JP3438028B2 - Nb3Si5Al2-Al2O3 two-layer coated Nb-based alloy and method for producing the same - Google Patents
Nb3Si5Al2-Al2O3 two-layer coated Nb-based alloy and method for producing the sameInfo
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- JP3438028B2 JP3438028B2 JP2000362089A JP2000362089A JP3438028B2 JP 3438028 B2 JP3438028 B2 JP 3438028B2 JP 2000362089 A JP2000362089 A JP 2000362089A JP 2000362089 A JP2000362089 A JP 2000362089A JP 3438028 B2 JP3438028 B2 JP 3438028B2
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- based alloy
- nb3si5al2
- sintering
- coated
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Description
【０００１】[0001]
【発明の属する技術分野】本発明は、超高温用構造材料
の候補として注目されながら高温における耐酸化性に劣
るNb基合金表面を耐酸化性のある材料でコーティングす
る技術であり、コーティングされた材料は例えば航空機
用エンジンの燃焼器、タービン等の超高温に耐える構造
材料として使用される。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is a technique for coating the surface of an Nb-based alloy, which is inferior in oxidation resistance at high temperature with a material having oxidation resistance, which is attracting attention as a candidate for a structural material for ultra-high temperature. The material is used, for example, as a structural material that withstands extremely high temperatures, such as combustors and turbines for aircraft engines.
【０００２】[0002]
【従来の技術】近年、航空機用エンジンの高出力化等を
目的として、従来使用されてきたNi基超合金より高温で
使用できる材料の開発が急務になっている。Nb基合金は
融点がNi基超合金より約1000℃高く、比重もNi基超合金
と同程度であることから、超高温用構造材料としての応
用が期待されている。2. Description of the Related Art In recent years, there has been an urgent need to develop materials that can be used at higher temperatures than the conventionally used Ni-base superalloys for the purpose of increasing the output of aircraft engines. Since the melting point of Nb-based alloys is about 1000 ° C higher than that of Ni-based superalloys and the specific gravity is about the same as that of Ni-based superalloys, it is expected to be applied as a structural material for ultrahigh temperature.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、現在ま
でに開発されてきているNb基合金は全て高温における耐
酸化性が非常に悪く、実用化への大きな障害となってい
る。本発明は、焼結法とくに放電プラズマ焼結法を用い
て、Nb基合金表面上を高温において耐酸化性に優れるNb
3Si5Al2金属間化合物で被覆し、同時にNb基合金とNb3Si
5Al2層間に両者の密着性を向上しかつ拡散防止層となる
Al2O3層を中間層として挟むことにより高温において安
定でかつ耐酸化性の優れるNb基合金を作製する技術を提
供することを目的とするものである。However, all of the Nb-based alloys that have been developed so far have very poor oxidation resistance at high temperatures, which is a major obstacle to their practical use. The present invention uses a sintering method, in particular, a discharge plasma sintering method, to form Nb-based alloys having excellent oxidation resistance at high temperatures on the surface of an Nb-based alloy.
3Si5Al2 intermetallic compound coating, Nb-based alloy and Nb3Si
5Al2 improves adhesion between layers and becomes a diffusion prevention layer
It is an object of the present invention to provide a technique for producing an Nb-based alloy that is stable at high temperatures and has excellent oxidation resistance by sandwiching an Al2O3 layer as an intermediate layer.
【０００４】[0004]
【課題を解決するための手段】本発明は上記課題を解決
するために、Nb基合金基材上に薄いAl箔、さらにその上
にNb3Si5Al2金属間化合物粉末をのせ、真空あるいはAr
ガス雰囲気中で焼結とくに放電プラズマ焼結を行い、Al
箔に周辺の微量の酸素を吸収させ、Nb3Si5Al2層、Nb基
合金基材両者に対して反応が起こらずかつ密着性が良い
Al2O3層を形成させることにより、高温における耐酸化
性に優れかつ被覆層の密着性に優れたNb基合金基材上
に、Al 2 O 3 層さらにその上にNb 3 Si 5 Al 2 層の二層で被覆さ
れた高耐酸化性のNb基合金を作製できることを特徴とす
るNb3Si5Al2−Al2O3 の二層で被覆されたNb基合金及びそ
の製造方法を提供する。In order to solve the above-mentioned problems, the present invention provides a thin Al foil on a Nb-based alloy base material, and a Nb 3 Si 5 Al 2 intermetallic compound powder on it, and then vacuum or Ar
Sintering in a gas atmosphere, especially spark plasma sintering,
The foil absorbs a small amount of oxygen around it, and it does not react with both the Nb 3 Si 5 Al 2 layer and the Nb-based alloy substrate and has good adhesion.
By forming an Al 2 O 3 layer on a Nb-based alloy base material that has excellent oxidation resistance at high temperatures and excellent coating layer adhesion
The Al 2 O 3 layer and a Nb 3 Si 5 Al 2 layer on top of it.
Providing Nb 3 Si 5 A l2 -Al 2 O 3 two layers coated with Nb-based alloy and a manufacturing method thereof, characterized in that it produced a high oxidation resistance of Nb-based alloys.
【０００５】[0005]
【発明の実施の形態】本発明に係る、放電プラズマ焼結
法を用いた高耐酸化性Nb3Si5Al2−Al2O3二層被覆Nb基合
金作製技術の実施の形態を実施例、実験例等に基づいて
図面を参照して説明する。本発明は、Nb3Si5Al2層とNb
基合金基材の密着性を向上させ、かつ高温において両者
の拡散反応を抑制するために、両者の間に薄いAl箔を挟
んで放電プラズマ焼結を行い、焼結中Al箔に周辺の微量
の酸素を吸収させ、Nb3Si5Al2層、Nb基合金基材両者に
対して反応が起こらずかつ密着性が良いAl2O3層を中間
層として形成させることを特徴とする。本発明で言う微
量の酸素とは、Nb基合金基材、Al箔、Nb3Si5Al2金属間
化合物粉末の表面に吸着されたもの、又は真空あるいは
Arガス雰囲気中に微量に存在する酸素を言う。BEST MODE FOR CARRYING OUT THE INVENTION An embodiment of a high oxidation resistance Nb3Si5Al2-Al2O3 two-layer coated Nb-based alloy production technique using a spark plasma sintering method according to the present invention will be described based on Examples and Experimental Examples. Will be described with reference to. The present invention is based on the Nb3Si5Al2 layer and Nb
In order to improve the adhesion of the base alloy base material and to suppress the diffusion reaction of both at high temperature, spark plasma sintering is performed with a thin Al foil sandwiched between the two, and the trace amount of the surrounding Al foil during sintering. It is characterized by forming an Al2O3 layer as an intermediate layer, which absorbs oxygen and has good adhesion to both the Nb3Si5Al2 layer and the Nb-based alloy substrate. The trace amount of oxygen referred to in the present invention, Nb-based alloy substrate, Al foil, those adsorbed on the surface of the Nb3Si5Al2 intermetallic compound powder, or vacuum or
Oxygen present in trace amounts in Ar gas atmosphere.
【０００６】Nb基合金基材とNb3Si5Al2粉末の間にAl箔
を挟んだ理由は次の通りである。Nb基合金基材とNb3Si5
Al2粉末の間にボンディング材として挟む材料を変化さ
せ放電プラズマ焼結を行い、得られた被覆材の組織・密
着性等を検討した結果、高温において安定で、かつ耐酸
化性が期待できる被覆材が作製できるのはボンディング
材としてAl箔を用いる時であることが明らかになった。The reason why the Al foil is sandwiched between the Nb-based alloy base material and the Nb3Si5Al2 powder is as follows. Nb-based alloy substrate and Nb3Si5
As a result of examining the structure and adhesion of the obtained coating material by changing the material sandwiched between Al2 powders as a bonding material and performing spark plasma sintering, a coating material that is stable at high temperatures and can be expected to have oxidation resistance It was clarified that can be manufactured when using Al foil as a bonding material.
【０００７】そして、Nb基合金基材とNb3Si5Al2粉末の
間に何も挟まないで焼結を行うと両者は全く接合しな
い。ボンディング材として他の金属、セラミック等を挟
んでもNb3Si5Al2の融点（約1650℃）以下の温度で接合
しなかったり、接合できる場合も焼結中にNb3Si5Al2
層、ボンディング材、Nb基合金基材三者の間で拡散反応
が起こり、Nb基合金基材上には劣化しやすい被覆層が形
成される。またNb基合金上に被覆する層をAl2O3層のみ
にしても耐酸化性は期待できるが、この場合被覆したAl
2O3層が非常に割れやすく、高温保持中割れたところか
らNb基合金基材の酸化が進むため、Nb基合金基材の高温
における安定で良好な耐酸化性を保持するためにはNb3S
i5Al2−Al2O3二層被覆が必要である。本発明において、
焼結はどのような方法で行っても良いが、放電プラズマ
焼結が望ましい。また、加圧する圧力は２０〜８０ＭＰ
ａが適当であり、特に４０〜８０ＭＰａが望ましい。When sintering is performed without sandwiching anything between the Nb-based alloy base material and the Nb3Si5Al2 powder, the two are not joined at all. Even if other metals or ceramics are sandwiched as a bonding material, they will not be joined at a temperature below the melting point (about 1650 ° C) of Nb3Si5Al2, or if they can be joined, Nb3Si5Al2 will be produced during sintering.
A diffusion reaction occurs between the layer, the bonding material, and the Nb-based alloy substrate, and a coating layer that easily deteriorates is formed on the Nb-based alloy substrate. In addition, the oxidation resistance can be expected even if only the Al2O3 layer is coated on the Nb-based alloy.
Since the 2O3 layer is very fragile and the oxidation of the Nb-based alloy base material progresses from the place where it cracks during high-temperature holding, Nb3S is required to maintain stable and good oxidation resistance of the Nb-based alloy base material at high temperatures.
i5Al2-Al2O3 bilayer coating is required. In the present invention,
The sintering may be performed by any method, but discharge plasma sintering is preferable. Moreover, the pressure to be applied is 20 to 80 MP.
a is suitable, and particularly 40 to 80 MPa is desirable.
【０００８】ここで、本発明の一実施例を説明する。Nb
基合金は高融点で高温強度に優れているが、高温におけ
る耐酸化性は非常に乏しい。このようなNb基合金基材表
面上に薄いAl箔、その上にNb3Si5Al2粉末をのせて放電
プラズマ焼結を行うことにより、密着性が良好でかつ高
温における良好な耐酸化性が期待できるNb3Si5Al2−Al2
O3二層被覆Nb基合金の作製技術を提供することができ
た。Here, an embodiment of the present invention will be described. Nb
The base alloy has a high melting point and excellent strength at high temperatures, but has very poor oxidation resistance at high temperatures. Such a thin Al foil on the surface of the Nb-based alloy substrate, by performing Nd3Si5Al2 powder on it by spark plasma sintering, good adhesion and good oxidation resistance at high temperature Nb3Si5Al2- Al2
We could provide the fabrication technology of O3 two-layer coated Nb-based alloy.
【０００９】（１） Nb基合金基材上に、Al2O3層さら
にその上にNb3Si5Al2層の二層で被覆された高耐酸化性
のNb基合金。
（２） Nb基合金基材上に、Al箔、さらにその上にNb3S
i5Al2金属間化合物粉末をのせて、真空あるいはArガス
雰囲気中で、加圧焼結を行い、焼結中Al箔に周辺の微量
の酸素を吸収させAl2O3層を形成させることにより、Nb3
Si5Al2層及びAl2O3層の二層で被覆された高耐酸化性のN
b基合金の製造方法。
（３） 焼結が放電プラズマ焼結である上記２記載のNb
3Si5Al2層及びAl2O3層の二層で被覆された高耐酸化性の
Nb基合金の製造方法。
（４） 加圧が２０〜８０ＭＰａである上記２又は上記
３記載のNb3Si5Al2層及びAl2O3層の二層で被覆された高
耐酸化性のNb基合金の製造方法。(1) High oxidation resistance obtained by coating a Nb-based alloy base material with an Al 2 O 3 layer and a Nb 3 Si 5 Al 2 layer on the Al 2 O 3 layer .
Nb-based alloy. (2) Al foil on Nb-based alloy substrate and Nb 3 S on it
i 5 Al 2 Intermetallic compound powder is placed and pressure-sintered in a vacuum or Ar gas atmosphere, and the Al foil absorbs a small amount of oxygen in the vicinity to form an Al 2 O 3 layer. By Nb 3
High oxidation resistance N coated with two layers of Si 5 Al 2 layer and Al 2 O 3 layer
b-based alloy manufacturing method. (3) Nb as described in 2 above, wherein the sintering is spark plasma sintering
3 Si 5 Al 2 layer and the Al 2 O 3 layer of high oxidation resistance, which is coated with two layers of
Manufacturing method of Nb-based alloy. (4) The method for producing a highly oxidation-resistant Nb-based alloy coated with two layers of the Nb 3 Si 5 Al 2 layer and the Al 2 O 3 layer according to the above 2 or 3, wherein the pressure is 20 to 80 MPa.
【００１０】実施例及び比較例
放電プラズマ焼結法を用いてNb基材上にNb3Si5Al2層を
被覆した材料の被覆層の密着性を調べるために、Nb基材
とNb3Si5Al2粉末の間に（１）何も挟まない（２）薄いA
l箔を挟む（３）Nb5Si3粉末を挟んだ被覆材を作製し、
得られた試料の組織観察を行った。Examples and Comparative Examples In order to investigate the adhesion of the coating layer of the material in which the Nb3Si5Al2 layer was coated on the Nb substrate by using the spark plasma sintering method, between the Nb substrate and the Nb3Si5Al2 powder (1) Nothing sandwiched (2) Thin A
l Sandwich foil (3) Make a covering material sandwiching Nb5Si3 powder,
The texture of the obtained sample was observed.
【００１１】直径15mm、厚さ4mmのNb基材と焼結後の厚
さが約0.5mmになる重量のNb3Si5Al2（組成Nb-47原子%Si
-20原子%Al）粉末の間に（１）何も挟まない、（２）厚
さ15mmのAl箔を挟む（図１）、（３）焼結後の厚さが0.
2mmになる重量のNb5Si3粉末を挟む、の三通りの状態に
なるようにNb基材等をを内径15mmのグラファイト製のダ
イスにセットした後、グラファイト製型側面の表面温度
1200℃（試料部の温度約1600℃）、加圧力50MPa、真空
度15Pa、保持時間0.6ksの条件で放電プラズマ焼結を行
った。A Nb base material having a diameter of 15 mm and a thickness of 4 mm and a weight of Nb3Si5Al2 (composition Nb-47 atomic% Si, which makes the thickness after sintering about 0.5 mm).
-20 atom% Al) powder (1) Nothing is sandwiched, (2) 15 mm thick Al foil is sandwiched (Fig. 1), (3) Thickness after sintering is 0.
The surface temperature of the side surface of the graphite mold is set after setting the Nb base material, etc. in a graphite die with an inner diameter of 15 mm so that there are three ways of sandwiching Nb5Si3 powder with a weight of 2 mm.
Spark plasma sintering was performed under the conditions of 1200 ° C (temperature of the sample part: about 1600 ° C), applied pressure of 50 MPa, vacuum degree of 15 Pa, and holding time of 0.6 ks.
【００１２】焼結後得られた被覆材をマイクロカッター
を用いて切り出し、切り出した試料を樹脂埋めした後、
1mmのダイヤモンドペーストを用いて研磨した。研磨
後、被覆層断面の組織をSEMを用いて観察した。Nb基材
とNb3Si5Al2粉末の間に厚さ15mmのAl箔を挟んで焼結し
て得た被覆材の断面写真を図２（ａ）及び図２（ｂ）に
示す。The coating material obtained after sintering was cut out using a micro cutter, and the cut sample was embedded in resin,
Polished with 1 mm diamond paste. After polishing, the structure of the cross section of the coating layer was observed using SEM. 2 (a) and 2 (b) are cross-sectional photographs of the coating material obtained by sintering a 15 mm thick Al foil sandwiched between a Nb base material and Nb3Si5Al2 powder.
【００１３】Nb基材とNb3Si5Al2粉末の間に何も挟まな
い場合及びNb5Si3粉末を挟んだ場合、被覆層はNb基材に
全く付着しなかったが、図２（ａ）及び図２（ｂ）から
明らかなように、Nb基材とNb3Si5Al2粉末の間に厚さ15m
mのAl箔を挟んで焼結した場合、非常に密着性が良好で
高温における安定性も期待できるNb3Si5Al2−Al2O3二層
被覆Nb基合金が作製できることが明らかになった。When nothing was sandwiched between the Nb base material and the Nb3Si5Al2 powder or when the Nb5Si3 powder was sandwiched, the coating layer did not adhere to the Nb base material at all, but FIGS. 2 (a) and 2 (b) As can be seen from the figure, the thickness between the Nb base material and the Nb3Si5Al2 powder is 15m.
It was clarified that a Nb3Si5Al2-Al2O3 two-layer coated Nb-based alloy with very good adhesion and stability at high temperature could be produced when sintered with m Al foil sandwiched.
【００１４】以上、本発明に係る実施の形態を説明した
が、本発明は以上のような実施例、実験例に示す構成に
限定されることなく、特許請求の範囲記載の技術的事項
の範囲内でいろいろな実施の態様があることは言うまで
もない。The embodiments of the present invention have been described above. However, the present invention is not limited to the configurations shown in the examples and experimental examples described above, and the scope of the technical matters described in the claims is not limited. It goes without saying that there are various embodiments within.
【００１５】[0015]
【発明の効果】以上説明した通り、本発明のを用いて作
製したNb3Si5Al2−Al2O3二層被覆Nb基合金は、中間層と
して形成されたAl2O3層がNb基合金基材とNb3Si5Al2層の
密着性を向上させるばかりでなく拡散防止層としての効
果もあり高温における安定性も期待できることから、耐
酸化性に劣る従来のNb基合金のコーティング技術として
の応用が可能である。As described above, the Nb3Si5Al2-Al2O3 two-layer coated Nb-based alloy produced by using the present invention has an Al2O3 layer formed as an intermediate layer, which has an adhesion between the Nb-based alloy base material and the Nb3Si5Al2 layer. Not only can it be improved, but it can also be expected to have stability as a diffusion prevention layer at high temperatures. Therefore, it can be applied as a coating technology for conventional Nb-based alloys with poor oxidation resistance.
【図１】放電プラズマ焼結法を用いた高耐酸化性Nb3Si5
Al2−Al2O3二層被覆Nb基合金作製技術の概略図Fig. 1 High oxidation resistance Nb3Si5 using spark plasma sintering method
Schematic diagram of Al2-Al2O3 two-layer coating Nb-based alloy production technology
【図２ａ】放電プラズマ焼結法を用いて作製したNb3Si5
Al2−Al2O3二層被覆Nb基合金の被覆層全体の断面写真FIG. 2a: Nb3Si5 produced by spark plasma sintering
Cross-sectional photograph of the entire coating layer of Al2-Al2O3 two-layer coating Nb-based alloy
【図２ｂ】放電プラズマ焼結法を用いて作製したNb3Si5
Al2−Al2O3二層被覆Nb基合金のAl2O3層付近の断面写真FIG. 2b: Nb3Si5 produced by spark plasma sintering
Cross-sectional photograph of the Al2O3 layer near the Al2-Al2O3 two-layer coated Nb-based alloy
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平９−300024（ＪＰ，Ａ) 特開 昭62−30804（ＪＰ，Ａ) 特開 昭61−250101（ＪＰ，Ａ) 村上敬，放電プラズマ焼結法により作 製したＮｂ−Ｓｉ−Ｘ（Ｘ：Ｂ，Ｎ，Ａ １）合金の耐酸化性，機械研ニュース, 日本，1999年 ８月24日，Ｎｏ．８, Ｐ．９−11 (58)調査した分野(Int.Cl.7，ＤＢ名) B22F 1/00 - 9/10 C22C 27/02 ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-9-300024 (JP, A) JP-A-62-30804 (JP, A) JP-A-61-250101 (JP, A) Takashi Murakami, discharge plasma Oxidation resistance of Nb-Si-X (X: B, N, A1) alloy produced by sintering method, Mechanical Research News, Japan, August 24, 1999, No. 8, P. 9-11 (58) Fields surveyed (Int.Cl. 7 , DB name) B22F 1/00-9/10 C22C 27/02
Claims (4)
上にNb3Si5Al2層の二層で被覆された高耐酸化性のNb基
合金。 1. A highly oxidation-resistant Nb-based material comprising a Nb-based alloy base material, an Al 2 O 3 layer, and a Nb 3 Si 5 Al 2 layer coated thereon.
alloy.
にNb3Si5Al2金属間化合物粉末をのせて、真空あるいはA
rガス雰囲気中で、加圧焼結を行い、焼結中Al箔に周辺
の微量の酸素を吸収させAl2O3層を形成させることによ
り、Nb3Si5Al2層及びAl2O3層の二層で被覆された高耐酸
化性のNb基合金の製造方法。2. A Nb-based alloy base material, an Al foil, and Nb 3 Si 5 Al 2 intermetallic compound powder placed on the Al foil.
Nb 3 Si 5 Al 2 layer and Al 2 O 3 layer are formed by performing pressure sintering in an r gas atmosphere and absorbing a small amount of oxygen around the aluminum foil during sintering to form an Al 2 O 3 layer. Method for producing a high oxidation resistance Nb-based alloy coated with two layers.
記載のNb3Si5Al2層及びAl2O3層の二層で被覆された高耐
酸化性のNb基合金の製造方法。3. The sintering is spark plasma sintering.
A method for producing a high oxidation-resistant Nb-based alloy, which is coated with two layers of the Nb 3 Si 5 Al 2 layer and the Al 2 O 3 layer described.
又は請求項３記載のNb3Si5Al2層及びAl2O3層の二層で被
覆された高耐酸化性のNb基合金の製造方法。4. The pressure is 20 to 80 MPa.
Alternatively, a method for producing an Nb-based alloy having high oxidation resistance, which is coated with two layers of the Nb 3 Si 5 Al 2 layer and the Al 2 O 3 layer according to claim 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011080133A (en) * | 2009-10-09 | 2011-04-21 | General Electric Co <Ge> | Oxide forming type protective coating film for niobium-based material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103614713B (en) * | 2013-12-05 | 2015-07-22 | 广西大学 | Method for preparing high-temperature composite coating on niobium-based surface by utilizing sol-gel method |
| CN107900352A (en) * | 2017-12-19 | 2018-04-13 | 哈尔滨理工大学 | A kind of stratiform high niobium containing titanium aluminium alloy composite panel and preparation method thereof |
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| Title |
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| 村上敬，放電プラズマ焼結法により作製したＮｂ−Ｓｉ−Ｘ（Ｘ：Ｂ，Ｎ，Ａ１）合金の耐酸化性，機械研ニュース，日本，１９９９年 ８月２４日，Ｎｏ．８，Ｐ．９−１１ |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011080133A (en) * | 2009-10-09 | 2011-04-21 | General Electric Co <Ge> | Oxide forming type protective coating film for niobium-based material |
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