JP3812981B2 - Ceramic fiber for processing material, manufacturing method thereof and processing material - Google Patents
Ceramic fiber for processing material, manufacturing method thereof and processing material Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は金属或いは非金属を切断、穿孔、研磨等の加工をするために用いるのに好適な加工材並びにこの加工材の加工要素として用いられるアルミナ系セラミック繊維とその製造方法に関する。
【０００２】
【従来の技術】
従来、この種の加工材として、例えば、特開平１ー２２２８６５号公報に開示されるように、アルミナ繊維を一方向に引き揃えて、これをエポキシ樹脂等の熱硬化性樹脂で結着してなるラッピング材が知られている。また、特開平２ー２３２１７４号公報に開示されるように、アルミナ繊維を一方向に引き揃えて、これをエポキシ樹脂等の熱硬化性樹脂で結着してなる切削、研磨用回転工具が知られている。
【０００３】
【発明が解決しようとする課題】
しかしながら、上記従来の加工材に使用されているアルミナ繊維は繊維強度が大きく且つ柔軟性にも優れているものの、例えば研磨材として使用した場合には、研磨性が必ずしも満足できるものでなく、更なる加工性の向上が望まれていた。
そこで、本発明は、通常のアルミナ繊維よりも更に繊維強度の大きな加工性に優れたセラミック繊維並びにこのセラミック繊維を含む加工材を提供することを目的とする。
また、本発明は、このような加工性に優れたセラミック繊維の製造方法を提供することも目的とする。
【０００４】
【課題を解決するための手段】
本発明の加工材用セラミック繊維は、加工材の加工要素として用いられるセラミック繊維であって、アルミナ繊維の前駆体繊維を焼成してセラミック繊維とし、前記前駆体繊維を１２００℃以下で焼成してセラミックス化した後、１３００℃以上の高温で３０秒間以内加熱処理し、アルミナ成分８０〜９０重量％とシリカ成分２０〜１０重量％とによって形成され、該セラミック繊維の結晶構造が主としてムライト結晶と中間アルミナとで構成され、該ムライト結晶の平均粒径が２５〜７０ナノメータとしたことを特徴とする。
また、請求項２記載の加工材用セラミック繊維は、前記アルミナ成分が８５重量％以上であることを特徴とする。
また、請求項３記載の加工材用セラミック繊維は、前記前駆体繊維は塩基性塩化アルミニウムとコロイダルシリカとポリビニルアルコールからなる水性の紡糸原液を乾式紡糸して得られたものであることを特徴とする。
また、請求項４記載の加工材は、請求項１又は２に記載のセラミック繊維を含むことを特徴とする。
また、請求項５記載の加工材は、前記セラミック繊維を樹脂バインダで結着してなることを特徴とする。
また、請求項６記載の加工材は、前記セラミック繊維を結着する樹脂バインダがエポキシ樹脂であることを特徴とする。
【０００５】
【発明の実施の形態】
本発明の加工材用セラミック繊維は平均粒径が２５〜７０ナノメータであるムライト結晶で構成され、本発明の加工材は前記平均粒径が２５〜７０ナノメータであるムライト結晶で構成されるセラミック繊維を含む。
前記ムライト結晶は、通常の中間アルミナ質の製品に比べて硬度が高く、また、平均結晶粒径が約１０倍程度大きいために良好な加工性を示す。
【０００６】
一般に、アルミナ繊維と呼ばれるものは７０〜８５重量％のＡｌ2Ｏ3と１５〜３０重量％のＳｉＯ2 を主成分とする多結晶質の繊維であって、繊維径は５〜４０μｍ程度である。その結晶状態は主として中間アルミナで、平均結晶径はせいぜい５ナノメーター程度の極めて微細な結晶粒子からなる焼結体である。このため、適度な柔軟性と高い機械的強度を示し、各種の繊維強化材料（ＦＲＰ，ＦＲＭ）への利用が期待されている。
このようなアルミナ繊維は１４００℃以上の高温で長い時間加熱されると中間アルミナの他にムライトやコランダムといった粗大な結晶が生成し、その結果、収縮や脆化が進み繊維としての機能が著しく低下する。
【０００７】
本発明の加工性のよいセラミック繊維は、従来のアルミナ繊維に比べて結晶の成長を進めてある点が特徴である。しかし、上記の説明のように過度の熱処理は繊維の強度特性を著しく低下させる。本発明のセラミック繊維はこの点を考慮し、１３００℃以上の高い温度で短時間、具体的には３０秒以内の熱処理をすることでムライトとしては微細な粒径の結晶を生成させることにより繊維の脆化を抑制しながら硬度を高め、加工性のよいセラミック繊維を製造することに特徴がある。
【０００８】
本発明の製造方法によって加工性のよいセラミック繊維を得ることができるが、この場合ムライト結晶の粒径を２５ナノメーター以上にすると、特に加工性に優れたセラミック繊維が得られる。しかし、１００ナノメーター以上に成長させてしまうと脆化が著しく進行するので好ましくない。従って、ムライト結晶の粒径は２５〜７０ナノメーターの範囲にする必要がある。
【０００９】
また、本発明のセラミック繊維の成分組成は、高い高度を得るために、アルミナ成分が少なくとも８０重量％以上含まれることが必要で、８５重量％以上含まれることが特に好ましい。尚、その他の残部は主としてシリカ成分である。
【００１０】
本発明の加工材用セラミック繊維の製造方法は、アルミナ繊維の前駆体繊維を焼成してセラミック繊維とするときの焼成温度と、その後の加熱処理に特徴があるものであって、前駆体繊維を製造するための出発原料等については従来のアルミナ繊維の製造方法と特に異なるものではない。
具体的には、塩基性塩化アルミニウムとコロイダルシリカとポリビニルアルコールから成る水性の紡糸原液を乾式紡糸して前駆体繊維を得、この前記前駆体繊維を１２００℃以下で焼成してセラミックス化した後、１３００℃以上の高温で３０秒間以内加熱処理すればよい。
【００１１】
加工要素として前記セラミック繊維を含む加工材は、これら繊維を適当に引き揃え、エポキシ樹脂、フェノール樹脂等の熱硬化性樹脂に含浸して硬化することにより簡単に製造することができる。
【００１２】
【実施例】
以下本発明の実施例を比較例と共に説明する。
先ず、アルミニウムイオン１３．２重量％、塩素イオン１１．４５重量％含有する塩基性塩化アルミニウムの水溶液を３４ｋｇ、二酸化ケイ素を２０重量％含有するコロイダルシリカ７．５ｋｇに、平均重合度１７００の部分ケン化ポリビニルアルコール２．５ｋｇを溶解して粘度が約１０００ポイズ／２０℃の紡糸原液を調製した。
【００１３】
これを１０００ホールの紡糸ノズルから押し出して乾式紡糸し、さらに１２００℃まで焼成してセラミック繊維束を得た。更に、このセラミック繊維束を１４００℃のパイプ炉に通して連続的に巻き取った。この時、１４００℃での加熱時間が２秒および５秒となるように繊維束の通過速度を調整して実施例１，２として２種類の繊維束を得た。
尚、比較例１として１２００℃で焼成しただけで１４００℃での加熱処理を行わない繊維束を得た。
【００１４】
得られた繊維束の繊維径、Ｘ線回折による結晶構造、２θが約２６°付近に現れるムライトの（２１０）面の回折線の半減値巾（β1/2 ）から下記の一般式によって求めた平均粒径（Ｄhkl）を表１に示した。
Ｄhkl＝０．９λ／β1/2・ＣＯＳθ
（但し、Ｄhkl：（２１０）面の平均粒径，λ：Ｘ線の波長，θ：Ｘ線の視斜角）
【００１５】
次に、上記各繊維束とエポキシ樹脂による一方向強化材（以下「ＵＤーＦＲＰ」と略記する）を作成し、金属に対する研磨性を調べた。
ＵＤーＦＲＰの作成は次のようにして行った。
先ず、定法に従って、繊維束をドラムに平行巻きし、下記の組成の樹脂を塗布し、余剰の樹脂を絞り取り、ドラムから切り開いて繊維が一方向配列した樹脂含浸シートを得た。これを温風乾燥機内で９５℃、１時間乾燥した後、ポリエステルフィルムで上下から挟み込み、約６０℃に加熱したローラープレスにかけてＵＤプリプレグシートを得た。
エポキシ樹脂（エピコート８２８ 油化シェルエポキシ社製） ６０重量部
エポキシ樹脂（エピコート１００１ 油化シェルエポキシ社製） ４０重量部
三弗化ホウ素モノエチルアミン ２．５重量部
ＭＥＫ ３５重量部
このＵＤプリプレグシートを積み重ね、２０Ｋｇ／ｃｍ2 の圧力下で１７０℃、１時間加熱して硬化させ、厚さ３．７ｍｍのＵＤーＦＲＰを得た。
【００１６】
次に、これらＵＤーＦＲＰの研削性を試験し、表１にその結果を示した。
各試験片はＬ×Ｗ×Ｔ＝２０ｍｍ×５ｍｍ×３．７ｍｍの立方体とし、ＵＤーＦＲＰから切り出すに当たり、辺Ｌ（２０ｍｍ）が繊維の配列方向と６０℃の角度をなすようにした。図１は試験片（加工材）の斜視図を示すもので、図中１はセラミック繊維を示す。
尚、研削性の試験方法については、次のようにした。
被研削材として、Ｌ×Ｗ×Ｔ＝８０ｍｍ×１５ｍｍ×２ｍｍの鉄板を用意し、これをしかりと固定して、この鉄板のＬＷ面を被研削面とし、ＵＤ−ＦＲＰの各試験片のＬＴ面を乗せ、上から一定の荷重（１３７５ｇ）をかけながら試験片を往復運動させた。この時、運動巾は４５ｍｍ、運動速度は１２５往復／分、総往復運動回数は１００００回とした。
この時、初めの被研削材の重さをＡ、研削後の被研削材の重さをＢとして、次の式から研削率を求めた。
研削率（重量％）＝（ＡーＢ／Ａ）×１００
【００１７】
【表１】
次に実施例１と比較例１のＵＤ−ＦＲＰから得られた前記試験片を、鉄製の金型磨きを専門とする５社に持ち込み、研磨性の評価をしたところ、表２に示すような結果が得られた。
【００１９】
【表２】
表２から明らかなように、粒径が２５〜７０ナノメータと大きなムライト結晶を含むセラミック繊維が非常に研磨性に優れていることが確認できた。
【００２１】
【発明の効果】
以上のように本発明によれば、通常のアルミナ繊維よりもさらに繊維強度の高い加工性に優れたセラミック繊維並びにこのセラミック繊維を含む加工材を得ることができるとともに、このような加工性の優れたセラミック繊維を製造することができる。
【図面の簡単な説明】
【図１】本発明の加工材の一実施例の斜視図
【符号の説明】
１ セラミック繊維[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a processing material suitable for use in processing such as cutting, drilling and polishing of metal or nonmetal, an alumina-based ceramic fiber used as a processing element of the processing material, and a method for producing the same.
[0002]
[Prior art]
Conventionally, as this type of processed material, for example, as disclosed in JP-A-1-222865, alumina fibers are aligned in one direction and bonded with a thermosetting resin such as an epoxy resin. A wrapping material is known. Further, as disclosed in JP-A-2-232174, there is known a rotary tool for cutting and polishing in which alumina fibers are aligned in one direction and bonded with a thermosetting resin such as an epoxy resin. It has been.
[0003]
[Problems to be solved by the invention]
However, although the alumina fiber used in the above-described conventional processed material has high fiber strength and excellent flexibility, for example, when used as an abrasive, the abrasiveness is not always satisfactory, and further, Improvement of processability has been desired.
Accordingly, an object of the present invention is to provide a ceramic fiber having a higher fiber strength and excellent workability than a normal alumina fiber, and a processed material containing the ceramic fiber.
Another object of the present invention is to provide a method for producing such a ceramic fiber excellent in workability.
[0004]
[Means for Solving the Problems]
The ceramic fiber for a processing material of the present invention is a ceramic fiber used as a processing element of a processing material, and a precursor fiber of alumina fiber is fired to form a ceramic fiber, and the precursor fiber is fired at 1200 ° C. or less. After being ceramicized , it is heat-treated at a high temperature of 1300 ° C. or higher for 30 seconds and formed by 80 to 90% by weight of the alumina component and 20 to 10% by weight of the silica component. is composed of alumina, average particle size of the mullite crystals is characterized in that a 25 to 70 nanometers.
Moreover, the ceramic fiber for processed materials according to claim 2 is characterized in that the alumina component is 85% by weight or more.
The ceramic fiber for processing material according to claim 3 , wherein the precursor fiber is obtained by dry-spinning an aqueous spinning stock solution composed of basic aluminum chloride, colloidal silica, and polyvinyl alcohol. To do.
A processed material according to a fourth aspect includes the ceramic fiber according to the first or second aspect.
The processed material according to claim 5 is characterized in that the ceramic fibers are bound by a resin binder.
The processed material according to claim 6 is characterized in that the resin binder for binding the ceramic fibers is an epoxy resin.
[0005]
DETAILED DESCRIPTION OF THE INVENTION
The ceramic fiber for processing material of the present invention is composed of mullite crystal having an average particle diameter of 25 to 70 nanometers, and the processing material of the present invention is ceramic fiber composed of mullite crystal having an average particle diameter of 25 to 70 nanometers. including.
The mullite crystal has a higher hardness than a normal intermediate alumina product, and exhibits an excellent workability because the average crystal grain size is about 10 times larger.
[0006]
In general, what is called alumina fiber is a polycrystalline fiber mainly composed of 70 to 85% by weight of Al 2 O 3 and 15 to 30% by weight of SiO 2 , and the fiber diameter is about 5 to 40 μm. . The sintered body is mainly composed of intermediate alumina and is composed of extremely fine crystal particles having an average crystal diameter of about 5 nanometers at most. For this reason, moderate softness | flexibility and high mechanical strength are shown, and the utilization to various fiber reinforced materials (FRP, FRM) is anticipated.
When such an alumina fiber is heated at a high temperature of 1400 ° C. or higher for a long time, coarse crystals such as mullite and corundum are formed in addition to intermediate alumina, and as a result, shrinkage and embrittlement progress and the function as a fiber is significantly reduced. To do.
[0007]
The ceramic fiber with good processability of the present invention is characterized in that crystal growth is advanced as compared with the conventional alumina fiber. However, as described above, excessive heat treatment significantly reduces the strength properties of the fiber. In consideration of this point, the ceramic fiber of the present invention is produced by generating crystals with a fine grain size as mullite by performing heat treatment at a high temperature of 1300 ° C. or higher for a short time, specifically within 30 seconds. It is characterized by increasing the hardness while suppressing the embrittlement of the ceramic and producing ceramic fibers with good workability.
[0008]
Ceramic fibers with good processability can be obtained by the production method of the present invention. In this case, when the particle size of mullite crystals is 25 nanometers or more, ceramic fibers having particularly excellent processability can be obtained. However, if it grows to 100 nanometers or more, embrittlement will remarkably progress, which is not preferable. Therefore, the particle size of the mullite crystal needs to be in the range of 25 to 70 nanometers.
[0009]
In addition, in order to obtain a high altitude, the component composition of the ceramic fiber of the present invention needs to contain at least 80% by weight of the alumina component, and particularly preferably 85% by weight or more. The remaining balance is mainly a silica component.
[0010]
The method for producing a ceramic fiber for a processing material according to the present invention is characterized by a firing temperature when a precursor fiber of alumina fiber is fired to form a ceramic fiber, and a subsequent heat treatment. The starting material for production is not particularly different from the conventional method for producing alumina fibers.
Specifically, a precursor fiber is obtained by dry spinning an aqueous spinning stock solution composed of basic aluminum chloride, colloidal silica, and polyvinyl alcohol, and the precursor fiber is fired at 1200 ° C. or less to be converted into ceramics. What is necessary is just to heat-process within 30 second at the high temperature of 1300 degreeC or more.
[0011]
A processed material containing the ceramic fiber as a processing element can be easily manufactured by properly aligning these fibers and impregnating them with a thermosetting resin such as an epoxy resin or a phenol resin and curing.
[0012]
【Example】
Examples of the present invention will be described below together with comparative examples.
First, 34 kg of an aqueous solution of basic aluminum chloride containing 13.2% by weight of aluminum ions and 11.45% by weight of chlorine ions and 7.5 kg of colloidal silica containing 20% by weight of silicon dioxide were mixed with a partial sapon having an average degree of polymerization of 1700. 2.5 kg of polyvinyl alcohol was dissolved to prepare a spinning dope having a viscosity of about 1000 poise / 20 ° C.
[0013]
This was extruded from a spinning nozzle with 1000 holes, dry-spun, and fired to 1200 ° C. to obtain a ceramic fiber bundle. Further, the ceramic fiber bundle was continuously wound through a pipe furnace at 1400 ° C. At this time, the passing speed of the fiber bundle was adjusted so that the heating time at 1400 ° C. was 2 seconds and 5 seconds, and two types of fiber bundles were obtained as Examples 1 and 2.
As Comparative Example 1, a fiber bundle was obtained which was baked at 1200 ° C. and was not subjected to heat treatment at 1400 ° C.
[0014]
Obtained by the following general formula from the fiber diameter of the obtained fiber bundle, the crystal structure by X-ray diffraction, and the half-value width (β 1/2 ) of the diffraction line on the (210) plane of mullite where 2θ appears around 26 °. The average particle diameter (D hkl ) is shown in Table 1.
D hkl = 0.9λ / β 1/2・ COSθ
(However, D hkl : Average particle diameter of (210) plane, λ: X-ray wavelength, θ: Oblique angle of X-ray)
[0015]
Next, a unidirectional reinforcing material (hereinafter abbreviated as “UD-FRP”) made of each of the above fiber bundles and an epoxy resin was prepared, and the abrasiveness to metal was examined.
Creation of UD-FRP was performed as follows.
First, according to a conventional method, a fiber bundle was wound in parallel on a drum, a resin having the following composition was applied, excess resin was squeezed out, cut out from the drum, and a resin-impregnated sheet in which fibers were aligned in one direction was obtained. After drying this at 95 ° C. for 1 hour in a hot air dryer, it was sandwiched from above and below with a polyester film and applied to a roller press heated to about 60 ° C. to obtain a UD prepreg sheet.
Epoxy resin (Epicoat 828 made by Yuka Shell Epoxy) 60 parts by weight Epoxy resin (Epicoat 1001 made by Yuka Shell Epoxy) 40 parts by weight Boron trifluoride monoethylamine 2.5 parts by weight MEK 35 parts by weight This UD prepreg sheet Stacking and curing by heating at 170 ° C. for 1 hour under a pressure of 20 kg / cm 2, a 3.7 mm thick UD-FRP was obtained.
[0016]
Next, the grindability of these UD-FRPs was tested, and Table 1 shows the results.
Each test piece was a cube of L × W × T = 20 mm × 5 mm × 3.7 mm, and when cut out from the UD-FRP, the side L (20 mm) formed an angle of 60 ° C. with the fiber arrangement direction. FIG. 1 shows a perspective view of a test piece (processed material), in which 1 denotes a ceramic fiber.
The grindability test method was as follows.
As a material to be ground, an iron plate of L × W × T = 80 mm × 15 mm × 2 mm is prepared, and this is firmly fixed, and the LW surface of this iron plate is used as a surface to be ground, and LT of each test piece of UD-FRP The test piece was reciprocated while placing a surface and applying a constant load (1375 g) from above. At this time, the movement width was 45 mm, the movement speed was 125 reciprocations / minute, and the total number of reciprocations was 10,000.
At this time, the weight of the first material to be ground was A, and the weight of the material to be ground after grinding was B, and the grinding rate was obtained from the following equation.
Grinding rate (% by weight) = (A−B / A) × 100
[0017]
[Table 1]
Next, the test pieces obtained from the UD-FRP of Example 1 and Comparative Example 1 were brought into five companies specializing in iron mold polishing and evaluated for abrasiveness, as shown in Table 2. Results were obtained.
[0019]
[Table 2]
As is apparent from Table 2, it was confirmed that the ceramic fiber containing a large mullite crystal having a particle size of 25 to 70 nanometers was very excellent in abrasiveness.
[0021]
【The invention's effect】
As described above, according to the present invention, it is possible to obtain a ceramic fiber having higher fiber strength than ordinary alumina fibers and excellent workability, and a processed material containing the ceramic fiber, and such excellent workability. Ceramic fibers can be produced.
[Brief description of the drawings]
FIG. 1 is a perspective view of an embodiment of a processed material according to the present invention.
1 Ceramic fiber
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35526296A JP3812981B2 (en) | 1996-12-20 | 1996-12-20 | Ceramic fiber for processing material, manufacturing method thereof and processing material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35526296A JP3812981B2 (en) | 1996-12-20 | 1996-12-20 | Ceramic fiber for processing material, manufacturing method thereof and processing material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10183427A JPH10183427A (en) | 1998-07-14 |
| JP3812981B2 true JP3812981B2 (en) | 2006-08-23 |
Family
ID=18442914
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35526296A Expired - Lifetime JP3812981B2 (en) | 1996-12-20 | 1996-12-20 | Ceramic fiber for processing material, manufacturing method thereof and processing material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3812981B2 (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002206421A (en) * | 2001-01-11 | 2002-07-26 | Ibiden Co Ltd | Holding-seal material for catalytic converter, ceramic fiber, and method of manufacturing the ceramic fiber |
| JP2011231774A (en) * | 2011-07-26 | 2011-11-17 | Ibiden Co Ltd | Method of manufacturing holding seal material for catalytic converter |
| CN105051272A (en) * | 2013-01-23 | 2015-11-11 | 电气化学工业株式会社 | Alumina fiber and alumina fiber aggregate |
| WO2023042385A1 (en) | 2021-09-17 | 2023-03-23 | 大明化学工業株式会社 | Linear abrasive member for polishing brush, and polishing brush |
| CN117980435A (en) * | 2021-09-17 | 2024-05-03 | 大明化学工业株式会社 | Linear abrasive for polishing brush and polishing brush |
| JP7239951B1 (en) * | 2022-08-02 | 2023-03-15 | 大明化学工業株式会社 | Stick grindstone and polishing method |
-
1996
- 1996-12-20 JP JP35526296A patent/JP3812981B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH10183427A (en) | 1998-07-14 |
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