JPS6355111A - Method for grinding silicon - Google Patents
Method for grinding siliconInfo
- Publication number
- JPS6355111A JPS6355111A JP19562486A JP19562486A JPS6355111A JP S6355111 A JPS6355111 A JP S6355111A JP 19562486 A JP19562486 A JP 19562486A JP 19562486 A JP19562486 A JP 19562486A JP S6355111 A JPS6355111 A JP S6355111A
- Authority
- JP
- Japan
- Prior art keywords
- silicon
- copper
- grinding
- copper compound
- ball mill
- 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
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 26
- 239000010703 silicon Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052802 copper Inorganic materials 0.000 claims abstract description 15
- 239000010949 copper Substances 0.000 claims abstract description 15
- 150000001880 copper compounds Chemical class 0.000 claims abstract description 14
- 239000005749 Copper compound Substances 0.000 claims abstract description 13
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims abstract description 7
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims abstract description 7
- 229940045803 cuprous chloride Drugs 0.000 claims abstract description 7
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 6
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 6
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229960003280 cupric chloride Drugs 0.000 claims abstract description 3
- 229960004643 cupric oxide Drugs 0.000 claims abstract description 3
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229940112669 cuprous oxide Drugs 0.000 claims abstract description 3
- 238000010298 pulverizing process Methods 0.000 claims description 11
- 238000007711 solidification Methods 0.000 abstract description 2
- 230000008023 solidification Effects 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 22
- 230000000694 effects Effects 0.000 description 6
- 239000011863 silicon-based powder Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000005046 Chlorosilane Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910004028 SiCU Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical group Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 description 1
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Crushing And Grinding (AREA)
- Silicon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
〔技術分野〕
本発明はボールミルを用いたケイ素の粉砕方法に関する
。DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to a method of pulverizing silicon using a ball mill.
ケイ素粉末は、近年エレクトロニクス工業材料としてそ
の重要性を増しているテトラクロロシラン（ＳｉＣｕ、
）やヘキサクロロジシラン（ｓｉｔ ｅＱＴｌ ）の原
料として、あるいはセラミックス材料として注目されて
居る窒化ケイ素の原料として、需要が急激に増大してい
る。これら各用途に用いられるケイ素粉末としては反応
効率の点から微粒子で非酸化の物が望まれている。Silicon powder is tetrachlorosilane (SiCu,
) and hexachlorodisilane (sit eQTl), and as a raw material for silicon nitride, which is attracting attention as a ceramic material, demand is rapidly increasing. From the viewpoint of reaction efficiency, it is desired that the silicon powder used in each of these applications be fine-grained and non-oxidized.
従来、ケイ素の粉砕はスタンプミル、ジェットミル、ボ
ールミルに依って行われて居た。しかしスタンプミルで
は微粉末を得る事は困難であり、またジェットミルでは
非酸化性雰囲気での粉砕に問題がある。ボールミルを用
いた粉砕では非酸化性雰囲気の粉砕を容易に得られるが
、ケイ素を乾式で粉砕した場合、微粉末になる前にポッ
トの内壁にケイ素が付着し、固化して剥離に手間取る等
のため粉砕効率が極めて悪い欠点がある。Conventionally, silicon has been pulverized using stamp mills, jet mills, and ball mills. However, it is difficult to obtain fine powder with a stamp mill, and there are problems with grinding in a non-oxidizing atmosphere with a jet mill. Grinding using a ball mill can easily produce a non-oxidizing atmosphere, but when silicon is dry-ground, silicon adheres to the inner wall of the pot before it becomes a fine powder, solidifies, and takes time to peel off. Therefore, it has the disadvantage of extremely low pulverization efficiency.
本発明者等はボールミルを用いてケイ素を粉砕する場合
、銅、銅化合物の存在下で粉砕すれば、該ケイ素が粉砕
途中にポット内壁に付着固化せず効率良く粉砕できるこ
とを見出した。The present inventors have found that when silicon is crushed using a ball mill, if the silicon is crushed in the presence of copper or a copper compound, the silicon does not adhere to the inner wall of the pot during the crushing process and can be crushed efficiently.
本発明に依れば、ボールミルを用いたケイ素の粉砕方法
において、銅ないし銅化合物の存在下でケイ素を粉砕す
ることを特徴とするケイ素の粉砕方法が提供される。According to the present invention, there is provided a method for pulverizing silicon using a ball mill, characterized in that silicon is pulverized in the presence of copper or a copper compound.
本発明に於いて銅化合物とは、特に限定されず、例えば
、塩化第一銅、塩化第二銅、酸化第一銅、酸化第二銅が
用いられる。In the present invention, the copper compound is not particularly limited, and for example, cuprous chloride, cupric chloride, cuprous oxide, and cupric oxide are used.
銅ないし銅化合物の添加量は銅換算で０．１重量％以上
２０重量％以下である事が望ましく、０．１重量％より
少ないと効果がなく、また２０重量％を超えてもケイ素
の付着を防止する効果はそれ程向上しない。The amount of copper or copper compound added is preferably 0.1% by weight or more and 20% by weight or less in terms of copper; less than 0.1% by weight has no effect, and more than 20% by weight may cause silicon adhesion. The effect of preventing this does not improve that much.
粉砕の際、銅ないし銅化合物をケイ素粉末と共にボール
ミルに入れ、同時に粉砕する。粉砕は通常のボールミル
の粉砕と同様に行えばよい。During pulverization, copper or copper compound is placed in a ball mill with silicon powder and pulverized at the same time. The pulverization may be carried out in the same manner as in a normal ball mill.
〔発明の効果〕
本発明の粉砕方法によれば、ボールミルを用いてケイ素
を粉砕する際、ケイ素がポット内壁に付着固化せず、効
率良く粉砕する事が出来る。[Effects of the Invention] According to the pulverization method of the present invention, when silicon is pulverized using a ball mill, silicon does not adhere to the inner wall of the pot and solidify, and the pulverization can be carried out efficiently.
この理由は１次のように推察される。即ち、添加した銅
ないし銅化合物が粉砕途上においてメカノケミカル効果
によってシリコン表面に薄層を形成し表面活性を低下さ
せる事によりシリコン粉末表面に＃ｌ量に存在するシラ
ノール基あるいはシロキサン基を媒体とした凝集、さら
には粉砕材壁面との付着を防止するためと考えられる。The reason for this is presumed to be as follows. That is, the added copper or copper compound forms a thin layer on the silicon surface due to the mechanochemical effect during the grinding process, reducing the surface activity, thereby using the silanol groups or siloxane groups present in #l amount on the silicon powder surface as a medium. This is thought to be to prevent agglomeration and further adhesion to the wall surface of the crushed material.
前記の方法で得られたケイ素と銅、銅化合物あるいはこ
れら両者との混合粉は、たとえばケイ素粉末の塩素化に
よるクロロシランの製造に際し、原料粉末として供給さ
れこの場合は、ケイ素と銅、銅化合物との共存がポリク
ロロシランの収率を向上させる効果がある。The mixed powder of silicon, copper, a copper compound, or both obtained by the above method is supplied as a raw material powder, for example, when producing chlorosilane by chlorinating silicon powder. The coexistence of these has the effect of improving the yield of polychlorosilane.
実施例１
ステンレスｉｌＱポットに径２０ｍｍのステンレス製球
４０個、径１５ｍｍのステンレス製球４０個を平均粒径
２ｎ＋ｍのケイ素４５０ｇ、塩化第一銅粉Ｌｏｇと共に
入れ２４時間粉砕を行なった。粉砕後ケイ素はポット内
壁に付着固化する事なく、平均粒径は１μｍであった。Example 1 Forty stainless steel balls with a diameter of 20 mm and 40 stainless steel balls with a diameter of 15 mm were placed in a stainless steel ILQ pot together with 450 g of silicon having an average particle size of 2n+m and cuprous chloride powder Log, and pulverized for 24 hours. After pulverization, silicon did not adhere to the inner wall of the pot and solidify, and the average particle size was 1 μm.
比較例１
塩化第一銅を用いなかった他は実施例１と同様の粉砕を
行なった。粉砕後ケイ素はポット内壁に付着固化して居
り剥離に手間取る上、平均粒径は１００μｍであった。Comparative Example 1 Grinding was carried out in the same manner as in Example 1, except that cuprous chloride was not used. After pulverization, the silicon adhered to the inner wall of the pot and was hard to peel off, and the average particle size was 100 μm.
実施例２〜５
塩化第一銅の量を変えた他は実施例１と同様の粉砕を行
った。結果は表１の通りである。Examples 2 to 5 Grinding was carried out in the same manner as in Example 1, except that the amount of cuprous chloride was changed. The results are shown in Table 1.
表１
塩化第一銅の量 粉砕後の平均 ポット内壁への実施
例・（銅換算）〔重量％〕 粒径〔μｍ〕 付着固化
の有無実施例２ ０．０１ ９４
、ｐ１１３０．１１．２無
１１４２０ ０．８無
１１５３０ ０．９無
実施例６〜８Table 1 Amount of cuprous chloride Average after crushing Examples on the inner wall of the pot (copper equivalent) [wt%] Particle size [μm] Presence or absence of adhesion and solidification Example 2 0.01 94
, p1130.11.2 No 11420 0.8 No 11530 0.9 No Examples 6-8
Claims (1)
ないし銅化合物の存在下でケイ素を粉砕することを特徴
とするケイ素の粉砕方法。 ２、上記銅化合物が塩化第一銅、塩化第二銅、酸化第一
銅、酸化第二銅よりなる群から選ばれた少くとも１種で
ある特許請求の範囲第１項に記載の方法。 ３、銅ないし銅化合物の添加量が銅換算で０．１重量％
以上２０重量％以下である特許請求の範囲第１項に記載
の方法。[Scope of Claims] 1. A method for pulverizing silicon using a ball mill, which comprises pulverizing silicon in the presence of copper or a copper compound. 2. The method according to claim 1, wherein the copper compound is at least one selected from the group consisting of cuprous chloride, cupric chloride, cuprous oxide, and cupric oxide. 3. Addition amount of copper or copper compound is 0.1% by weight in terms of copper
The method according to claim 1, wherein the amount is 20% by weight or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19562486A JPS6355111A (en) | 1986-08-22 | 1986-08-22 | Method for grinding silicon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19562486A JPS6355111A (en) | 1986-08-22 | 1986-08-22 | Method for grinding silicon |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6355111A true JPS6355111A (en) | 1988-03-09 |
Family
ID=16344263
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19562486A Pending JPS6355111A (en) | 1986-08-22 | 1986-08-22 | Method for grinding silicon |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6355111A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0893408A1 (en) * | 1997-07-24 | 1999-01-27 | Pechiney Electrometallurgie | Process for manufacturing active silicon powder for the preparation of alkyl or aryle halogenosilanes |
-
1986
- 1986-08-22 JP JP19562486A patent/JPS6355111A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0893408A1 (en) * | 1997-07-24 | 1999-01-27 | Pechiney Electrometallurgie | Process for manufacturing active silicon powder for the preparation of alkyl or aryle halogenosilanes |
| FR2766474A1 (en) * | 1997-07-24 | 1999-01-29 | Pechiney Electrometallurgie | PROCESS FOR THE MANUFACTURE OF ACTIVE SILICON POWDER FOR THE PREPARATION OF ALKYL- OR ARYL-HALOGENOSILANES |
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