金属または金
属酸化物としては、アンチモン、インジウム、そ
れら金属の酸化物が挙げられる。また、錫の融点
を増減させた錫合金としては、例えば銅、亜鉛と
の錫合金が挙げられるが、本発明にいう錫合金と
は、錫が70％以上であり、したがつて、加える金
属の量は30％以下である。錫に加える金属の種類
及び量によつて融点を調整することができる。酸
化第二錫と、これに混合溶融する錫または錫合
金、酸化錫の導電性を増加させる金属またはその
金属酸化物との混合割合は、重量比で１：４以上
であることが好ましい。これより酸化第二錫の量
が多くなると、製造装置の炉芯管や容器が損傷さ
れ易くなる欠点が生ずる。 Metals or metal oxides that increase the conductivity of stannic oxide include antimony, indium, and oxides of these metals. In addition, examples of tin alloys in which the melting point of tin is increased or decreased include tin alloys with copper and zinc, but the tin alloys referred to in the present invention are those in which tin accounts for 70% or more. The amount of is less than 30%. The melting point can be adjusted by the type and amount of metal added to tin. The mixing ratio of stannic oxide and the tin or tin alloy mixed and melted therein, a metal that increases the conductivity of tin oxide, or a metal oxide thereof is preferably 1:4 or more by weight. If the amount of stannic oxide is larger than this, a disadvantage arises in that the furnace core tube and container of the manufacturing equipment are easily damaged.
これらの原料混合物を耐熱性容器に入れ、この
容器を加熱炉に入れて、不活性ガス雰囲気下また
は錫、錫合金が酸化されない酸素分圧のガス雰囲
気下で温度を上げ溶融させる。更に酸化第二錫が
蒸発の開始する温度以上に昇温させて酸化錫を蒸
発させる。蒸発物には導電性を増加させる金属ま
たは金属酸化物が含有される。温度はその蒸発量
に応じて調整する。耐熱容器を収容した電気炉内
に低温部を設け蒸発物をそれに導く。低温部の温
度を溶融物の温度より低い温度、例えば溶融物の
温度より50〜500℃低い温度とし、前記ガス雰囲
気下でこの温度下で１日以上維持すると、低温部
に酸化第二錫（導電性金属を含有）繊維が析出成
長する。なお、低温部の形成は、その部分に低温
ガスを吹付けたりあるいは水等の冷却剤を通ずる
ことによつても行うことができる。 A mixture of these raw materials is placed in a heat-resistant container, and the container is placed in a heating furnace, and the temperature is raised and melted under an inert gas atmosphere or a gas atmosphere with an oxygen partial pressure that does not oxidize tin and tin alloys. Furthermore, the temperature is raised to a temperature higher than the temperature at which stannic oxide starts to evaporate, thereby evaporating the tin oxide. The evaporate contains metals or metal oxides that increase conductivity. The temperature is adjusted according to the amount of evaporation. A low-temperature section is provided in the electric furnace containing the heat-resistant container, and the evaporated material is introduced into it. When the temperature of the low-temperature section is set lower than the temperature of the melt, for example, 50 to 500 degrees Celsius lower than the temperature of the melt, and maintained at this temperature in the gas atmosphere for one day or more, tin oxide (stannic oxide) is added to the low-temperature section. (containing conductive metal) fibers precipitate and grow. Note that the formation of the low-temperature portion can also be performed by spraying low-temperature gas or passing a coolant such as water through the portion.
実施例 １
99.99％のSnO215ｇ、99.99％の五酸化アンチモ
ン0.25ｇ、99.99％の錫100ｇとを混合し、この混
合物をアルミナ製ボートに入れ、該ボートを雰囲
気ガスを制御できるように炉芯管中に入れてこれ
を横型電気炉内に設置した。その設置位置は炉芯
管の３：２の分割点をボート位置とし、この点が
電気炉内の温度分布の最高温度部となるように固
定し、前記分割点から短い炉芯管の端部の方から
窒素ガスを毎分0.8〜1.0流し、毎時50℃の昇温
速さで1050℃まで昇温させて溶融し、SnO2を蒸
発させた。この状態で４日間保持することにより
炉芯管の他部の内壁に酸化第二繊維が析出成長し
た。５日後室温まで徐冷して酸化錫繊維を取出し
た。Example 1 15 g of 99.99% SnO 2 , 0.25 g of 99.99% antimony pentoxide, and 100 g of 99.99% tin were mixed, this mixture was placed in an alumina boat, and the boat was placed in a furnace core so that the atmospheric gas could be controlled. It was placed in a tube and placed in a horizontal electric furnace. The installation position is the 3:2 split point of the furnace core tube as the boat position, fixed so that this point becomes the highest temperature part of the temperature distribution in the electric furnace, and the end of the furnace core tube that is short from the dividing point. Nitrogen gas was flowed from 0.8 to 1.0 per minute, and the temperature was raised to 1050°C at a heating rate of 50°C per hour to melt and evaporate SnO 2 . By maintaining this state for 4 days, oxidized second fibers were deposited and grown on the inner wall of the other part of the furnace core tube. After 5 days, it was slowly cooled to room temperature and the tin oxide fibers were taken out.
得られた酸化錫繊維は直径0.5μｍ、長さ約３mm
のものであつた。またその導電性は100Ω・cm以
下であつた。 The obtained tin oxide fiber has a diameter of 0.5 μm and a length of about 3 mm.
It was from. Moreover, its conductivity was 100Ω·cm or less.
実施例 ２
実施例１の錫に代え、錫−亜鉛合金（錫90％）
を使用し、他は実施例１と同様にして導電性酸化
第二錫繊維が得られた。得られたものは実施例１
と同様なものであつた。Example 2 Tin-zinc alloy (90% tin) in place of tin in Example 1
Conductive tin oxide fibers were obtained in the same manner as in Example 1 except that What was obtained is Example 1
It was similar to that.
実施例 ３
実施例１のSnO2と五酸化アンチモンに代え、
市販のSnO210ｇと、酸化アンチモンを10モルド
ープさせたSnO22.5ｇを使用し、実施例１と同様
にしてSnO2繊維を製造した。得られた繊維及び
その導電性は略同じであつた。Example 3 In place of SnO 2 and antimony pentoxide in Example 1,
SnO 2 fibers were produced in the same manner as in Example 1 using 10 g of commercially available SnO 2 and 2.5 g of SnO 2 doped with 10 moles of antimony oxide. The obtained fibers and their conductivity were approximately the same.
発明の効果
本発明の方法によると、従来得られなかつた導
電性の酸化第二錫繊維を容易に製造することがで
きる優れた効果を奏し得られる。Effects of the Invention According to the method of the present invention, an excellent effect of easily producing conductive stannic oxide fibers, which could not be obtained conventionally, can be achieved.
Claims (1)
せるアンチモンまたはイリジウムまたはその金属
酸化物と、錫または錫の融点を増減させた錫合金
とを、不活性雰囲気下または錫、錫合金が酸化さ
れない酸素分圧のガス雰囲気下で、混合溶融し、
該溶融物から前記導電性を増加させる金属または
金属酸化物を含んだ酸化錫を蒸発させ、蒸発物を
低温部に導いて酸化第二錫繊維を析出成長させる
ことを特徴とする繊維状導電性酸化第二錫の製造
法。1. Add stannic oxide, antimony or iridium or its metal oxide that increases the conductivity of stannic oxide, and tin or a tin alloy with an increased or decreased melting point of tin under an inert atmosphere or with tin or a tin alloy. is mixed and melted in a gas atmosphere with an oxygen partial pressure that does not oxidize,
A fibrous conductive material characterized by evaporating tin oxide containing a metal or metal oxide that increases the conductivity from the melt, and guiding the evaporated material to a low temperature part to precipitate and grow stannic oxide fibers. Method for producing stannic oxide.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13857184A JPS6117421A (en) | 1984-07-04 | 1984-07-04 | Preparation of fibrous electrically-conductive stannic oxide |
| US06/647,656 US4623424A (en) | 1983-09-07 | 1984-09-06 | Process for producing tin oxide fibers |
| US06/885,441 US4725331A (en) | 1983-09-07 | 1986-07-14 | Process for producing tin oxide fibers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13857184A JPS6117421A (en) | 1984-07-04 | 1984-07-04 | Preparation of fibrous electrically-conductive stannic oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6117421A JPS6117421A (en) | 1986-01-25 |
| JPH0351657B2 true JPH0351657B2 (en) | 1991-08-07 |
Family
ID=15225241
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13857184A Granted JPS6117421A (en) | 1983-09-07 | 1984-07-04 | Preparation of fibrous electrically-conductive stannic oxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6117421A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2827586B2 (en) * | 1991-07-04 | 1998-11-25 | 松下電器産業株式会社 | Method for producing tin dioxide whiskers |
| TW455568B (en) * | 1994-12-27 | 2001-09-21 | Ishihara Sangyo Kaisha | Process for the preparation of acicular electroconductive tin oxide fine particles |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60161337A (en) * | 1984-02-01 | 1985-08-23 | Natl Inst For Res In Inorg Mater | Manufacture of tin oxide fiber |
-
1984
- 1984-07-04 JP JP13857184A patent/JPS6117421A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60161337A (en) * | 1984-02-01 | 1985-08-23 | Natl Inst For Res In Inorg Mater | Manufacture of tin oxide fiber |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6117421A (en) | 1986-01-25 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |