JPH02248489A - Manufacture of conductive white powder - Google Patents

Manufacture of conductive white powder

Info

Publication number
JPH02248489A
JPH02248489A JP7094789A JP7094789A JPH02248489A JP H02248489 A JPH02248489 A JP H02248489A JP 7094789 A JP7094789 A JP 7094789A JP 7094789 A JP7094789 A JP 7094789A JP H02248489 A JPH02248489 A JP H02248489A
Authority
JP
Japan
Prior art keywords
powder
oxide
sno
tin
white
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
Application number
JP7094789A
Other languages
Japanese (ja)
Other versions
JP2782768B2 (en
Inventor
Seiji Takao
高尾 精二
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Japan Exlan Co Ltd
Original Assignee
Japan Exlan Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Japan Exlan Co Ltd filed Critical Japan Exlan Co Ltd
Priority to JP7094789A priority Critical patent/JP2782768B2/en
Publication of JPH02248489A publication Critical patent/JPH02248489A/en
Application granted granted Critical
Publication of JP2782768B2 publication Critical patent/JP2782768B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Paints Or Removers (AREA)
  • Conductive Materials (AREA)

Abstract

PURPOSE:To obtain the title powder excellent in conductivity and whiteness in a simple process industrially advantageously by mixing an SnO and/or SnO2 powder with an Sb oxide powder and baking the mixture at a specified temperature. CONSTITUTION:An SnO and/or SnO2 powder is mixed with a powder of an Sb oxide, such as Sb2O3, Sb2O4, Sb2O5 or Sb6O13, so as to provide the weight ratios of SnO:SnO2:(Sb oxide) of (0 to 100):(100 to 0):(0.5 to 40). This mixture is baked at 900-1200 deg.C.

Description

【発明の詳細な説明】 (産業上の利用分計) 本発明は、製造工程の簡略された導1性白色粉末の製造
法に関する。
DETAILED DESCRIPTION OF THE INVENTION (Industrial Utilization) The present invention relates to a method for producing a monoconductive white powder with a simplified production process.

(従来技術と問題点ン 従来から、導電性スズ系酸化物白色粉末の製造法として
は、例えば各種の有amスズ塩とアンチモン化合物とを
溶媒と共に混合、乾燥し、次いで有機酸の熱分解、焼成
を行なう、或いは、酸化チタン粉末の加熱水系懸濁UK
塩化スズ又はシユク#第1スズと塩化アンチモンとのア
ルコール溶液を徐々に添加し、酸化チタン粉末表面にア
ンチモン含有酸化スズの被覆層を形成させて焼成する、
という方法等が提案されている。
(Prior Art and Problems) Conventionally, as a method for producing a conductive tin-based oxide white powder, for example, various ammonium tin salts and an antimony compound are mixed together with a solvent, dried, and then thermal decomposition of an organic acid is carried out. Calcination or heating aqueous suspension of titanium oxide powder UK
Gradually add an alcoholic solution of tin chloride or stannous tin and antimony chloride to form a coating layer of antimony-containing tin oxide on the surface of the titanium oxide powder, and then bake.
A method has been proposed.

しかし、上述し九方法の前者は、湿式混合−乾燥による
a峰除夫、有m醗の熱分解、焼成による導電性の付与等
の繁雑な工程を要し、しかも熱分解ガス発生による毒性
のため、排気処理も必要である。
However, the former of the above-mentioned nine methods requires complicated steps such as removal of the a-peak by wet mixing and drying, thermal decomposition of a certain amount, and imparting conductivity by baking, and moreover, it is toxic due to the generation of pyrolysis gas. Therefore, exhaust treatment is also required.

ま九、後者は、粉末の白皮は優れるものの反応液の7J
I熱操作、アルコール溶液添加による塩化物原料の加水
分解コントロールが困難である、さらに出発原料の塩素
成分の洗浄除去が必要である等の繁雑な工程を要する等
の欠点が60な。
Nine, the latter has an excellent powder white peel, but the reaction liquid 7J
The disadvantages are that it is difficult to control the hydrolysis of chloride raw materials by thermal operation and the addition of alcoholic solutions, and that it requires complicated steps such as the need to wash and remove the chlorine component of the starting raw materials.

(発明が解決しようとする課題〉 本発明の目的は、上述した従来の導電性7ズ系酸化物白
色粉末の繁雑な製造工程を簡略にし、且つ白色度、導1
!c性等性能の優れ良導を性白色粉末を工業的有利に提
供することにある。
(Problems to be Solved by the Invention) An object of the present invention is to simplify the complicated manufacturing process of the conventional conductive 7Z-based oxide white powder, and to improve the whiteness and conductivity.
! The object of the present invention is to provide an industrially advantageous white powder with excellent properties such as c properties and good conductivity.

(課題を解決するための手段) 上述した本発明の目的は、酸化スズ(1) (以下、S
nOという)及び/又は虐化スズ(IV) (以下、加
lという)の粉末とアンチモン酸化物の粉末とを混合し
、900〜1200℃で焼成することによシミA成され
る。
(Means for Solving the Problems) The object of the present invention described above is to produce tin oxide (1) (hereinafter referred to as S
The stain A is formed by mixing powders of tin(IV) (hereinafter referred to as nO) and/or antimony oxide (hereinafter referred to as tin(IV)) and powder of antimony oxide, and firing at 900 to 1200°C.

以下、本発明を詳述する。The present invention will be explained in detail below.

本発明にかかるSnO,8nC)z  及びアンチモン
酸化物の粉末は、工業用、試薬用等一般に市販されてい
る粉末を用いることができるが、導電性が艮く、白皮の
高い粉末を得るためには、高純度且つ粒径の小さい粉末
が好ましい。粉末粒径は、好ましくは60μ以下、さら
に好ましくはlOμ以下が望ましい。
As the powder of SnO, 8nC)z and antimony oxide according to the present invention, commercially available powders for industrial use, reagent use, etc. can be used, but in order to obtain a powder with high conductivity and a high white skin, For this purpose, powders with high purity and small particle size are preferred. The powder particle size is preferably 60 μ or less, more preferably 10 μ or less.

ここで、アンチモン酸化物はアンチモン元素の原子価に
よυm々の酸化物があるが、酸化物であればよく、例え
ば5bzOa%5bz04、Sb20g。
Here, the antimony oxide has various oxides depending on the valence of the antimony element, but any oxide may be used, for example, 5bzOa%5bz04, Sb20g.

8ba01a等を挙げることができる。Examples include 8ba01a.

上述したSn0%5nOz及びアンチモン酸化物粉末の
混合組成比は、重量比でSnO/ 5n02 /アンチ
モン酸化物−〇−100/100〜0 / 0.6−4
0、好ましくは0−100/100〜0/1−10が必
要であ1.かかる範囲を外れる場合は、充分な4を性効
果が得られない、白皮が低下する等の問題が生じ、所期
の目的が達成されない。
The mixing composition ratio of the above-mentioned Sn0%5nOz and antimony oxide powder is SnO/5n02/antimony oxide-〇-100/100~0/0.6-4 in weight ratio.
0, preferably 0-100/100 to 0/1-10, and 1. If it is out of this range, problems such as insufficient sexual effects and deterioration of white skin will occur, and the intended purpose will not be achieved.

かかる粉末の混合は乳鉢、ニーダ−プレンダー等公知の
乾式混合機、ボールミル等公知の粉砕機を使用すること
ができる。ま九、湿式混合しても何等さしつかえない。
For mixing such powders, a known dry mixer such as a mortar or a kneader-blender, or a known pulverizer such as a ball mill can be used. Also, there is no harm in wet mixing.

次に、混合した該粉末の焼成は、900〜1200℃の
温度が必要であ1.かかる範囲を外れる場合は、充分な
4wL性効果が得られず、さらに粉末が茶色、灰色等の
色相を帯び好ましくない。
Next, the mixed powder needs to be fired at a temperature of 900 to 1200°C. If it is out of this range, a sufficient 4wL property effect cannot be obtained, and furthermore, the powder takes on a brown, gray, or other hue, which is undesirable.

かかる粉末の焼成は、磁器、坩堝、甲鉢、サヤ等充分耐
熱性を有する容器に入れ、電気炉、ガス炉等の焼成炉又
はロータリーキルン等を用いて行なうことができる。
The powder can be fired by placing it in a sufficiently heat-resistant container such as a porcelain, crucible, pot, or pod, and using a firing furnace such as an electric furnace or gas furnace, or a rotary kiln.

焼成に際しての焼成時間は、5nO1SnOz、アンチ
モン酸化物の混合組成比、目標とする導電性、白皮によ
り一概に限定することはできず、また焼成の昇温速度も
同様に限定することはできないが、昇温は概ね1.6℃
/分〜80で7分の範囲で設定される。
The firing time during firing cannot be unconditionally limited depending on the mixing composition ratio of 5nO1SnOz and antimony oxide, the target conductivity, and the white peel, and the heating rate of firing cannot be similarly limited. , the temperature rise is approximately 1.6℃
It is set in the range of /minute to 80 for 7 minutes.

焼成後の粉末の取り出しは、焼成直後でも降温後に行な
ってもよく、焼成後は焼結の起る場合もめるので、適宜
再粉砕を行なう。
The powder after firing may be taken out immediately after firing or after the temperature has cooled down, and since sintering may occur after firing, re-pulverization is performed as appropriate.

(作用、効果) 本発明は、固相反応法であるが、原料に粉末を用いるた
めに反応表面が広くなっていること、アンチモンの蒸気
圧が比較的高いことが相まって、均一な酸素空孔形成が
為されていると考えられる。
(Functions and Effects) The present invention is a solid-phase reaction method, but the reaction surface is wide due to the use of powder as a raw material, and the vapor pressure of antimony is relatively high. It is thought that formation is taking place.

本発明にかかる製造法は、従来の製造法に比べて極めて
簡便な処理方法であ1.且つ優れた導電性効果、白皮を
有する粉末を工業的有利に作製し得る点が特筆すべき効
果である。
The manufacturing method according to the present invention is an extremely simple processing method compared to conventional manufacturing methods.1. In addition, a noteworthy effect is that powder having excellent conductivity and white skin can be produced industrially advantageously.

さらに、酸化スズを用いているが故に、耐熱性、ll1
1#!I性、耐アルカリ性、耐溶剤性等に優れてお1.
又優れた白皮、必要に応じて着色できること、さらに優
れた導電性が相俟りて、樹脂、紙、塗料等広範な分野に
用いることができる。
Furthermore, since tin oxide is used, heat resistance,
1#! 1. Excellent in I properties, alkali resistance, solvent resistance, etc.
In addition, due to its excellent white skin, ability to be colored if necessary, and excellent conductivity, it can be used in a wide range of fields such as resins, paper, and paints.

(突 施 例) 以下に実施例を示し、本発明を具体的に説明するが、本
発明はこれらの実施例の記載によって、その範囲を限定
されるものではない。実施例中に示される部は、特に断
らない限り重量基準である。
(Examples) The present invention will be specifically described below with reference to Examples, but the scope of the present invention is not limited by the description of these Examples. Parts shown in the examples are by weight unless otherwise specified.

なお、体積抵抗率及び白皮は、下記のように供試試料2
fを内径1.1701のテフロン製円筒中に入れs 2
 tOn / cdの加圧下で試料円柱の高さ、lc気
抵抗i1 (ADEX■製 デジタルLCRメータ使用
)を測定し、下記式によシ求め九。
In addition, the volume resistivity and white skin are as follows for sample sample 2.
Put f into a Teflon cylinder with an inner diameter of 1.1701 mm and s 2
Measure the height of the sample cylinder and the LC air resistance i1 (using a digital LCR meter manufactured by ADEX■) under a pressure of tOn/cd, and calculate it using the following formula.9.

ここで/V一体積抵抗率(Ω・帖 R−電気抵抗 (Ωン S−試料円柱底面積(d) h−試料円柱の高さ(CII) 12)   白  度 酸化チタン(白色粉末ン及びSnO(黒色粉末)を酸化
チp ン/ 5nO= 6部70部、4部71部、am
/2部、2部78部、1部74部の割合テ混合した白皮
見本を作製し、1〜5級を与え、該見本と比較して得ら
れ九粉末を内眼判定した。
Where /V - volume resistivity (Ω・带R-electrical resistance (Ω・S-sample cylinder base area (d) h-height of sample cylinder (CII) 12) Whiteness titanium oxide (white powder and SnO (black powder) as titanium oxide/5nO = 6 parts 70 parts, 4 parts 71 parts, am
Samples of white skin were prepared by mixing 2 parts, 78 parts of 2 parts, and 74 parts of 1 part, and grades 1 to 5 were given, and the obtained 9 powders were compared with the samples for intraocular evaluation.

実施例1 8nO(林純薬工業■製試薬1級)、5nOz(林純薬
工業■製試薬1級)及びSb20g (三国製練剰1粉
末を下記第1表に示す組成比で乳鉢で混合した後、混合
粉末6Fを磁器製坩堝に入れて、電気炉(mデンケンI
fりで80℃/minで外温1000℃×1.5時間焼
成を行ない、室温で放冷した。取り出した粉末を乳鉢で
粉砕し、導電性白色粉末1−16を得た。
Example 1 8nO (1st class reagent manufactured by Hayashi Pure Chemical Industries Ltd.), 5nOz (1st class reagent manufactured by Hayashi Pure Chemical Industries Ltd.) and 20 g of Sb (Mikuni Seikan Refined 1 powder were mixed in a mortar at the composition ratio shown in Table 1 below) After that, the mixed powder 6F was put into a porcelain crucible and heated in an electric furnace (M Denken I).
Firing was performed at an external temperature of 1000° C. for 1.5 hours at 80° C./min for 1.5 hours and allowed to cool at room temperature. The taken-out powder was ground in a mortar to obtain conductive white powder 1-16.

体積抵抗率及び白皮の結果を、第工表に併記する。The results of volume resistivity and white skin are also recorded in Table 1.

第     1     表 *印のものは、店子茶色の色相を帯びていた。Chapter 1 Table The one marked with * had a brownish hue.

本発明品(気2〜7.9〜18.1−6及び16)は優
れた41t!l:と白皮とを兼ね備えていることがわか
る。これに比べて、アンチ七ン酸化物を用いない粉末(
Nal、8及び17)は白皮は優れるものの4″rt!
1:効果が極めて劣)、また、Sb20g  の使用量
が本発明推奨範囲t−越える粉末(NIL14)は、導
[!1″効果は認められるものの白皮が劣る。
The products of the present invention (Ki 2-7.9-18.1-6 and 16) have an excellent 41t! It can be seen that it has both l: and white skin. In comparison, powder without anti-heptane oxide (
Nal, 8 and 17) have excellent white skin, but 4″rt!
1: Extremely poor effect), and the powder (NIL14) in which the amount of Sb20g used exceeds the recommended range of the present invention (NIL14) is Although the 1″ effect was observed, the white skin was inferior.

実施例2 実施例1の嵐lOの組成比の粉末を、焼成温度を下記第
2辰の如く変化させる以外は、実施例1と同様にして導
電性白色粉末18〜24を得た。
Example 2 Conductive white powders 18 to 24 were obtained in the same manner as in Example 1, except that the powder having the composition ratio of Arashi 1O in Example 1 was changed in firing temperature as shown in the second section below.

体積抵抗率及び白皮の結果を第2表に併記す第 表 *印のものは、店子茶色の色相を帯びていた。The results of volume resistivity and white peel are also listed in Table 2. table The one marked with * had a brownish hue.

第2表よシ明らかなように、本発明の焼成温度推奨範囲
を外れる418.19及α24は、充分な導電性効果が
ないことがわかる。また焼成温度の低いNa18及び1
9は白皮が劣ることも理解できる。
As is clear from Table 2, 418.19 and α24, which are outside the recommended firing temperature range of the present invention, do not have a sufficient conductive effect. In addition, Na18 and 1, which have a low firing temperature,
It is also understandable that 9 has inferior white skin.

実施例8 アンチモン鎖化物として、5bzOsのかゎシに5bz
Os (半片化学薬品11を用いる以外は、実施例1.
 胤10と同様にして導!を性向色粉末&26を得た。
Example 8 As an antimony chain product, 5bz was added to the base of 5bzOs.
Os (Example 1. except using half-piece chemical 11.
Lead in the same way as Seed 10! A colored powder &26 was obtained.

該粉末の体積抵抗率は2.6(Ω・cat)で、白皮は
1〜2級の優れた性能を示した。
The volume resistivity of the powder was 2.6 (Ω·cat), and the white bark showed excellent performance of grade 1 to 2.

Claims (2)

【特許請求の範囲】[Claims] 1.酸化スズ(III)(SnO)及び/又は酸化スズ(
IV)(SnO_2)の粉末とアンチモン酸化物粉末とを
混合し、900〜1200℃で焼成することを特徴とす
る導電性白色粉末の製造法。
1. Tin(III) oxide (SnO) and/or tin oxide (
IV) A method for producing conductive white powder, which comprises mixing powder of (SnO_2) and antimony oxide powder and firing the mixture at 900 to 1200°C.
2.酸化スズ(III)及び/又は酸化スズ(IV)の粉末
とアンチモン酸化物の粉末との組成比が重量比で、Sn
O/SnO_2/アンチモン酸化物=0〜100/10
0〜0/0.6〜40混合することを特徴とする請求項
1記載の導電性白色粉末の製造法。
2. The composition ratio of tin (III) oxide and/or tin (IV) oxide powder and antimony oxide powder is by weight, and Sn
O/SnO_2/antimony oxide = 0 to 100/10
2. The method for producing a conductive white powder according to claim 1, wherein the conductive white powder is mixed at a ratio of 0 to 0/0.6 to 40.
JP7094789A 1989-03-22 1989-03-22 Manufacturing method of conductive white powder Expired - Fee Related JP2782768B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP7094789A JP2782768B2 (en) 1989-03-22 1989-03-22 Manufacturing method of conductive white powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP7094789A JP2782768B2 (en) 1989-03-22 1989-03-22 Manufacturing method of conductive white powder

Publications (2)

Publication Number Publication Date
JPH02248489A true JPH02248489A (en) 1990-10-04
JP2782768B2 JP2782768B2 (en) 1998-08-06

Family

ID=13446210

Family Applications (1)

Application Number Title Priority Date Filing Date
JP7094789A Expired - Fee Related JP2782768B2 (en) 1989-03-22 1989-03-22 Manufacturing method of conductive white powder

Country Status (1)

Country Link
JP (1) JP2782768B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100345764C (en) * 2005-08-23 2007-10-31 浙江大学 Two-step method for preparing stannic oxide nano material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100345764C (en) * 2005-08-23 2007-10-31 浙江大学 Two-step method for preparing stannic oxide nano material

Also Published As

Publication number Publication date
JP2782768B2 (en) 1998-08-06

Similar Documents

Publication Publication Date Title
EP0384728A2 (en) Preparation method for zircon powder
JPH02248489A (en) Manufacture of conductive white powder
JP2594555B2 (en) Method for producing lithium niobate powder
JPS63248719A (en) Production of powder as starting material for multicomponent ceramic
CN104030362A (en) Preparing method for nano Fe2O3 powder
SU1456395A1 (en) Method of producing complex fertilizer
JPS6217005A (en) Preparation of mullite powder having high purity
Silva et al. Influence of the network former on the properties of magnesium spinels
JP3256570B2 (en) Manufacturing method of conductive material
JPS63252927A (en) Production of fine particle powder of sodium hexatitanate
JPH06183733A (en) Electric conductive white powder and it production
JPH0527571B2 (en)
JPH0574528B2 (en)
JP2001010816A (en) Metal-oxide thin film-forming composition
JPH10167728A (en) Production of crystalline metal oxide
SU948974A1 (en) Method for making piezoelectric ceramic
JPH059375B2 (en)
JPS6146403B2 (en)
JP3616362B2 (en) Method for producing metal titanate compound having specific shape
JPS5911532B2 (en) Method for producing conductive tin dioxide powder
JPS6186427A (en) Preparation of low melting point glass
JPH04219358A (en) Production of calcinated product for making bmt sintered compact and bmt sintered compact
SU1293107A2 (en) Method of lumping phosphate raw material
JPS6317219A (en) Production of ceramic powder
JPH09183611A (en) Production of crystalline silicate compound

Legal Events

Date Code Title Description
R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

LAPS Cancellation because of no payment of annual fees