JPH01176440A - Vapor phase synthesizing apparatus for producing powdery compound - Google Patents
Vapor phase synthesizing apparatus for producing powdery compoundInfo
- Publication number
- JPH01176440A JPH01176440A JP33507587A JP33507587A JPH01176440A JP H01176440 A JPH01176440 A JP H01176440A JP 33507587 A JP33507587 A JP 33507587A JP 33507587 A JP33507587 A JP 33507587A JP H01176440 A JPH01176440 A JP H01176440A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- compound
- reaction
- phase synthesis
- vapor phase
- 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.)
- Pending
Links
- 150000001875 compounds Chemical class 0.000 title claims abstract description 26
- 239000012808 vapor phase Substances 0.000 title claims abstract description 13
- 230000002194 synthesizing effect Effects 0.000 title 1
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 18
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 17
- 239000011701 zinc Substances 0.000 claims abstract description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 31
- 239000002994 raw material Substances 0.000 claims description 17
- 230000004888 barrier function Effects 0.000 claims description 12
- 239000012071 phase Substances 0.000 claims description 3
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 description 1
- 229910000058 selane Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Landscapes
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
Description
【発明の詳細な説明】
イ０発明の目的
（ａ）産業上の利用分野
この発明は二種類の原料ガスを供給して化合物粉末、特
にＺｎＳ、ＺｎＳｅ等の粉末を気相合成する装置に関す
るものである。DETAILED DESCRIPTION OF THE INVENTION A.Objective of the Invention (a) Industrial Field of Application This invention relates to an apparatus for vapor phase synthesis of compound powders, particularly powders of ZnS, ZnSe, etc., by supplying two types of raw material gases. It is.
（ｂ）従来の技術
Ｚｎ ｓ ｔ ＺｎＳｅなどの化合物粉末は螢光体の原
料として使用されるものであシ、特に高純度で微細粉末
であることが要求されるものである。(b) Prior Art Compound powders such as Zn s t ZnSe are used as raw materials for phosphors, and are particularly required to be highly pure and fine powders.
これらの粉末を製造するには反応室にキャリアーガスを
用いた金属亜鉛蒸気とＨ２Ｓ又はＨ２Ｓｅガスを原料と
したＣＶＤ法（Ｃｈｅｍｉｃａｌ ＶａｐｏｕｒＤｅｐ
ｏｓｉｔｉｏｎ ）で合成することが行われ、それによ
って高純度で微細な粉末を製造することができる。To produce these powders, a CVD method (Chemical Vapor Dep
position), thereby making it possible to produce highly pure and fine powders.
従来からこのＣＶＤ法による化合物粉末の気相合成装置
は、第３図に示すように、一端に排気管（３）を有する
管状の反応管（６）の反応室の外側にヒーター（１）を
もうけ、該反応管（６）の他端に２本の原料供給ノズル
（２）をもうけた構造である。通常反応管は石英製であ
るが、その他の材料でもよい。この装置では二種類の原
料ガス、即ちＡｒガスをキャリアーとした金属亜鉛蒸気
とＨ２Ｓ又はＨ２Ｓｅガスをそれぞれ原料供給ノズル（
２）から管状の反応室に導入して他端から排気すると加
熱によシ反応が生じて生成した化合物はバルク状或いは
粉末状となって管壁に付着する。Conventionally, a vapor phase synthesis apparatus for compound powder using the CVD method, as shown in Fig. 3, has a heater (1) installed outside the reaction chamber of a tubular reaction tube (6) having an exhaust pipe (3) at one end. In addition, two raw material supply nozzles (2) are provided at the other end of the reaction tube (6). The reaction tube is usually made of quartz, but other materials may be used. In this device, two types of raw material gases, namely metal zinc vapor using Ar gas as a carrier and H2S or H2Se gas, are supplied to the raw material supply nozzle (
When introduced into a tubular reaction chamber from 2) and exhausted from the other end, a reaction occurs due to heating and the generated compound becomes bulk or powder and adheres to the tube wall.
（Ｃ）発明が解決しようとする問題点
ところが従来の合成装置では反応室が直線状であるため
、供給された原料ガスは層流化し易く、従って化合物が
生成する際の核が均一に発生しにりく、合成反応が反応
管の壁に沿って生じてバルク状に壁に付着する部分が多
くなり、粉末化するものは僅かで比率が小さいので、化
合物粉末の製造収率が低いという問題点があった。(C) Problems to be Solved by the Invention However, in conventional synthesis equipment, since the reaction chamber is linear, the supplied raw material gas tends to flow laminarly, and therefore, when the compound is produced, the nuclei are not uniformly generated. The problem is that the synthesis reaction occurs along the wall of the reaction tube, and there is a large amount of bulk that adheres to the wall, and only a small amount of material is turned into powder, resulting in a low production yield of compound powder. was there.
口０発明の構成
（ａ）問題点を解決するための手段
化合物の粉末が合成されるためには反応室内の空中で原
料ガスが混合し化合物の核が均一大量に発生して、その
核を中心に粉末が形成される必要があり、そのた゛めに
は反応室内での原料ガス種（分子）の衝突頻度を高める
必要がある。0 Structure of the Invention (a) Means for Solving the Problem In order to synthesize powder of a compound, the raw material gases are mixed in the air in the reaction chamber, a large amount of nuclei of the compound are uniformly generated, and the nuclei are It is necessary to form a powder at the center, and for this purpose it is necessary to increase the frequency of collisions of source gas species (molecules) within the reaction chamber.
この発明は反応管中の原料ガスの乱流化を促進し原料ガ
ス種の衝突頻度を高めるために、反応管の内壁に一個あ
るいは複数個の原料ガスの流れを妨げる障壁板をもうけ
た構造を有する化合物粉末の気相合成装置である。This invention has a structure in which one or more barrier plates are provided on the inner wall of the reaction tube to prevent the flow of the source gas, in order to promote turbulence of the source gas in the reaction tube and increase the frequency of collisions of source gas species. This is a vapor phase synthesis device for compound powder with
以下具体例の図面を用いて本発明を説明する。The present invention will be explained below using drawings of specific examples.
第１図は本発明の一例を示す断面図である。第１図のよ
うに一端に排気管（３）をもうけ他端には原料ガスの供
給ノズル（２）を２本もうけた円筒形の反応管（６）の
反応管の外側にヒーター（１）をもうけである。反応管
（６）の内壁には反応管の軸即ち原料ガスの流れ方向に
直角にリング状の障壁板（５）がもうけられている。こ
の具体例においては反応管（６）は円筒状であシ、障壁
板（５）は中央に円形の孔の空いたリンク状である。FIG. 1 is a sectional view showing an example of the present invention. As shown in Figure 1, a cylindrical reaction tube (6) has an exhaust pipe (3) at one end and two raw material gas supply nozzles (2) at the other end.A heater (1) is installed on the outside of the reaction tube. It is profitable. A ring-shaped barrier plate (5) is provided on the inner wall of the reaction tube (6) at right angles to the axis of the reaction tube, that is, the flow direction of the raw material gas. In this specific example, the reaction tube (6) is cylindrical, and the barrier plate (5) is link-shaped with a circular hole in the center.
障壁板としてはリング状に限るものではなく、反応管内
に突起した他の形状でもよいことは勿論である。It goes without saying that the barrier plate is not limited to a ring shape, but may be of other shapes that protrude into the reaction tube.
（ｂ）作用
本発明の化合物粉末製造装置では、例えば第１図の構造
の場合には、原料ガスの流れは同図の矢印に示すよう、
反応管内で障壁板（５）の上流部分で渦を巻いて乱流と
なシ原料ガス種同志の衝突頻度が増加し、化合物の核が
大量に造られて化合物の微粉末の生成が促進され、粉末
（４）は反応管の内壁に堆積される。(b) Effect In the compound powder manufacturing apparatus of the present invention, for example, in the case of the structure shown in FIG. 1, the flow of the raw material gas is as shown by the arrow in the figure.
In the reaction tube, a vortex swirls in the upstream part of the barrier plate (5), creating a turbulent flow, and the frequency of collisions between raw material gas species increases, and a large number of compound nuclei are created, promoting the production of fine powder of the compound. , the powder (4) is deposited on the inner wall of the reaction tube.
この場合に生成粉末は障壁板の取り付は部周辺に堆積す
るので生成粉末を捕集するという効果も生ずるものであ
る。In this case, since the generated powder accumulates around the area where the barrier plate is attached, there is also the effect of collecting the generated powder.
（Ｃ）実施例
第２図に示す従来の装置と第３図に示す本発明の装置（
リング状障壁板を３枚取シ付け）を用いてＺｎＳ の粉
末をＣＶＤ法により合成した。(C) Example of the conventional device shown in FIG. 2 and the device of the present invention shown in FIG.
ZnS powder was synthesized by CVD using a ring-shaped barrier plate (three ring-shaped barrier plates were attached).
即ちＨ２８ガスとＡｒガスをキャリアーとした金属亜鉛
蒸気を見料ガスとして反応管に導入し、反応管内で次ぎ
の反応を行わせて気相合成した。That is, metal zinc vapor using H28 gas and Ar gas as carriers was introduced into the reaction tube as a sample gas, and the following reaction was carried out in the reaction tube to perform gas phase synthesis.
ＺｎＭ ＋ Ｈ２Ｓ （ｇ） −一→Ｚｎ Ｓ （Ｓ
） ＋ Ｈ（ｇ）但し （Ｖ）＝蒸気、 位）＝ガスｌ
（Ｓ）＝固体いずれの場合も合成条件は下記の通り
で同じとした。ZnM + H2S (g) -1 → Zn S (S
) + H (g) where (V) = steam, position) = gas l
(S)=Solid In both cases, the synthesis conditions were the same as shown below.
炉内圧 ・・・・・・・・・・・・・・・・・・・・
・ ５０ ’ｒｏｒｒ反応温度 ・・・・・・・・・・
・・・・・・・・・・・ ７５０°ＣＨ２５ガス流量・
・・・・・・・・・・・・・・ ０．４ Ｎ６／ｍｉｎ
亜鉛蒸気のキャリアー用
Ａｒガスの流量・・・・・・・・・・・・・−・ ２−
ＯＮ’／ｍｉｎ反応時間 ・・・・・・・・・・・・
・・・・・・・・・ １００時間以上の合成の結果を比
較すると
（１）従来装置の場合
管状反応管内にＺｎＳ化合物が合成されたが、その大部
分はバルク状のＺｎＳであり、粉末ＺｎＳは投入原料の
約１０％に当たる１０５０ｇであった０
（２）本発明の装置の場合
ＺｎＳの粉末が６８００ｆ／回収でき、原料に対する収
率は約６０％に達した。また生成粉末は障壁板の取り付
は部に大部分が堆積しており、粉末を採集するのに便利
であった。Furnace pressure ・・・・・・・・・・・・・・・・・・・・・
・ 50'rorr reaction temperature ・・・・・・・・・・・・
・・・・・・・・・・・・ 750°CH25 gas flow rate・
・・・・・・・・・・・・・・・ 0.4 N6/min
Flow rate of Ar gas for carrier of zinc vapor・・・・・・・・・・・・・・・2-
ON'/min reaction time ・・・・・・・・・・・・
...... Comparing the results of synthesis over 100 hours, (1) In the case of the conventional device, a ZnS compound was synthesized in the tubular reaction tube, but most of it was bulk ZnS, and powder The amount of ZnS was 1050 g, which is about 10% of the input raw material. (2) In the case of the apparatus of the present invention, 6800 f/ZnS powder could be recovered, and the yield based on the raw material reached about 60%. Also, most of the generated powder was deposited on the area where the barrier plate was attached, making it convenient to collect the powder.
以上の結果から本発明の装置によると気相合成法による
生成粉末の収率が向上することが分かった。From the above results, it was found that the apparatus of the present invention improves the yield of powder produced by vapor phase synthesis.
ハ１発明の効果
以上に説明したように本発明の化合物粉末の気相合成装
置によれば、反応室内での原料ガスの流れが乱流化し、
原料ガス種の衝突頻度が向上するので、化合物粉末を収
率良く製造できる効果があるものである。C1 Effects of the Invention As explained above, according to the compound powder vapor phase synthesis apparatus of the present invention, the flow of the raw material gas in the reaction chamber becomes turbulent.
Since the collision frequency of raw material gas species is improved, compound powder can be produced with high yield.
第１図は本発明の装置の具体例を示す断面図である。第
２図は従来の化合物の気相合成装置の断面図である。
（１）・・・ヒーター、
（２）・・・原料ガス供給ノズル、
（３）・・・排気管、 （４）・・・堆積物、
（５）・・・障壁板、 （６）・・・反応管、
矢印・・・ガスの流れ。
代理人 弁理士 １）中 理 夫
第１図
第２図FIG. 1 is a sectional view showing a specific example of the device of the present invention. FIG. 2 is a sectional view of a conventional compound vapor phase synthesis apparatus. (1)...Heater, (2)...Source gas supply nozzle, (3)...Exhaust pipe, (4)...Deposit,
(5)...Barrier plate, (6)...Reaction tube,
Arrow: Gas flow. Agent Patent Attorney 1) Rio Naka Figure 1 Figure 2
Claims (1)
て加熱された反応管内で反応を起こさせて化合物を気相
合成する気相合成装置において、反応室内壁に１個或い
は複数個の障壁板をもうけたことを特徴とする化合物粉
末の気相合成装置 ２、障壁板がリング状であることを特徴とする特許請求
の範囲第１項記載の化合物粉末の気相合成装置 ３、原料ガスとしてＡｒガスをキャリアーガスとした金
属亜鉛蒸気とＨ＿２Ｓガス或いはＨ＿２Ｓｅガスを用い
てＺｎＳ或いはＺｎＳｅの粉末を合成することを特徴と
する特許請求の範囲第１項もしくは第２項記載の化合物
粉末の気相合成装置[Claims] 1. In a gas phase synthesis apparatus that has an exhaust pipe at one end and supplies a raw material gas from the other end to cause a reaction in a heated reaction tube to synthesize a compound in the gas phase, the inner wall of the reaction chamber A compound powder vapor phase synthesis apparatus 2 characterized in that one or more barrier plates are provided in the compound powder, and the compound powder vapor phase synthesis apparatus 2 as claimed in claim 1, characterized in that the barrier plate is ring-shaped. The vapor phase synthesis apparatus 3 synthesizes ZnS or ZnSe powder using metal zinc vapor and H_2S gas or H_2Se gas with Ar gas as a carrier gas as a raw material gas. Vapor phase synthesis device for compound powder according to item 2
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33507587A JPH01176440A (en) | 1987-12-30 | 1987-12-30 | Vapor phase synthesizing apparatus for producing powdery compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33507587A JPH01176440A (en) | 1987-12-30 | 1987-12-30 | Vapor phase synthesizing apparatus for producing powdery compound |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01176440A true JPH01176440A (en) | 1989-07-12 |
Family
ID=18284482
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33507587A Pending JPH01176440A (en) | 1987-12-30 | 1987-12-30 | Vapor phase synthesizing apparatus for producing powdery compound |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01176440A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101292862B1 (en) * | 2011-01-13 | 2013-08-02 | 한국수력원자력 주식회사 | Apparatus to filter gas of high temperature and high pressure |
-
1987
- 1987-12-30 JP JP33507587A patent/JPH01176440A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101292862B1 (en) * | 2011-01-13 | 2013-08-02 | 한국수력원자력 주식회사 | Apparatus to filter gas of high temperature and high pressure |
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