JP3369643B2 - Method for producing pyrolytic boron nitride compact - Google Patents
Method for producing pyrolytic boron nitride compactInfo
- Publication number
- JP3369643B2 JP3369643B2 JP16349893A JP16349893A JP3369643B2 JP 3369643 B2 JP3369643 B2 JP 3369643B2 JP 16349893 A JP16349893 A JP 16349893A JP 16349893 A JP16349893 A JP 16349893A JP 3369643 B2 JP3369643 B2 JP 3369643B2
- Authority
- JP
- Japan
- Prior art keywords
- pbn
- molded body
- boron nitride
- core metal
- core
- 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 - Fee Related
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 11
- 239000002184 metal Substances 0.000 claims description 23
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 5
- 229910052582 BN Inorganic materials 0.000 claims description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Landscapes
- Ceramic Products (AREA)
- Producing Shaped Articles From Materials (AREA)
- Chemical Vapour Deposition (AREA)
Description
【発明の詳細な説明】
【０００１】
【産業上の利用分野】本発明は熱分解窒化ほう素成形体
の製造方法、特にはクビレ部を有する耐熱性芯金を用い
る熱分解窒化ほう素成形体の製造方法に関するものであ
る。
【０００２】
【従来の技術】熱分解窒化ほう素（以下、ＰＢＮと略記
する）の成形体は従来から基材の上にＣＶＤ法でＰＢＮ
を成膜してＰＢＮ成形体を形成し、ついでこれを基材か
ら分離するという方法で作られており、この基材として
は通常グラファイト材が用いられている。そして、この
ＰＢＮと基材との分離はＰＢＮの蒸着反応終了後にこれ
を炉より取り出し、ＰＢＮを基材より引き抜くことによ
り行なわれている。
【０００３】
【発明が解決しようとする課題】しかし、このＰＢＮ成
形体の製造方法においてこの基材がクビレ部をもつよう
なものであるときには、このＰＢＮの基材からの引き抜
きが容易ではなく、例えばパイプ状のＰＢＮ成形体の製
造でも両端の開口部より寸法が小さく、クビレ部をもつ
ものは、そこが細いために引き抜くことができず、した
がってこれについてはこのＰＢＮ成形体と基材とを酸化
炉に入れ、 800℃程度で基材を酸化し、これを酸化除去
するという方法が採られているのであるが、この酸化に
は数日間という長時間が必要とされるし、ＰＢＮ表面も
酸化されるという懸念があり、したがってこれにはＰＢ
Ｎ成形体の製造に非常に長い日程を要するし、これがコ
ストアップの要因になるという欠点がある。
【０００４】
【課題を解決するための手段】本発明はこのような不
利、欠点を解決したＰＢＮの製造方法に関するものであ
り、これは耐熱性芯金上に、ＣＶＤ法によってＰＢＮを
堆積し、ついで該芯金を除去することよりなるＰＢＮ成
形体の製造方法において、クビレ部を有する耐熱性芯金
上に熱分解窒化ほう素を堆積してクビレ部を有する成形
体を形成し、該成形体から耐熱性芯金をクビレ部で切断
して取り出し、クビレ部を有する熱分解窒化ほう素成形
体を得ることを特徴とするものである。
【０００５】すなわち、本発明者らはクビレを有する耐
熱性芯金上にＰＢＮ成形体を形成したときのＰＢＮ成形
体の取得方法について種々検討した結果、これについて
はクビレ部を有する耐熱性芯金上にＣＶＤ法でＰＢＮを
成膜してクビレ部を有するＰＢＮ成形体を形成させたの
ち、この芯金をクビレ部で切断すると、この芯金がクビ
レ部を中心にして２分割されるので、この芯金を上下に
引き抜けばＰＢＮ成形体を容易に得ることができるとい
うことを見出し、これによれば芯金を長時間かけて酸化
除去する必要がなくなるので短時間で目的とするＰＢＮ
成形体を得ることができることを確認して本発明を完成
させた。以下にこれをさらに詳述する。
【０００６】
【作用】本発明はＰＢＮ成形体の製造方法、特にはクビ
レ部を有する耐熱性芯体を用いてＰＢＮ成形体を製造す
る方法に関するものであるが、これは前記したようにク
ビレ部を有する耐熱性芯体上にＣＶＤ法によってＰＢＮ
を成膜してクビレ部を有するＰＢＮ成形体を成形したの
ち、この芯金をクビレ部で切断してこの芯金を除去する
ことを特徴とするものであり、これによればＰＢＮ成形
体を短時間で容易に得ることができるという有利性が与
えられる。
【０００７】本発明によるＰＢＮ成形体の製造は特にク
ビレ部を有する耐熱性芯体上にＰＢＮを成膜する方法に
関するものであり、これはクビレ部を有する耐熱性芯金
上にＣＶＤ法によってＰＢＮを成膜させてクビレ部を有
するＰＢＮ成形体を形成させるのであるが、このままで
は芯金を形成するグラファイトとＰＢＮとの熱膨張率が
相違するとしても冷却時に芯金を引き抜くことができな
いので、本発明ではこの芯金をクビレ部を中心として上
下に切断し、この芯金を上下に引き出すこととしたもの
で、これによれば目的とするＰＢＮ成形体を容易に得る
ことができる。
【０００８】この芯金のクビレ部を中心として上下に切
断するには各種の方法があり、これはどのような方法で
行なってもよいが、これには図１に示した方法が例示さ
れる。図１は本発明によるＰＢＮ成形体の製造工程の縦
断面図を示したものであるが、これにはまず図１（ａ）
に示したように中心が中空部２でクビレ部３を有するグ
ラファイト製の芯金１が準備され、この芯金１には図１
（ｂ）に示したようにＣＶＤ法でＢＣｌ3 ガスとＮＨ3
ガスとの反応により生成したＰＢＮ膜４が成膜される。
【０００９】この方法では芯金１をクビレ部３で上下に
分別するために、図１（ｂ）、（ｃ）に示したように、
この成形体の上下部についたＰＢＮ部を切断除去したの
ち、図１（ｄ）に示したように芯金１の下部を万力など
で固定し、上部をパイプレンチなどで保持し、水平方向
に回転して芯金の中間の径小で薄い部分をねじきって芯
金１を上下に切断すると、冷却によってグラファイトと
ＰＢＮとの熱膨張率の差によって芯金１は容易に引き抜
けるので、これを引き抜けばクビレ部を有するＰＢＮ成
形品を容易に得ることができるという有利性が与えられ
る。
【００１０】
【実施例】つぎに本発明の実施例、比較例をあげる。実
施例１
中心部に直径８mmの中空部がある、直径20mm、長さ10cm
で中間部に10mmのクビレ部を有するグラファイト製の基
材（芯金）を電気炉内に設置し、この電気炉に真空ポン
プを接続して炉内を１Torrまで減圧したのち、ここにＢ
Ｃｌ3 ガス１リットル／分とＮＨ3 ガス２リットル／分
との混合ガスを供給し、10時間反応させて反応終了後に
Ｎ2 ガスを導入して冷却し、室温になってからこの基材
を取り出したところ、基材上にはＰＢＮが約１mmの厚さ
を被着していた。
【００１１】ついで、これを室温まで冷却後、この成形
体の上下部のＰＢＮ層を切断除去し、芯金部の下部を万
力で固定し、上部をパイプレンチで保持して水平方向に
回転してこの基材（芯金）のクビレ部を切断したのち、
２分された基材を上下方向に引き抜いたところ、クビレ
部をもつＰＢＮ成形体が得られ、この間の作業時間は約
10分間であった。
【００１２】比較例
実施例１で使用したグラファイト製基材と同形のクビレ
部を有しているが、中空部を有しないグラファイト基材
に実施例１と同じ方法でＰＢＮ膜を作成したが、この場
合には基材をクビレ部で切断せず、これを 800℃に保っ
た酸化炉内でグラファイト基材を酸化して除去したとこ
ろ、クビレ部をもつＰＢＮ成形体が得られたけれども、
これには基材の酸化除去に約１週間の時間が必要であっ
た。
【００１３】
【発明の効果】本発明はＰＢＮ成形体の製造方法に関す
るものであり、これは前記したようにクビレ部を有する
耐熱体芯金上に、ＣＶＤ法によってＰＢＮを堆積してク
ビレ部を有する成形体を形成し、ついで該芯金を除去す
ることよりなるＰＢＮ成形体の製造方法において、該芯
金の除去を該芯金のクビレ部の切断により行なうことを
特徴とするものであり、これによれば従来法のようにこ
の芯金の除去をその酸化処理で行なう必要がないので、
短時間で容易に目的とするＰＢＮ成形体を得ることがで
きるという有利性が与えられる。Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a thermally decomposed boron nitride molded article, and more particularly to a thermally decomposed boron nitride molded article using a heat-resistant core having a cracked portion. And a method for producing the same. 2. Description of the Related Art Conventionally, a molded body of pyrolytic boron nitride (hereinafter abbreviated as PBN) has been conventionally formed on a base material by a PBN method.
Is formed by forming a PBN molded body and then separating the PBN molded body from a base material, and a graphite material is usually used as the base material. The separation of the PBN from the substrate is performed by taking out the PBN from the furnace after the completion of the PBN deposition reaction and extracting the PBN from the substrate. [0003] The present invention is to provide, however, when this method of manufacturing a PBN moldings this substrate is such that with the neck portion is not easily pulled out from the base material of the PBN, For example, even in the production of a pipe-shaped PBN molded product, the one having a smaller size than the openings at both ends and having a cracked portion cannot be pulled out due to its thinness. A method has been adopted in which the substrate is oxidized at about 800 ° C and then oxidized and removed at around 800 ° C. This oxidation requires a long time of several days, and the PBN surface is There is concern that it will be oxidized, and
It takes a very long time to manufacture the N molded body, and this has the disadvantage of increasing the cost. [0004] The present invention relates to a method for producing a PBN which has solved the above disadvantages and drawbacks. This method comprises depositing PBN on a heat-resistant core by a CVD method . Then , a method for producing a PBN molded body, comprising removing the core metal, the heat-resistant core metal having a cracked portion.
Forming with cracks by depositing pyrolytic boron nitride on top
A body is formed, and a heat-resistant core metal is cut from the molded body at a cracked portion.
Pyrolytic boron nitride molding with cracks
It is characterized by obtaining a body . That is, the present inventors have conducted various studies on a method of obtaining a PBN molded body when a PBN molded body is formed on a cracked heat-resistant cored metal. After having formed a PBN molded body having a neck portion by forming a PBN by CVD on, cutting the metal core by the neck portion then, since the metal core is divided into two around the neck portion, It has been found that a PBN molded body can be easily obtained by pulling this core bar up and down. According to this, it is not necessary to oxidize and remove the core bar over a long period of time.
After confirming that a molded article can be obtained, the present invention was completed. This will be described in more detail below. The present invention relates to a method for producing a PBN molded article, and more particularly to a method for producing a PBN molded article using a heat-resistant core having a cracked portion. PBN on a heat-resistant core having
After forming a PBN molded body having a concave portion by forming a film, the core metal is cut at the concave portion and the core metal is removed. The advantage is that it can be easily obtained in a short time. The production of a PBN molded article according to the present invention particularly relates to a method of forming a PBN film on a heat-resistant core having a cracked portion, which is formed on a heat-resistant core having a cracked portion by CVD. Is formed to form a PBN molded body having a cracked portion. However, if the thermal expansion coefficients of graphite and PBN forming the core metal are different, the core metal cannot be pulled out during cooling. In the present invention, the core is cut up and down around the cracked portion, and the core is pulled up and down, whereby the desired PBN molded body can be easily obtained. [0008] This cored bar is cut up and down around the cracked part.
There are various methods for disconnecting , and any method may be used. For example, the method shown in FIG. 1 is exemplified. FIG. 1 is a longitudinal sectional view showing a manufacturing process of a PBN molded body according to the present invention.
As shown in FIG. 1, a graphite core 1 having a hollow portion 2 and a concave portion 3 is prepared.
As shown in (b), BCl 3 gas and NH 3
The PBN film 4 generated by the reaction with the gas is formed. In this method, since the cored bar 1 is separated vertically by the crack portion 3, as shown in FIGS. 1 (b) and 1 (c),
After cutting and removing the PBN portions attached to the upper and lower portions of the molded body, as shown in FIG. Rotate to the center of the metal core
When cutting the gold 1 vertically, since the metal core 1 by the difference in thermal expansion coefficient between the graphite and PBN by cooling easily pulled out, PBN formed with neck portion is pulled out of this
Given the advantage that shapes can be obtained easily
You. Next, examples of the present invention and comparative examples will be described. Example 1 There is a hollow part having a diameter of 8 mm at the center, a diameter of 20 mm and a length of 10 cm.
A graphite base material (core metal) having a 10 mm crack portion in the middle is set in an electric furnace, and a vacuum pump is connected to the electric furnace to reduce the pressure in the furnace to 1 Torr.
A mixed gas of 1 liter / minute of Cl 3 gas and 2 liter / minute of NH 3 gas was supplied, and the mixture was reacted for 10 hours. After the reaction was completed, N 2 gas was introduced and cooled. Upon removal, the substrate had a PBN thickness of about 1 mm. Then, after cooling to room temperature, the upper and lower PBN layers of the molded body are cut and removed, the lower part of the cored bar is fixed with a vice, and the upper part is held by a pipe wrench and rotated horizontally. Then, after cutting the cracked part of this substrate (core metal),
When the two-minute base material was pulled out in the vertical direction, a PBN molded body having a cracked portion was obtained.
10 minutes. Comparative Example A PBN film was formed on a graphite substrate having the same shape as that of the graphite substrate used in Example 1 but having no hollow portion by the same method as in Example 1. In this case, the base material was not cut at the cracked part, and the graphite base material was oxidized and removed in an oxidation furnace maintained at 800 ° C. As a result, a PBN molded body having a cracked part was obtained.
This required about one week for the oxidative removal of the substrate . The present invention relates to a method for manufacturing a PBN molded body, which comprises depositing PBN on a heat-resistant core having a cracked portion by a CVD method to form the cracked portion as described above. Forming a molded body having, and then removing the core metal, a method for producing a PBN molded body, characterized in that the core metal is removed by cutting a crack portion of the core metal, According to this, it is not necessary to remove the core metal by the oxidation treatment as in the conventional method.
The advantage is that the desired PBN compact can be easily obtained in a short time.
【図面の簡単な説明】
【図１】 （ａ）〜（ｄ）は本発明によるＰＢＮ成形体
製造工程の工程順の縦断面図を示したものである。
【符号の説明】１
…芯金、 ２…中空部、３…クビレ部、４…ＰＢＮ膜、
５…ＰＢＮ成形体。 BRIEF DESCRIPTION OF THE DRAWINGS FIGS. 1 (a) to 1 (d) are longitudinal sectional views in the order of the steps of manufacturing a PBN compact according to the present invention. [Explanation of Signs ] 1 ... core metal, 2 ... hollow part, 3 ... cracked part, 4 ... PBN film,
5 ... PBN molded body .
───────────────────────────────────────────────────── フロントページの続き (72)発明者 佐藤 健司 群馬県安中市磯部２丁目13番１号 信越 化学工業株式会社 群馬事業所内 (56)参考文献 特開 平４−197701（ＪＰ，Ａ) 特開 昭63−189223（ＪＰ，Ａ) 特表 昭61−502066（ＪＰ，Ａ) 米国特許1598059（ＵＳ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) B28B 1/30 C04B 35/583 C23C 16/01 ──────────────────────────────────────────────────続 き Continuation of the front page (72) Inventor Kenji Sato 2-3-1-1, Isobe, Annaka-shi, Gunma Shin-Etsu Chemical Co., Ltd. Gunma Office (56) References JP-A-4-197701 (JP, A) JP-A-63-189223 (JP, A) JP-T-61-502066 (JP, A) U.S. Pat. No. 15,980,59 (US, A) (58) Fields investigated (Int. Cl. 7 , DB name) B28B 1/30 C04B 35/583 C23C 16/01
Claims (1)
解窒化ほう素を堆積し、ついで該芯金を除去することよ
りなる熱分解窒化ほう素成形体の製造方法において、ク
ビレ部を有する耐熱性芯金上に熱分解窒化ほう素を堆積
してクビレ部を有する成形体を形成し、該成形体から耐
熱性芯金をクビレ部で切断して取り出し、クビレ部を有
する熱分解窒化ほう素成形体を得ることを特徴とする熱
分解窒化ほう素成形体の製造方法。(57) [Claims 1] A pyrolytic boron nitride molded body formed by depositing pyrolytic boron nitride on a heat-resistant core metal by a CVD method and then removing the core metal. in the method of production, click
Pyrolytic boron nitride deposited on heat-resistant core metal with knurls
Forming a molded body having a cracked portion,
Cut and remove the thermal core metal at the cracked part, and
A method for producing a thermally decomposed boron nitride molded body, comprising obtaining a thermally decomposed boron nitride molded body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16349893A JP3369643B2 (en) | 1993-07-01 | 1993-07-01 | Method for producing pyrolytic boron nitride compact |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16349893A JP3369643B2 (en) | 1993-07-01 | 1993-07-01 | Method for producing pyrolytic boron nitride compact |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0716815A JPH0716815A (en) | 1995-01-20 |
| JP3369643B2 true JP3369643B2 (en) | 2003-01-20 |
Family
ID=15775013
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16349893A Expired - Fee Related JP3369643B2 (en) | 1993-07-01 | 1993-07-01 | Method for producing pyrolytic boron nitride compact |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3369643B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5827371A (en) * | 1995-05-03 | 1998-10-27 | Chorus Corporation | Unibody crucible and effusion source employing such a crucible |
| US5820681A (en) * | 1995-05-03 | 1998-10-13 | Chorus Corporation | Unibody crucible and effusion cell employing such a crucible |
-
1993
- 1993-07-01 JP JP16349893A patent/JP3369643B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0716815A (en) | 1995-01-20 |
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