JPH03115140A - Boron nitride film, method for forming boron nitride film, boron nitride-coated fiber and composite material having boron-nitride- coated fiber - Google Patents
Boron nitride film, method for forming boron nitride film, boron nitride-coated fiber and composite material having boron-nitride- coated fiberInfo
- Publication number
- JPH03115140A JPH03115140A JP2179400A JP17940090A JPH03115140A JP H03115140 A JPH03115140 A JP H03115140A JP 2179400 A JP2179400 A JP 2179400A JP 17940090 A JP17940090 A JP 17940090A JP H03115140 A JPH03115140 A JP H03115140A
- Authority
- JP
- Japan
- Prior art keywords
- fibers
- boron nitride
- matrix
- boron
- fiber
- 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
- 239000000835 fiber Substances 0.000 title claims abstract description 62
- 239000002131 composite material Substances 0.000 title claims abstract description 15
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 34
- 229910052582 BN Inorganic materials 0.000 title claims description 32
- 238000000034 method Methods 0.000 title claims description 11
- 239000002657 fibrous material Substances 0.000 title 1
- 238000000576 coating method Methods 0.000 claims abstract description 23
- 239000011159 matrix material Substances 0.000 claims abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 14
- 239000012159 carrier gas Substances 0.000 claims abstract description 11
- 239000000919 ceramic Substances 0.000 claims abstract description 8
- 229910052796 boron Inorganic materials 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000011521 glass Substances 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 4
- 239000011248 coating agent Substances 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 claims description 3
- 239000002241 glass-ceramic Substances 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 3
- 239000012815 thermoplastic material Substances 0.000 claims description 3
- 229920001187 thermosetting polymer Polymers 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 2
- 230000003993 interaction Effects 0.000 claims description 2
- 229910052863 mullite Inorganic materials 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 239000000376 reactant Substances 0.000 abstract description 6
- 229910015844 BCl3 Inorganic materials 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000005452 bending Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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Abstract
Description
【発明の詳細な説明】
［発明の目的］
〈産業上の利用分野〉
本発明は、繊維の被覆に関し、特に窒化硼素の厚膜を繊
維に被覆する方法及びその結果得られる被覆繊維に関す
る。DETAILED DESCRIPTION OF THE INVENTION OBJECTS OF THE INVENTION <Industrial Field of Application> The present invention relates to the coating of fibers, and more particularly to a method of coating fibers with a thick film of boron nitride and the resulting coated fibers.
〈従来の技術〉
ガラス、ガラス−セラミック、セラミックス、金属、熱
硬化性材料及び熱可塑性材料は、繊維強化によって強度
が増加し、適用範囲を拡大することができる。しかしな
がら、特にセラミックス複合材に於ける強力なマトリッ
クス／繊維結合は、実質的に全く繊維のプルアウト（ｐ
ｌｌｌｏｕｔ ） 、即ち繊維が引き出された状態では
なく概ね平坦な破壊表面となる脆性破壊が生じ、破壊靭
性が低下する。繊維のプルアウトは、破損クラックが進
む距離を増大させ、その表面積を増加させて複合材の靭
性を向上させる。<Prior Art> Glass, glass-ceramics, ceramics, metals, thermosetting materials, and thermoplastic materials can be reinforced with fibers to increase their strength and expand their range of applications. However, strong matrix/fiber bonds, especially in ceramic composites, result in virtually no fiber pull-out (p
llout ), that is, brittle fracture occurs in which the fibers are not pulled out but have a generally flat fracture surface, resulting in a decrease in fracture toughness. Fiber pull-out increases the distance that the failure crack travels, increasing its surface area and improving the toughness of the composite.
マトリックスを形成する前に繊維に例えば炭素等の皮膜
を形成することによって、マトリックス／繊維の結合及
び化学的相互作用を低減させることができ、破壊靭性が
向上する。カーボン皮膜（米国特許箱４．４２５，４０
７号及び第４，７３１、２９８号明細書を参照）は、容
易に酸化されかつ高い導電性を有し、或る条件下での使
用が制限されている。By forming a coating, such as carbon, on the fibers before forming the matrix, matrix/fiber bonding and chemical interactions can be reduced, improving fracture toughness. Carbon coating (U.S. Patent Box 4.425,40
7 and 4,731,298) are easily oxidized and have high conductivity, limiting their use under certain conditions.
高い電気抵抗と優れた熱衝撃抵抗と不燃性を有する窒化
硼素（ＢＮ）が同様に繊維の皮膜として使用されている
。（例えば米国特許箱４，６４２。Boron nitride (BN), which has high electrical resistance, excellent thermal shock resistance, and non-flammability, has also been used as a fiber coating. (For example, U.S. Patent Box 4,642.
２７１号明細書を参照。）窒化硼素は、そのグラファイ
トに類似の六角板構造によって、炭素に類似しているが
、炭素が有するいくつかの制限を有しておらず、有効な
代替物である。See specification No. 271. ) Boron nitride, although similar to carbon due to its graphite-like hexagonal plate structure, does not have some of the limitations that carbon has and is an effective substitute.
〈発明が解決しようとする課題〉
ＢＮ皮膜は、約り５０℃〜約２２００℃の範囲内の温度
でＣＶＤ （化学蒸着法）を用いて形成することができ
る。しかしながら、理論的ＢＮ皮膜は１７００℃以上の
析出温度に於でのみ達成されているが、この温度では通
常繊維に重大な劣化がもたらされる。このような温度に
繊維を加熱し、冷却し、かつ室温で試験した場合、その
元の強度を維持することができない。更に、従来技術を
用いて得られたＢＮ皮膜は一般に約０．３５ミクロン以
下で薄く、厚い皮膜は約７６０℃（１４００″Ｆ）以上
の温度に於でのみ達成される（米国特許箱４．４８１，
２５７号明細書を参照）。この結果、より改善された繊
維の被覆及び皮膜形成方法が引き続き要望されている。<Problems to be Solved by the Invention> The BN film can be formed using CVD (chemical vapor deposition) at a temperature within the range of about 50°C to about 2200°C. However, theoretical BN coatings have only been achieved at precipitation temperatures above 1700°C, which typically results in significant fiber degradation. When a fiber is heated to such a temperature, cooled and tested at room temperature, it is unable to maintain its original strength. Furthermore, BN coatings obtained using prior art techniques are generally thin, less than about 0.35 microns, and thick coatings are only achieved at temperatures above about 760° C. (1400"F) (see US Patent Box 4. 481,
257). As a result, there continues to be a need for improved fiber coating and coating methods.
［発明の構成］
〈課題を解決するための手段及び作用〉本発明は、繊維
とマトリックスの間の化学反応を減少させ、かつ破壊靭
性を向上させるべ（ＢＮで繊維を被覆することに関する
。繊維はＣＶＤ反応器内に配置されて加熱される。硼素
と窒素とを含む反応ガスが前記反応器内にキャリアガス
によって導入される。これらガスが反応してＢＮを生成
し、析出が生じ、厚いＢＮ皮膜（即ち約０．４０ミクロ
ン以上）が前記繊維の周囲に形成される。[Structure of the Invention] Means and Effects for Solving the Problems The present invention relates to coating fibers with BN to reduce chemical reactions between fibers and matrix and improve fracture toughness. is placed in a CVD reactor and heated. Reactant gases containing boron and nitrogen are introduced into said reactor by a carrier gas. These gases react to form BN, resulting in a thick deposit. A BN coating (ie, about 0.40 microns or greater) is formed around the fibers.
この厚さは、繊維とマトリックスとの間の化学反応を低
減させかつ所望の靭性を得るのに必要な厚さである。This thickness is that necessary to reduce chemical reactions between the fibers and matrix and to obtain the desired toughness.
上述した本発明の特徴及び他の特徴並びに利点について
は、以下に添付図面を参照しつつ詳細に説明する。The above-mentioned features and other features and advantages of the invention will be explained in detail below with reference to the accompanying drawings.
く実施例〉
セラミックマトリックス内に埋め込まれた非被覆繊維ま
たは薄い被覆繊維からなるセラミックス複合材にとって
、脆性破壊は重要な問題である。Examples: Brittle fracture is an important problem for ceramic composites consisting of uncoated fibers or thin coated fibers embedded within a ceramic matrix.
複合材の脆性によって、応力による破壊から生じるクラ
ックは複合材の中を概ね真直に走るように形成される。Due to the brittleness of the composite material, cracks resulting from stress failure form in a generally straight line through the composite material.
しかしながら、マトリックス内の繊維６＜ＢＮで十分に
被覆されている場合には、ＢＮ皮膜がクラックディフレ
クション及びブランティング即ちクラック先端の鈍化を
介して破壊靭性を増大させ、脆性破壊を防止する。ＢＮ
被覆繊維を有する複合材に応力を作用させると、円滑な
破壊面ではなく繊維のプルアウトが生じる。しかし、全
てのＢＮ皮膜が繊維のプルアウトを生じるのではない。However, if the fibers in the matrix are sufficiently coated with 6 < BN, the BN coating increases fracture toughness through crack deflection and blunting, or blunting of the crack tips, and prevents brittle fracture. B.N.
Applying stress to a composite with coated fibers results in fiber pull-out rather than a smooth fracture surface. However, not all BN coatings result in fiber pull-out.
ＢＮ皮膜の厚さが約０．３０ミクロン程度またはそれ以
下の場合には、非被覆繊維を含む複合材と同様に円滑な
破壊面が生じる。When the thickness of the BN coating is on the order of about 0.30 microns or less, a smooth fracture surface is produced similar to a composite material containing uncoated fibers.
第１図は、ガラスマトリックスに埋め込まれたネクステ
ル（Ｎｅｗｔｅｌ） （登録商標）繊維からなる被覆
繊維複合材と非被覆繊維複合材との曲げ強さの試験結果
を示している。本発明によるＢＮ被覆繊維を有する複合
材（１）は、非被覆繊維を有する複合材（５）と比較し
て非常に大きな曲げ強さを有する。第２Ａ図、第２Ｂ図
及び第２Ｃ図によって、それぞれ０．０８ミクロンの厚
さのＢＮ皮膜（第２Ａ図）についての破壊面及び０．１
６ミクロンの厚さを有するＢＮ皮膜（第２Ｂ図）（米国
特許第４．６４２，２７１号明細書に於て開示されてい
る。）の破壊面を比較する。前記両面は概ね円滑な破壊
面を示している。他方、第２Ｃ図は、０．１４ミクロン
の厚さのＢＮ皮膜を有する繊維について実質的に繊維の
プルアウトを示している。FIG. 1 shows the results of testing the flexural strength of coated and uncoated fiber composites consisting of Newtel® fibers embedded in a glass matrix. The composite material (1) with BN coated fibers according to the invention has a much higher bending strength compared to the composite material (5) with uncoated fibers. Figures 2A, 2B and 2C show the fracture surface and 0.1 micron thickness for a 0.08 micron thick BN film (Fig. 2A), respectively.
Compare the fracture surface of a BN coating (FIG. 2B) (disclosed in U.S. Pat. No. 4,642,271) having a thickness of 6 microns. Both surfaces exhibit generally smooth fracture surfaces. On the other hand, FIG. 2C shows substantial fiber pullout for a fiber with a 0.14 micron thick BN coating.
この方法には窒化シリコン、ムライト、アルミナを主成
分とする繊維等の様々な繊維を使用することができ、米
国ミネソタ州の３Ｍカンパニーにより製造されているネ
クステル（Ｎｅｗｔｅｌ） （登録商標）４８０及び
スミトモ（Ｓｕｍｉｔｏｍｏ） （登録商標）Ａ１２
０３が好都合である。ガラス、ガラス−セラミック、セ
ラミックス（ＣＶＩ炭化珪素及び窒化シリコンを含む）
、熱可塑性材料、熱硬化性材料及び金属のようなマトリ
ックスを用いて上述した繊維を被包することができる。A variety of fibers can be used in this method, including silicon nitride, mullite, and alumina-based fibers, including Newtel® 480 and Sumitomo fibers manufactured by 3M Company, Minnesota, USA. (Sumitomo) (registered trademark) A12
03 is convenient. Glass, glass-ceramic, ceramics (including CVI silicon carbide and silicon nitride)
Matrices such as thermoplastic materials, thermoset materials, and metals can be used to encapsulate the fibers described above.
更に、硼素と窒素とを含む様々な反応ガスを使用するこ
とができる。特に三塩化硼素（ＢＣｌ２）及びアンモニ
ア（ＮＨ３）が適していることが証明されている。これ
らの反応ガスはキャリアガスによって反応器に導入され
る。Additionally, various reactive gases can be used, including boron and nitrogen. In particular boron trichloride (BCl2) and ammonia (NH3) have proven suitable. These reaction gases are introduced into the reactor by a carrier gas.
一般にキャリアガスとして使用される水素（Ｈ２）は上
記工程に適していないことが判明した。It has been found that hydrogen (H2), commonly used as carrier gas, is not suitable for the above process.
Ｈ２は繊維の劣化及び弱体化を引き起こす。アルゴン（
Ａｒ ）のような不活性ガスは、通常一般的な基準ガス
Ｈ２よりも繊維を劣化させない。この結果として、特に
Ａｒの不活性ガスを本発明のキャリアガスとして使用し
た。H2 causes fiber degradation and weakening. Argon(
Inert gases such as Ar) usually degrade the fibers less than the common reference gas H2. As a result of this, an inert gas, in particular Ar, was used as a carrier gas in the present invention.
次の表は、Ｈ２またはＡｒをキャリアガスとして３分間
所定の温度に維持された被覆ネクステル（Ｎｅｘｔｅｌ
） ４８０繊維の試験結果を示している。The following table lists the coated Nextel samples maintained at a given temperature for 3 minutes with H2 or Ar as carrier gas.
) 480 fiber test results are shown.
（以下余白）
パージガス 温度”ＣＲＴ引張強さｋｇｆ’／ｃｍ２（
ｋｓｉ）Ｈ２１０５０１０８９８（１５５）
Ｈ２１０８０８５７８（１２２）
Ｈ２１１００計測不可
Ａｒ １０５０ ２６５７７ （３７８）Ａｒ
１０６０ １７６４８ （２５１）Ａｒ １１００
９０７０ （１２９）Ａｒ １１５０ ６８
９０ （９８）Ａｒ １２００ ５９０６
（８４）本発明を以下の実施例を用いてより詳細に説
明する。(Left below) Purge gas temperature "CRT tensile strength kgf'/cm2 (
ksi) H2105010898 (155) H210808578 (122) H21100 measurement impossible Ar 1050 26577 (378) Ar
1060 17648 (251) Ar 1100
9070 (129) Ar 1150 68
90 (98) Ar 1200 5906
(84) The present invention will be explained in more detail using the following examples.
実施例１
以下の方法を用いてネタステル４８０繊維」二にＢＮ皮
膜が形成される。Example 1 A BN coating is formed on Netaster 480 fibers using the following method.
（１）内部にネクステル繊維を配設した直径５゜０８ｃ
ｍ（２，０インチ）（壁の厚さ０．３２ｃｍ（１／８イ
ンチ））長さ１０．１６ｃｍ（４，０インチ）のグラフ
ァイト製サセプタを、直径７．６２ｃｍ（３，０インチ
）長さ４０． ６４ｃｍ （１６゜０ ｃｍ）のＣＶＤ
反応器内に装着する。（第３図参照）
（２）前記反応器の圧力を２００ミクロンにし、かつ温
度を１５００°Ｃまで加熱する。(1) Diameter 5°08c with Nextel fiber inside
m (2,0 in.) (wall thickness 0.32 cm (1/8 in.)) and 10.16 cm (4.0 in.) long graphite susceptor with a diameter of 7.62 cm (3.0 in.) long. Sa40. 64cm (16°0 cm) CVD
Install inside the reactor. (See Figure 3) (2) Bring the pressure of the reactor to 200 microns and heat the temperature to 1500°C.
（３）前記反応ガス及びキャリアガスを前記システムの
中に流通させる。即ち、ＢＣｌ３を流量６７ ｃｃ／分
で、ＮＨ３を６７ＣＣ／分で、Ａｒを約２０８ＣＣ／分
で３分間流通させる。約１．３０ミクロンの厚さのＢＮ
皮膜が形成される。(3) flowing the reactant gas and carrier gas through the system; That is, BCl3 is flowed at a flow rate of 67 cc/min, NH3 is flowed at a flow rate of 67 cc/min, and Ar is flowed at a flow rate of about 208 cc/min for 3 minutes. approximately 1.30 micron thick BN
A film is formed.
実施例２
実施例１に於けるネタステル４８０繊維をスミトモの繊
維に置き換えて実施例１と同じパラメータで実行すると
、厚さ約Ｏ，ＳＯミクロンの皮膜が得られる。Example 2 If the Netastel 480 fiber in Example 1 is replaced with Sumitomo fiber and the same parameters as in Example 1 are used, a film with a thickness of about O, SO microns is obtained.
上記実施例１及び２に於て得られた皮膜の厚さは、ＢＣ
ｌ３及びＮ Ｈ３の濃度を変更する（キャリアガスＡｒ
の量を減少させる）ことによって、または運転時間を増
加することによって増大させることができる。The thickness of the film obtained in Examples 1 and 2 above was BC
Change the concentration of l3 and N H3 (carrier gas Ar
) or by increasing the operating time.
以上本発明について実施例を用いて詳細に説明したが、
当業者にとって明らかなように本発明はその技術的範囲
内に於て様々な変形・変更を加えて実施することができ
る。The present invention has been explained in detail using examples above, but
As will be apparent to those skilled in the art, the present invention can be implemented with various modifications and changes within its technical scope.
第１図は、複合材内の被覆繊維と非被覆繊維の温度対曲
げ強さを示す線図である。
第２Ａ図乃至第２Ｃ図は、それぞれ異なるＢＮ皮膜厚さ
の破壊断面に於ける組織の形状を示す拡大写真である。
第３図は、ＢＮ皮膜の形成に使用されるＣＶＤ反応器ア
センブリを示す構成図である。
１．５・・・曲線FIG. 1 is a diagram showing the bending strength versus temperature of coated and uncoated fibers in a composite material. FIGS. 2A to 2C are enlarged photographs showing the shapes of structures in fracture cross sections of different BN film thicknesses. FIG. 3 is a block diagram showing a CVD reactor assembly used to form a BN film. 1.5...Curve
Claims (7)
リックス内に埋め込まれる繊維を包囲し、それによって
前記マトリックスと前記繊維との間の物理的結合及び化
学的相互作用の双方を妨げ、前記繊維／マトリックスシ
ステムに応力が作用すると繊維のプルアウト（ｐｕｌｌ
ｏｕｔ）が生じるように破壊靭性をクラックディフレク
ション及びブランティング（ｂｌｕｎｔｉｎｇ）を介し
て増大させたことを特徴とする窒化硼素皮膜。(1) having a thickness of at least 0.40 microns and surrounding the fibers embedded within the matrix, thereby preventing both physical bonding and chemical interaction between the matrix and the fibers; Fiber pull-out occurs when stress is applied to the fiber/matrix system.
1. A boron nitride film characterized in that fracture toughness is increased through crack deflection and blunting so as to cause crack deflection and blunting.
窒化硼素皮膜をセラミックマトリックス内に埋め込まれ
る繊維に形成する方法であって、ａ．硼素と窒素とを含
む反応ガスを使用する工程と、 ｂ．前記キャリアガスとして不活性ガスを使用する工程
と、 ｃ．約１０００℃と１３００℃との間の温度で前記皮膜
を形成する工程とからなり、かつ 前記温度が前記窒化硼素皮膜の所望の純度と予想される
繊維の劣化とのバランスによって決定されることを特徴
とする窒化硼素皮膜形成方法。(2) A method of forming a boron nitride coating produced from a reactive gas on fibers embedded within a ceramic matrix using a carrier gas, the method comprising: a. using a reactive gas comprising boron and nitrogen; b. using an inert gas as the carrier gas; c. forming the coating at a temperature between about 1000°C and 1300°C, and wherein the temperature is determined by a balance between the desired purity of the boron nitride coating and expected fiber degradation. Characteristic boron nitride film formation method.
用することを特徴とする第２請求項に記載の窒化硼素皮
膜形成方法。(3) The method for forming a boron nitride film according to claim 2, characterized in that argon is used as the inert gas carrier gas.
モニア（ＮＨ＿３）とを使用することを特徴とする第２
請求項に記載の窒化硼素皮膜形成方法。(4) A second method characterized in that boron trichloride (BCl_3) and ammonia (NH_3) are used as reaction gases.
A boron nitride film forming method according to the claims.
る繊維からなる群から選択された繊維であって、その表
面に少なくとも約０．４０ミクロンの厚さの窒化硼素（
ＢＮ）の皮膜が形成され、ガラス、ガラス−セラミック
、セラミックス（ＣＶＩ炭化珪素及び窒化珪素を含む）
、熱硬化性材料、熱可塑性材料及び金属からなる群から
選択されるマトリックスに複合されることを特徴とする
被覆繊維。(5) fibers selected from the group consisting of mullite, silicon nitride, and alumina-based fibers having at least about 0.40 micron thickness of boron nitride (
BN) films are formed on glass, glass-ceramics, and ceramics (including CVI silicon carbide and silicon nitride).
A coated fiber, characterized in that it is composited with a matrix selected from the group consisting of thermosetting materials, thermoplastic materials and metals.
らなり、破壊時に繊維のプルアウトを生じることを特徴
とする窒化硼素被覆繊維を有する複合材料。(6) A composite material having boron nitride-coated fibers, which is composed of arranged boron nitride-coated fibers and a matrix, and is characterized in that the fibers pull out when fractured.
約０．４０ミクロンであることを特徴とする第６請求項
に記載の複合材料。7. The composite material of claim 6, wherein the coating thickness of the boron nitride coated fiber is at least about 0.40 microns.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US37737789A | 1989-07-07 | 1989-07-07 | |
| US377,377 | 1989-07-07 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03115140A true JPH03115140A (en) | 1991-05-16 |
Family
ID=23488872
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2179400A Pending JPH03115140A (en) | 1989-07-07 | 1990-07-06 | Boron nitride film, method for forming boron nitride film, boron nitride-coated fiber and composite material having boron-nitride- coated fiber |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JPH03115140A (en) |
| DE (1) | DE4021243A1 (en) |
| FR (1) | FR2649393A1 (en) |
| GB (1) | GB2236540A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006096659A (en) * | 2004-09-28 | 2006-04-13 | General Electric Co <Ge> | Method for manufacturing high performance ceramic matrix composite material at low cost |
| CN105016631A (en) * | 2015-07-20 | 2015-11-04 | 湖北菲利华石英玻璃股份有限公司 | Boron nitride-coated quartz fiber preparation method |
| EP3527547A2 (en) | 2014-12-12 | 2019-08-21 | Kyoto University | Silicon carbide fiber reinforced silicon carbide composite material |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5198302A (en) * | 1990-04-23 | 1993-03-30 | Corning Incorporated | Coated inorganic fiber reinforcement materials and ceramic composites comprising the same |
| US5842342A (en) * | 1997-02-21 | 1998-12-01 | Northrop Grumman Corporation | Fiber reinforced ceramic matrix composite internal combustion engine intake/exhaust port liners |
| US6593255B1 (en) | 1998-03-03 | 2003-07-15 | Ppg Industries Ohio, Inc. | Impregnated glass fiber strands and products including the same |
| US8105690B2 (en) | 1998-03-03 | 2012-01-31 | Ppg Industries Ohio, Inc | Fiber product coated with particles to adjust the friction of the coating and the interfilament bonding |
| US6419981B1 (en) | 1998-03-03 | 2002-07-16 | Ppg Industries Ohio, Inc. | Impregnated glass fiber strands and products including the same |
| US6770176B2 (en) | 2002-08-02 | 2004-08-03 | Itn Energy Systems. Inc. | Apparatus and method for fracture absorption layer |
| US8062746B2 (en) | 2003-03-10 | 2011-11-22 | Ppg Industries, Inc. | Resin compatible yarn binder and uses thereof |
| US7867554B2 (en) | 2005-01-06 | 2011-01-11 | United Technologies Corporation | Boron nitride coated fibers and composite articles containing same |
| US8242375B2 (en) | 2008-09-18 | 2012-08-14 | United Technologies Corporation | Conductive emissions protection |
| US8524317B2 (en) * | 2010-09-30 | 2013-09-03 | United Technologies Corporation | Composite article and method therefor |
| CN107326648A (en) * | 2017-06-30 | 2017-11-07 | 长兴泓矿炉料有限公司 | A kind of bibulous mullite fiber fire smothering blanket |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1358140A (en) * | 1962-05-31 | 1964-04-10 | Gen Electric | High strength fused silica fibers |
| GB2014972B (en) * | 1977-12-29 | 1982-04-28 | Defence Secret Of State For | Boron nitride fibre |
| US4481257A (en) * | 1979-11-26 | 1984-11-06 | Avco Corporation | Boron coated silicon carbide filaments |
| ZA833150B (en) * | 1982-05-28 | 1984-01-25 | Int Standard Electric Corp | Coating an optical fibre |
| FR2567874B1 (en) * | 1984-07-20 | 1987-01-02 | Europ Propulsion | PROCESS FOR MANUFACTURING A COMPOSITE MATERIAL WITH REFRACTORY FIBROUS REINFORCEMENT AND CERAMIC MATRIX, AND STRUCTURE AS OBTAINED BY THIS PROCESS |
| US4642271A (en) * | 1985-02-11 | 1987-02-10 | The United States Of America As Represented By The Secretary Of The Navy | BN coating of ceramic fibers for ceramic fiber composites |
| JPS61223183A (en) * | 1985-03-04 | 1986-10-03 | Res Dev Corp Of Japan | Production of rhombohedral system boron nitride |
| JPS6212671A (en) * | 1985-07-10 | 1987-01-21 | 株式会社日立製作所 | Fiber reinforced ceramics |
| DE3568571D1 (en) * | 1985-11-18 | 1989-04-13 | Battelle Memorial Institute | Method and apparatus for the on-line coating of silica based fibers with boron-nitride |
-
1990
- 1990-07-03 GB GB9014729A patent/GB2236540A/en not_active Withdrawn
- 1990-07-04 DE DE4021243A patent/DE4021243A1/en not_active Withdrawn
- 1990-07-06 JP JP2179400A patent/JPH03115140A/en active Pending
- 1990-07-06 FR FR9008623A patent/FR2649393A1/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006096659A (en) * | 2004-09-28 | 2006-04-13 | General Electric Co <Ge> | Method for manufacturing high performance ceramic matrix composite material at low cost |
| EP3527547A2 (en) | 2014-12-12 | 2019-08-21 | Kyoto University | Silicon carbide fiber reinforced silicon carbide composite material |
| US11142483B2 (en) | 2014-12-12 | 2021-10-12 | Kyoto University | Silicon carbide fiber reinforced silicon carbide composite material |
| CN105016631A (en) * | 2015-07-20 | 2015-11-04 | 湖北菲利华石英玻璃股份有限公司 | Boron nitride-coated quartz fiber preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2649393A1 (en) | 1991-01-11 |
| DE4021243A1 (en) | 1991-01-17 |
| GB9014729D0 (en) | 1990-08-22 |
| GB2236540A (en) | 1991-04-10 |
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