JPH04231317A - Refining method of dichlorosilane - Google Patents
Refining method of dichlorosilaneInfo
- Publication number
- JPH04231317A JPH04231317A JP41517490A JP41517490A JPH04231317A JP H04231317 A JPH04231317 A JP H04231317A JP 41517490 A JP41517490 A JP 41517490A JP 41517490 A JP41517490 A JP 41517490A JP H04231317 A JPH04231317 A JP H04231317A
- Authority
- JP
- Japan
- Prior art keywords
- dichlorosilane
- storage tank
- impurities
- oxygen
- carbon dioxide
- 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
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 10
- 238000007670 refining Methods 0.000 title abstract 2
- 238000003860 storage Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000010992 reflux Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 14
- 239000012535 impurity Substances 0.000 abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 7
- 239000010703 silicon Substances 0.000 abstract description 7
- 229910052710 silicon Inorganic materials 0.000 abstract description 7
- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 abstract description 4
- UBAZGMLMVVQSCD-UHFFFAOYSA-N carbon dioxide;molecular oxygen Chemical compound O=O.O=C=O UBAZGMLMVVQSCD-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000009835 boiling Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 210000000608 photoreceptor cell Anatomy 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は、ジクロルシランの精製
方法、詳しくは、酸素、窒素、一酸化炭素、二酸化炭素
等のジクロルシランよりも沸点の低いガスを含有しない
ジクロルシランを製造するためのジクロルシランの精製
方法に関する。[Industrial Application Field] The present invention relates to a method for purifying dichlorosilane, and more particularly, the purification of dichlorosilane for producing dichlorosilane that does not contain gases having a boiling point lower than that of dichlorosilane, such as oxygen, nitrogen, carbon monoxide, and carbon dioxide. Regarding the method.
【０００２】0002
【従来の技術】エレクトロ産業市場の急成長に伴いトリ
クロルシラン、ジクロルシラン、モノシランは、ＩＣ、
太陽電池、光感光体ドラム等における半導体薄膜を形成
するための原料ガスとして急速に需要が増加している。
特にジクロルシランはエピタキシャルシリコン及び窒化
珪素成膜用原料として高純度のものが要求されている。[Prior Art] With the rapid growth of the electronic industry market, trichlorosilane, dichlorosilane, and monosilane have become increasingly popular in IC,
Demand is rapidly increasing as a raw material gas for forming semiconductor thin films in solar cells, photoreceptor drums, etc. In particular, dichlorosilane is required to have high purity as a raw material for forming epitaxial silicon and silicon nitride films.
【０００３】ジクロルシランの主な合成法として、１）
トリクロルシランの不均化反応と２）シリコンからの直
接合成法、例えばシリコンと塩化水素との反応やシリコ
ンと水素と四塩化珪素との反応による合成がある。[0003] The main methods for synthesizing dichlorosilane are 1)
2) Direct synthesis from silicon, such as reaction of silicon with hydrogen chloride or reaction of silicon, hydrogen, and silicon tetrachloride.
【０００４】合成されたジクロルシランは、モレキュラ
シーブ等の吸着剤による吸着精製、蒸留精製あるいは両
者の組合せにより精製した後、製品貯槽内に液体として
蓄えられ、ボンベ等の容器に充填されて各種の用途に供
されている。After the synthesized dichlorosilane is purified by adsorption using an adsorbent such as molecular sieve, distillation, or a combination of both, it is stored as a liquid in a product storage tank and filled into containers such as cylinders for various purposes. It is provided.
【０００５】しかし、従来の精製方法では、ジクロルシ
ランよりも高沸点の不純物に対しては効果的であるが、
低沸点のものに対しては十分な効果をあげることはでき
ないので、数種の低沸点不純物が混入されたままで使用
されているのが現状である。However, although conventional purification methods are more effective against impurities with higher boiling points than dichlorosilane,
Since it is not sufficiently effective against substances with low boiling points, it is currently used with several types of low-boiling point impurities mixed in.
【０００６】[0006]
【発明が解決しようとする課題】高純度が要求される半
導体等の用途には、酸素、二酸化炭素、窒素等の不純物
の混入はエピタキシャルシリコンや窒化珪素成膜等の製
品の品質に大きな影響を与えるので、これらを含まない
ジクロルシランが望まれていた。[Problem to be solved by the invention] In applications such as semiconductors that require high purity, the contamination of impurities such as oxygen, carbon dioxide, and nitrogen has a significant impact on the quality of products such as epitaxial silicon and silicon nitride films. Therefore, a dichlorosilane that does not contain these substances was desired.
【０００７】本発明の目的は、高純度ジクロルシランを
得るためのジクロルシランの精製方法を提供することに
ある。An object of the present invention is to provide a method for purifying dichlorosilane to obtain highly pure dichlorosilane.
【０００８】[0008]
【課題を解決するための手段】すなわち、本発明は、液
体ジクロルシランの貯槽内でジクロルシランの還流下に
保持することを特徴とするジクロルシランの精製方法で
ある。[Means for Solving the Problems] That is, the present invention is a method for purifying dichlorosilane, which is characterized by maintaining dichlorosilane under reflux in a liquid dichlorosilane storage tank.
【０００９】以下、さらに詳しく本発明について説明す
る。本発明が適用されるジクロルシランは、どのような
製法によって得られたものであってもよく、その例とし
ては上記１）又は２）の方法によるものがあげられる。The present invention will be explained in more detail below. The dichlorosilane to which the present invention is applied may be obtained by any manufacturing method, and examples thereof include the method 1) or 2) above.
【００１０】ジクロルシランは液化されて貯槽内で貯蔵
されるが、この際に重要なことは、ジクロルシランを還
流下に保持することである。このように保持することに
よってジクロルシランよりも低沸点の不純物は液化され
ずに未凝縮ガスとして系内圧力を高めその増加分が系外
に排出される。[0010] Dichlorosilane is liquefied and stored in a storage tank, and in this case it is important to maintain dichlorosilane under reflux. By holding the impurities in this way, the impurities having a boiling point lower than that of dichlorosilane are not liquefied, but are turned into uncondensed gases, increasing the pressure within the system, and the increased pressure is discharged from the system.
【００１１】貯槽としては、還流に必要な熱を与えられ
るものが採用され、具体的にはジャケット付貯槽やその
他の加熱装置を備えた貯槽があげられる。還流コンデン
サーとしては、蒸発したジクロルシランを凝縮し凝縮液
を貯槽に戻すことができるものであればどのような型式
のものであってもよい。本発明においては、装置の清浄
化が行いやすい構造のものがよく、それにはジャケット
付貯槽と多管式熱交換器の組み合わせがよい。[0011] As the storage tank, one that can provide the heat necessary for reflux is used, and specific examples include a jacketed storage tank and a storage tank equipped with other heating devices. The reflux condenser may be of any type as long as it can condense the evaporated dichlorosilane and return the condensate to the storage tank. In the present invention, it is preferable to have a structure that allows easy cleaning of the apparatus, and a combination of a jacketed storage tank and a multi-tubular heat exchanger is preferable for this purpose.
【００１２】還流量については特に制約はないが、少な
すぎると低沸点不純物の除去が十分でなくなり、一方、
多すぎると熱的・設備的に不経済となるので、貯槽容積
と貯液量にもよるが、１時間あたり貯液量の１／１００
〜１／１を還流するのが望ましい。貯液温度は大気圧以
上の圧力を保持できる８．２℃以上が好ましい。There are no particular restrictions on the reflux amount, but if it is too small, low-boiling impurities will not be removed sufficiently;
If it is too large, it will be uneconomical in terms of heat and equipment, so it depends on the storage tank volume and the amount of liquid stored, but it should be 1/100 of the amount of liquid stored per hour.
It is desirable to reflux ~1/1. The temperature of the storage liquid is preferably 8.2° C. or higher to maintain a pressure higher than atmospheric pressure.
【００１３】[0013]
【実施例】以下、実施例と比較例をあげてさらに具体的
に本発明を説明する。[Examples] The present invention will be explained in more detail below with reference to Examples and Comparative Examples.
【００１４】実施例１
２５０リットルのジャケット付液体ジクロルシラン貯槽
に、０．７ｍ２ の伝熱面積を有するコンデンサーを設
置し、それを−２０℃の冷媒で冷却した。コンデンサー
出口にはＰＩＣを０．５Ｋｇ／ｃｍ２ にして設置し、
またジャケットには１９℃の冷却水を流した。Example 1 A condenser having a heat transfer area of 0.7 m2 was installed in a 250 liter jacketed liquid dichlorosilane storage tank, and the condenser was cooled with a -20°C refrigerant. A PIC is installed at the condenser outlet with a pressure of 0.5Kg/cm2.
Furthermore, cooling water at 19° C. was flowed through the jacket.
【００１５】この貯槽に２００リットルのジクロルシラ
ンを入れ、還流下に保持し上昇した圧力分のガスを系外
に随時排出した。１日後、貯槽下部よりジクロルシラン
を抜取り４０リットルのボンベに充填した。200 liters of dichlorosilane was placed in this storage tank, maintained under reflux, and gas corresponding to the increased pressure was discharged from the system at any time. One day later, dichlorosilane was extracted from the bottom of the storage tank and filled into a 40 liter cylinder.
【００１６】ボンベ内のジクロルシランの不純物をガス
クロマトグラフにより分析した結果、窒素、酸素とアル
ゴンの和及び二酸化炭素はいずれも検出されなかった。
なお、窒素、酸素とアルゴンの和及び二酸化炭素の検出
限界はいずれも０．１ｐｐｍである。As a result of gas chromatograph analysis of impurities in dichlorosilane in the cylinder, neither nitrogen, the sum of oxygen and argon, nor carbon dioxide were detected. Note that the detection limits for nitrogen, the sum of oxygen and argon, and carbon dioxide are all 0.1 ppm.
【００１７】比較例１
コンデンサーの冷媒とジャケットの冷却水を止め、ＰＩ
Ｃバルブを閉止したこと以外は実施例１と同様にしてボ
ンベに充填し不純物を分析したところ、窒素４ｐｐｍ、
二酸化炭素１ｐｐｍ及び酸素とアルゴンの和は０．１ｐ
ｐｍであった。Comparative Example 1 Stop the refrigerant in the condenser and the cooling water in the jacket, and turn off the PI
A cylinder was filled in the same manner as in Example 1 except that the C valve was closed, and impurities were analyzed.
Carbon dioxide 1ppm and the sum of oxygen and argon is 0.1p
It was pm.
【００１８】[0018]
【発明の効果】本発明により得られたジクロルシランに
は、窒素、酸素及び二酸化炭素の混入量はいずれも検出
限界（０．１ｐｐｍ）以下にすることができるので、高
品質のエピタキシャルシリコンや窒化珪素膜等の製品を
製造することができる。Effects of the Invention Since the dichlorosilane obtained by the present invention can contain nitrogen, oxygen, and carbon dioxide in amounts below the detection limit (0.1 ppm), it can be used for high-quality epitaxial silicon and silicon nitride. Products such as membranes can be manufactured.
Claims (1)
ルシランの還流下に保持することを特徴とするジクロル
シランの精製方法。1. A method for purifying dichlorosilane, which comprises maintaining dichlorosilane under reflux in a liquid dichlorosilane storage tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP41517490A JPH04231317A (en) | 1990-12-27 | 1990-12-27 | Refining method of dichlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP41517490A JPH04231317A (en) | 1990-12-27 | 1990-12-27 | Refining method of dichlorosilane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04231317A true JPH04231317A (en) | 1992-08-20 |
Family
ID=18523571
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP41517490A Pending JPH04231317A (en) | 1990-12-27 | 1990-12-27 | Refining method of dichlorosilane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04231317A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104140106A (en) * | 2014-07-28 | 2014-11-12 | 中国恩菲工程技术有限公司 | Method for treating polycrystalline silicon reduction tail gas |
-
1990
- 1990-12-27 JP JP41517490A patent/JPH04231317A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104140106A (en) * | 2014-07-28 | 2014-11-12 | 中国恩菲工程技术有限公司 | Method for treating polycrystalline silicon reduction tail gas |
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