JPS6253610B2 - - Google Patents
Info
- Publication number
- JPS6253610B2 JPS6253610B2 JP58236376A JP23637683A JPS6253610B2 JP S6253610 B2 JPS6253610 B2 JP S6253610B2 JP 58236376 A JP58236376 A JP 58236376A JP 23637683 A JP23637683 A JP 23637683A JP S6253610 B2 JPS6253610 B2 JP S6253610B2
- Authority
- JP
- Japan
- Prior art keywords
- fiber
- aluminosilicate ceramic
- carbon
- aluminosilicate
- fibers
- 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
Links
- 239000000835 fiber Substances 0.000 claims description 55
- 239000000919 ceramic Substances 0.000 claims description 32
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 30
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 239000012784 inorganic fiber Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- CVTZKFWZDBJAHE-UHFFFAOYSA-N [N].N Chemical compound [N].N CVTZKFWZDBJAHE-UHFFFAOYSA-N 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 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 description 5
- 238000000034 method Methods 0.000 description 5
- 229910052863 mullite Inorganic materials 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000012210 heat-resistant fiber Substances 0.000 description 4
- 239000002344 surface layer Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000005011 phenolic resin Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007833 carbon precursor Substances 0.000 description 2
- 229910000423 chromium oxide Inorganic materials 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 229910002796 Si–Al Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
Description
【発明の詳細な説明】
本発明は、高度の耐熱性を有する無機質繊維そ
の製造法に関するものである。
約800℃をこえる高温の雰囲気で連続使用可能
な耐熱性繊維としてはセラミツク繊維が代表的な
ものであり、近年はそのすぐれた耐熱性、耐熱衝
撃性、軽量性、電気絶縁性、化学的安定性、吸音
性などを生かして、製鉄その他各種の金属工業、
化学工業、機械工業等において断熱材、高温シー
ル材、パツキング、消音材、濾材などに広く利用
されるようになつた。しかしながら、上記セラミ
ツク繊維の用途分野における各種設備は近年ます
ます高性能化する傾向にあり、これにともない、
そこで使われる耐熱性繊維材料についてもより一
層耐熱性のすぐれたものが要望されるようになつ
た。たとえば最も普通に使われているアルミノシ
リケート質セラミツク繊維は、ほんらい非晶質の
ものが、1000℃付近から徐々に結晶化を起こし、
主にムライトと遊離シリカ（またはクリストバラ
イト）を生じて著しい体積減少と強度低下を起こ
すから、約1500℃をこえる温度での使用には通常
耐えられない。
多くの点で他のセラミツク繊維よりも有利なア
ルミノシリケート質セラミツク繊維を基にして、
より耐熱性のすぐれた繊維を製造しようとする試
みはすでに多数あり、その代表的な方法として
は、アルミノシリケート質セラミツク繊維の製造
原料中に酸化クロムを混入する方法や、アルミノ
シリケート質セラミツク繊維の表面に酸化クロ
ム、アルミナ、リン化合物等を付着させる方法な
どがある。しかしながら、これらの方法は上記ム
ライトの生成を根本的に抑制するものではないか
ら、耐熱性向上の効果はあまり顕著なものではな
い。
本発明者らは上述のような現状を背景に、より
高度の耐熱性を有するアルミノシリケート系セラ
ミツク繊維を求めて鋭意研究を重ねた結果、該繊
維を構成するアルミノシリケート質の一部を窒素
物に変換する化学的改質によつて目的を達成し得
ることを知り、本発明を完成するに至つた。
すなわち本発明は、アルミノシリケート質セラ
ミツク繊維の表面を炭素の薄層で被覆し、得られ
た炭素被覆アルミノシリケート質セラミツク繊維
を、窒素、アンモニア、窒素−アンモニア混合気
体またはこれらのいずれかと水素との混合気体中
で、該繊維を構成するアルミノシリケート質から
Si−Al−Ｏ−N4元素化合物が生成する温度に加
熱することにより、アルミノシリケート質セラミ
ツク繊維の少なくとも表層部をSi−Al−Ｏ−N4
元素化合物に変換することを特徴とする耐熱性無
機質繊維の製造法を提案するものである。
本発明による耐熱性繊維は、上記製法から明ら
かなようにアルミノシリケート質セラミツク繊維
が改質されたものであるが、改質度の進んだもの
は、もはやアルミノシリケート質セラミツク繊維
とはいえない新たな組成のセラミツク繊維であ
る。この繊維の表層部または全部を構成するSi−
Al−Ｏ−N4元素化合物は、その好ましい組成が
式Si6−ZAlZOZN8−Z（但し、ｚは1.0〜4.2の正
数）で表わされるものであつて、この化合物自体
は公知のものである（K.H.Jack，J.Mat.Sci.，
11，1135）。しかしながら、この化合物は従来非
繊維分野における焼結体製造原料としてのみ検討
されており、これからなる繊維がアルミノシリケ
ート質セラミツク繊維から誘導された例はなく、
また他の径路で作られた例もなかつた。
アルミノシリケート質セラミツク繊維と窒素と
の化学反応によつて形成された繊維状Si−Al−Ｏ
−N4元素化合物は熱的にきわめて安定であり、
また全体がSi−Al−Ｏ−N4元素化合物に変換さ
れていない場合でも残りの部分がやはり熱的に安
定なムライトに変換されているから、本発明によ
る繊維はアルミノシリケート質セラミツク繊維に
みられるような結晶化に伴う大きな収縮や強度低
下を起こさず、したがつてアルミノシリケート質
セラミツク繊維よりも苛酷な条件での使用に耐え
るものである。
次に本発明による上記耐熱性繊維の製造法につ
いて説明する。
出発原料として使用するアルミノシリケート質
セラミツク繊維は、周知の常法により製造された
ものをいずれも使用することができるが、なかで
もSi−Al−Ｏ−N4元素化合物への変換が円滑に
行われる点で好ましいのは、SiO235〜55重量
％、Al2O365〜45重量％、残部５重量％以下のも
のである。このような組成のアルミノシリケート
質セラミツク繊維の市販品の例としては、フアイ
ンフレツクス1300、同1500（いずれもニチアス株
式会社製品）、リフラシール（HITCO社製品）な
どがある。繊維径は１〜10μのものがよく、特に
好ましいのは３〜５μのものである。
原料繊維の表面を炭素の薄層で被覆する方法と
しては、微粒子状炭素（たとえばカーボンブラツ
ク、グラフアイトなど）の分散液または炭素前駆
体（加熱して炭化させると炭素微粉末を生成する
物質、たとえばフエノール樹脂、アクリル樹脂
等、炭素含有率の高い有機化合物）の溶液を原料
繊維に噴霧するか浸漬法により付着させて乾燥
し、炭素前駆体溶液を用いた場合は更に不活性雰
囲気中で有機物が炭化可能な温度に加熱する方法
があるが、これらに限定されるわけではない。繊
維表面は、繊維に対して５〜30重量％（特に好ま
しくは10〜20重量％）の炭素粒子で、なるべく均
一に被覆されることが望ましい。また炭素粒子は
繊維表面で直径が１μ以下（好ましくは0.5μ以
下）の微粒子状態を保つていることが望ましい。
アルミノシリケート質セラミツク繊維の表面を
炭素で被覆する上記処理は、アルミノシリケート
質セラミツク繊維製造の最終工程において実施し
てもよい。
次に、得られた炭素被覆アルミノシリケート質
セラミツク繊維を密閉可能な加熱炉に入れ、炉を
密閉して炉内を約１×10-4Torr以下（望ましく
は１×10-6Torr程度）の真空にした後、窒素、
アンモニア、窒素−アンモニア混合気体またはこ
れらのいずれかと水素との混合気体を導入してそ
の圧力を0.1〜200Kg／cm2、望ましくは１〜100
Kg／cm2に保ち、1600〜2000℃、望ましくは1700〜
1800℃に加熱する。この加熱処理により、加熱温
度にもよるが約60分までの処理では繊維の表層部
に厚さ0.1μ前後のSi−Al−Ｏ−N4元素化合物層
が形成され、更に処理を続けると、全体がSi−Al
−Ｏ−N4元素化合物に変換される（直径３〜５
μの繊維の場合）。原料繊維を被覆していた炭素
は、この熱処理においてSiO2およびAl2O3の還元
剤として作用し、窒化反応を促進する。
以上のように、本発明によれば、Si−Al−Ｏ−
N4元素化合物またはこれとムライトからなる高
度耐熱性無機質繊維をアルミノシリケート質セラ
ミツク繊維の改質により容易に製造することがで
きる。
以下実施例を示して本発明を説明する。
実施例 １
フエノール樹脂ワニス・PlyophenJ−325（大
日本インキ株式会社製品）をメタノールで２倍に
希釈し、これにアルミノシリケート質セラミツク
繊維・フアインフレツクス1300（ニチアス株式会
社製品；SiO248重量％、Al2O352重量％）を室温
で浸漬することにより上記希釈液を繊維に付着さ
せ、処理済繊維を50℃−60mmHgで減圧乾燥した
のち窒素雰囲気中800℃で３時間加熱して表面の
フエノール樹脂を炭化させることにより、繊維重
量に対して10％の炭素で被覆されたアルミノシリ
ケート質セラミツク繊維を調製した。次いでこの
繊維をグラフアイト製ルツボに入れて電気炉内に
置き、炉内を１×10-6Torrまで排気したのち窒
素ガスを導入し、窒素ガス圧を１Kg／cm2に保ちな
がら昇温速度30℃／minで1800℃まで昇温し、
1800℃で120分間加熱した。
得られた繊維は、その鉱物組成をＸ線回折とＸ
線マイクロアナライザーにより解析した結果、繊
維全体がSi−Ai−Ｏ−N4元素化合物からなるこ
とが確認された。
実施例 ２
炭素被覆アルミノシリケート質セラミツク繊維
の窒素中加熱処理の時間を30分に短縮したほかは
実施例１と同様にして、アルミノシリケート質セ
ラミツク繊維の改質を行なつた。得られた繊維
は、その鉱物組成をＸ線回折とＸ線マイクロアナ
ライザーにより解析した結果、厚さ約１μの表層
部がSi−Al−Ｏ−N4元素化合物からなり、芯部
がムライト結晶からなるものであることが確認さ
れた。
上記各例による製品および原料のアルミノシリ
ケート質セラミツク繊維について1500℃−３時間
の加熱試験を行い、加熱による収縮率および加熱
後の引張り強さを測定した。その結果を第１表に
示す。
【表】DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing an inorganic fiber having a high degree of heat resistance. Ceramic fiber is a typical heat-resistant fiber that can be used continuously in high-temperature environments exceeding approximately 800°C, and in recent years has received attention for its excellent heat resistance, thermal shock resistance, light weight, electrical insulation, and chemical stability. Taking advantage of its properties such as sound absorption and sound absorption, it is used in steel manufacturing and other various metal industries.
It has come to be widely used in the chemical industry, machinery industry, etc. for insulation materials, high-temperature sealing materials, packing materials, sound deadening materials, filter materials, etc. However, in recent years, the various types of equipment used in the above-mentioned fields of application of ceramic fibers have tended to become more and more sophisticated, and with this,
As for the heat-resistant fiber materials used therein, there has been a demand for materials with even better heat resistance. For example, the most commonly used aluminosilicate ceramic fibers are mostly amorphous, but gradually crystallize from around 1000℃.
It usually cannot withstand use at temperatures above about 1500°C, as it mainly forms mullite and free silica (or cristobalite), causing significant volume and strength loss. Based on aluminosilicate ceramic fibers, which have many advantages over other ceramic fibers,
There have already been many attempts to produce fibers with better heat resistance, and representative methods include mixing chromium oxide into the raw materials for producing aluminosilicate ceramic fibers, and There are methods such as attaching chromium oxide, alumina, phosphorus compounds, etc. to the surface. However, since these methods do not fundamentally suppress the formation of mullite, the effect of improving heat resistance is not so significant. Against the background of the above-mentioned current situation, the present inventors have conducted intensive research in search of aluminosilicate ceramic fibers with higher heat resistance. The present invention was completed based on the realization that the objective could be achieved through chemical modification to convert it into . That is, the present invention coats the surface of aluminosilicate ceramic fiber with a thin layer of carbon, and then injects the obtained carbon-coated aluminosilicate ceramic fiber with nitrogen, ammonia, a nitrogen-ammonia mixed gas, or any of these with hydrogen. In a mixed gas, the aluminosilicate that makes up the fiber
By heating to a temperature at which Si-Al-O-N4 elemental compounds are formed, at least the surface layer of the aluminosilicate ceramic fiber is converted into Si-Al-O-N4.
This paper proposes a method for producing heat-resistant inorganic fibers characterized by conversion into elemental compounds. As is clear from the above manufacturing method, the heat-resistant fiber according to the present invention is a modified aluminosilicate ceramic fiber, but the highly modified fiber is a new product that can no longer be called an aluminosilicate ceramic fiber. It is a ceramic fiber with a unique composition. Si- which constitutes the surface layer or all of this fiber
The preferred composition of the Al-O-N4 element compound is represented by the formula Si 6 - Z Al Z O Z N 8 - Z (where z is a positive number from 1.0 to 4.2), and the compound itself is It is a known one (KHJack, J.Mat.Sci.,
11, 1135). However, this compound has so far only been considered as a raw material for producing sintered bodies in the non-textile field, and there are no examples of fibers made from it being derived from aluminosilicate ceramic fibers.
There were also no examples of it being made using other routes. Fibrous Si-Al-O formed by chemical reaction between aluminosilicate ceramic fiber and nitrogen
−N4 element compounds are extremely thermally stable;
Furthermore, even if the entire portion is not converted to Si-Al-O-N4 elemental compound, the remaining portion is still converted to thermally stable mullite, so the fiber according to the present invention is found in aluminosilicate ceramic fiber. It does not undergo large shrinkage or strength reduction due to crystallization, and therefore can withstand use under harsher conditions than aluminosilicate ceramic fibers. Next, a method for producing the heat-resistant fiber according to the present invention will be explained. The aluminosilicate ceramic fiber used as a starting material can be any one manufactured by a well-known conventional method, but among them, the one that can be smoothly converted into a Si-Al-O-N4 elemental compound From this point of view, preferred is SiO 2 35-55% by weight, Al 2 O 3 65-45% by weight, and the remainder 5% by weight or less. Examples of commercially available aluminosilicate ceramic fibers with such compositions include Fineflex 1300 and Fineflex 1500 (both products of Nichias Corporation), and Refraseal (product of HITCO Corporation). The fiber diameter is preferably 1 to 10 microns, particularly preferably 3 to 5 microns. The surface of raw material fibers can be coated with a thin layer of carbon by using a dispersion of particulate carbon (e.g. carbon black, graphite, etc.) or a carbon precursor (a substance that produces fine carbon powder when heated and carbonized). For example, a solution of an organic compound with a high carbon content (such as phenolic resin or acrylic resin) is applied to the raw fiber by spraying or dipping, and then dried. If a carbon precursor solution is used, the organic compound is further removed in an inert atmosphere. There is a method of heating to a temperature at which it can be carbonized, but it is not limited to these methods. It is desirable that the fiber surface be coated as uniformly as possible with carbon particles in an amount of 5 to 30% by weight (particularly preferably 10 to 20% by weight) based on the fiber. Further, it is desirable that the carbon particles maintain a fine particle state with a diameter of 1 μm or less (preferably 0.5 μm or less) on the fiber surface. The above treatment of coating the surface of the aluminosilicate ceramic fiber with carbon may be carried out in the final step of producing the aluminosilicate ceramic fiber. Next, the obtained carbon-coated aluminosilicate ceramic fibers are placed in a sealable heating furnace, and the furnace is sealed to keep the inside of the furnace at a temperature of about 1×10 -4 Torr or less (preferably about 1×10 -6 Torr). After vacuuming, nitrogen,
Ammonia, a nitrogen-ammonia mixed gas, or a mixed gas of either of these and hydrogen is introduced and the pressure is adjusted to 0.1 to 200 Kg/cm 2 , preferably 1 to 100 Kg/cm 2 .
Kg/ cm2 , maintained at 1600~2000℃, preferably 1700~
Heat to 1800℃. Through this heat treatment, a Si-Al-O-N4 elemental compound layer with a thickness of around 0.1μ is formed on the surface layer of the fibers for up to about 60 minutes, depending on the heating temperature, and if the treatment is continued further, the entire is Si−Al
-O-N4 element compound (diameter 3-5
for μ fibers). The carbon that coated the raw material fiber acts as a reducing agent for SiO 2 and Al 2 O 3 during this heat treatment and promotes the nitriding reaction. As described above, according to the present invention, Si-Al-O-
Highly heat-resistant inorganic fibers made of N4 elemental compounds or N4 element compounds and mullite can be easily produced by modifying aluminosilicate ceramic fibers. The present invention will be explained below with reference to Examples. Example 1 Phenol resin varnish PlyophenJ-325 (product of Dainippon Ink Co., Ltd.) was diluted twice with methanol, and aluminosilicate ceramic fiber Fineflex 1300 (product of Nichias Co., Ltd.; SiO 2 48% by weight) was diluted twice with methanol. , Al 2 O 3 (52% by weight)) at room temperature to adhere the diluted solution to the fibers, and the treated fibers were dried under reduced pressure at 50℃-60mmHg, and then heated at 800℃ for 3 hours in a nitrogen atmosphere to coat the surface. Aluminosilicate ceramic fibers coated with 10% carbon based on the fiber weight were prepared by carbonizing phenolic resin. Next, this fiber was placed in a crucible made of graphite and placed in an electric furnace, and the furnace was evacuated to 1 × 10 -6 Torr, nitrogen gas was introduced, and the temperature was increased at a rate of increase while maintaining the nitrogen gas pressure at 1 kg/cm 2 . Raise the temperature to 1800℃ at 30℃/min,
Heated at 1800°C for 120 minutes. The mineral composition of the obtained fibers was determined by X-ray diffraction and
As a result of analysis using a line microanalyzer, it was confirmed that the entire fiber was composed of a Si-Ai-O-N4 elemental compound. Example 2 Aluminosilicate ceramic fibers were modified in the same manner as in Example 1, except that the time for heat treatment of the carbon-coated aluminosilicate ceramic fibers in nitrogen was shortened to 30 minutes. The mineral composition of the obtained fibers was analyzed using X-ray diffraction and an X-ray microanalyzer, and it was found that the surface layer, approximately 1μ thick, was composed of a Si-Al-O-N4 elemental compound, and the core was composed of mullite crystals. It was confirmed that it was. A heating test was conducted at 1500 DEG C. for 3 hours on the products and raw material aluminosilicate ceramic fibers according to each of the above examples, and the shrinkage rate due to heating and the tensile strength after heating were measured. The results are shown in Table 1. 【table】
Claims (1)
を炭素の薄層で被覆し、得られた炭素被覆アルミ
ノシリケート質セラミツク繊維を、窒素、アンモ
ニア、窒素−アンモニア混合気体またはこれらの
いずれかと水素との混合気体中で、該繊維を構成
するアルミノシリケート質からSi−Al−Ｏ−N4
元素化合物が生成する温度に加熱することを特徴
とする耐熱性無機質繊維の製造法。 ２ アルミノシリケート質セラミツク繊維が
SiO235〜55重量％、Al2O365〜45重量％、残部５
重量％以下のものである特許請求の範囲第１項記
載の製造法。 ３ 炭素被覆アルミノシリケート質セラミツク繊
維の加熱温度が1600〜2000℃である特許請求の範
囲１項または第２項記載の製造法。[Claims] 1. The surface of an aluminosilicate ceramic fiber is coated with a thin layer of carbon, and the obtained carbon-coated aluminosilicate ceramic fiber is heated with nitrogen, ammonia, a nitrogen-ammonia mixed gas, or any of these gases and hydrogen. Si-Al-O-N4 from the aluminosilicate material constituting the fiber in a gas mixture with
A method for producing heat-resistant inorganic fibers, which comprises heating to a temperature at which elemental compounds are generated. 2 Aluminosilicate ceramic fiber
SiO 2 35-55% by weight, Al 2 O 3 65-45% by weight, balance 5
% or less by weight. 3. The manufacturing method according to claim 1 or 2, wherein the carbon-coated aluminosilicate ceramic fiber is heated at a temperature of 1,600 to 2,000°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23637683A JPS60134025A (en) | 1983-12-16 | 1983-12-16 | Heat-resistant inorganic fiber and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23637683A JPS60134025A (en) | 1983-12-16 | 1983-12-16 | Heat-resistant inorganic fiber and its production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60134025A JPS60134025A (en) | 1985-07-17 |
| JPS6253610B2 true JPS6253610B2 (en) | 1987-11-11 |
Family
ID=16999871
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23637683A Granted JPS60134025A (en) | 1983-12-16 | 1983-12-16 | Heat-resistant inorganic fiber and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60134025A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4875823A (en) * | 1971-12-22 | 1973-10-12 |
-
1983
- 1983-12-16 JP JP23637683A patent/JPS60134025A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4875823A (en) * | 1971-12-22 | 1973-10-12 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60134025A (en) | 1985-07-17 |
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