JP2002146456A - Crack propagation suppressing member and its production method - Google Patents
Crack propagation suppressing member and its production methodInfo
- Publication number
- JP2002146456A JP2002146456A JP2000343571A JP2000343571A JP2002146456A JP 2002146456 A JP2002146456 A JP 2002146456A JP 2000343571 A JP2000343571 A JP 2000343571A JP 2000343571 A JP2000343571 A JP 2000343571A JP 2002146456 A JP2002146456 A JP 2002146456A
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- JP
- Japan
- Prior art keywords
- powder
- matrix
- volume
- tini
- alloy
- 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.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 229910010380 TiNi Inorganic materials 0.000 claims abstract description 37
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 36
- 239000011159 matrix material Substances 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims description 30
- 238000005551 mechanical alloying Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 239000011812 mixed powder Substances 0.000 claims description 11
- 238000002441 X-ray diffraction Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- 230000002401 inhibitory effect Effects 0.000 claims description 2
- 238000000748 compression moulding Methods 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 abstract description 20
- 239000000956 alloy Substances 0.000 abstract description 19
- 229910004337 Ti-Ni Inorganic materials 0.000 abstract description 12
- 229910011209 Ti—Ni Inorganic materials 0.000 abstract description 12
- KHYBPSFKEHXSLX-UHFFFAOYSA-N iminotitanium Chemical compound [Ti]=N KHYBPSFKEHXSLX-UHFFFAOYSA-N 0.000 abstract description 12
- 239000007795 chemical reaction product Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 229940098458 powder spray Drugs 0.000 description 3
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 229910000554 Admiralty brass Inorganic materials 0.000 description 1
- 229910018134 Al-Mg Inorganic materials 0.000 description 1
- 229910018182 Al—Cu Inorganic materials 0.000 description 1
- 229910018467 Al—Mg Inorganic materials 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910009367 Zn M Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000009931 pascalization Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000009704 powder extrusion Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、高エネルギーの衝
撃などが負荷された際の衝突による亀裂の進展を抑止す
る機能を有し、航空機、スペースシャトル等の宇宙移動
手段などの材料に用いて好適な亀裂進展抑止部材に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention has a function of suppressing the growth of a crack due to a collision when a high-energy impact or the like is applied, and is used as a material for space transportation means such as an aircraft and a space shuttle. The present invention relates to a suitable crack growth suppressing member.
【０００２】[0002]
【従来の技術】亀裂進展抑止部材では、通常時は一般の
構造物としての機械的特性を有するが、万一、何らかの
障害物などに衝突して高エネルギーの負荷が加わった際
に、衝突の熱エネルギーにより亀裂先端が局部的に高温
になり、超塑性現象を発現する金属間化合物が生成し、
この金属間化合物が亀裂の進展を抑止する。このような
亀裂進展抑止部材は、航空機の圧カバウンダリーの脆性
破壊防止や、宇宙漂流物対策等で適用が検討されてい
る。2. Description of the Related Art In general, a crack growth suppressing member has mechanical properties as a general structure. However, if a high energy load is applied by colliding with an obstacle or the like, the crushing of the member is prevented. The crack tip is locally heated to a high temperature by thermal energy, and an intermetallic compound that develops a superplastic phenomenon is generated.
This intermetallic compound suppresses crack growth. The application of such a crack growth suppressing member is being studied for preventing brittle fracture of a pressure boundary of an aircraft, countermeasures for space drifting objects, and the like.
【０００３】このような亀裂進展抑止部材としては、
「傾斜機能材料の二一ズ調査」（平成３年３月；（社）
未踏科学技術協会）で開示されたものがあり、以下のよ
うな方法で製造される。まず、Ｔｉ粒子、Ａ１２０３粒
子、ＴｉウイスカおよびＮｉウイスカを予め体積分率を
制御して混合する。この微細混合物を、粉末スプレー積
層法で外面をＴｉ、内面をＡ１２０３として外内面の材
料間組成が一方から他方へ傾斜して変化するように例え
ば管材の表面に成形した後、冷間静水圧形成（ＣＩＰ）
および熱間静水圧成形（ＨＩＰ）を用いて比較的低温・
高圧の処理を行う。この製法による亀裂進展抑止部材に
おいて、ウイスカは、マトリックスの短繊維強化、強靭
性化する働きを有するとともに、部材に高エネルギーの
負荷が加わった際、局部的な発熱によりＴｉとＮｉの共
晶温度（９６０℃）に達し、Ｔｉ−Ｎｉ合金が生成され
ることにより亀裂の進展を抑止するという機能を有す
る。[0003] As such a crack growth suppressing member,
"Studies on Functionally Gradient Materials" (March 1991; company)
There is one disclosed by the Japan Society of Unexplored Science and Technology, and is manufactured by the following method. First, Ti particles are mixed by controlling the A1 2 0 3 particles, pre volume fraction of Ti whiskers and Ni whiskers. After the fine mixture was molded outer surface with a powder spray lamination Ti, inner surface of A1 2 0 3 as the surface of for example the tubing so that the material between the composition of the outer interior surface is changed to be inclined from one to the other, cold Hydrostatic pressure formation (CIP)
And relatively low temperature using hot isostatic pressing (HIP)
Perform high pressure processing. In the crack growth suppressing member manufactured by this method, the whisker has the function of reinforcing the matrix with short fibers and increasing the toughness, and when a high energy load is applied to the member, the eutectic temperature of Ti and Ni due to local heat generation. (960 ° C.), and has the function of suppressing the growth of cracks by the generation of a Ti—Ni alloy.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、上述の
組織構造を有する亀裂進展抑止部材では、衝突などの高
エネルギーの負荷が加わったときに所望の合金のみが形
成されるとは限らない。すなわち、マトリックスに分散
したＴｉとＮｉが反応してＴｉ−Ｎｉ合金が生成される
だけではなく、ＴｉおよびＮｉとマトリックス合金との
反応も生じ、各種の生成物が形成され易い。このような
生成物は、衝突による亀裂進展の抑止に寄与するＴｉ−
Ｎｉ合金の生成量を減少させたり、新たな亀裂進展の起
点となる可能性を高くするため好ましくない。したがっ
て、マトリックス合金中に所望の合金組成を分散しただ
けの組織構造では、亀裂進展を抑止する効果を十分発揮
することができない恐れがある。However, in the crack growth suppressing member having the above-described structure, only a desired alloy is not always formed when a high energy load such as a collision is applied. That is, not only does Ti and Ni dispersed in the matrix react to form a Ti-Ni alloy, but also a reaction between Ti and Ni and the matrix alloy occurs, and various products are easily formed. Such products contribute to Ti-
This is not preferable because it reduces the amount of Ni alloy produced or increases the possibility of starting a new crack growth. Therefore, a structure in which a desired alloy composition is merely dispersed in a matrix alloy may not be able to sufficiently exhibit the effect of suppressing crack growth.
【０００５】さらに、粉末スプレー積層法は傾斜組成を
持った材料の成形法として有効な手段であるが、厚さの
ある大型の構造部品、三次元的に造形された複雑形状部
品の成形法には向かない。また、成形後の固化および繊
密化の手段としてＣＩＰおよびＨＩＰは極めて有効であ
るが、ゴム型あるいは缶などの加圧媒体への封入の工程
を必要とし、最終的な寸法精度を得るための機械加工が
必要であるため、全体の製造工程が煩雑となる。Further, the powder spray lamination method is an effective means as a method for molding a material having a gradient composition. However, the powder spray lamination method is not suitable for molding a large-sized structural part having a large thickness or a three-dimensionally shaped complex-shaped part. Is not suitable. CIP and HIP are extremely effective as means for solidification and densification after molding, but require a step of encapsulation in a pressurized medium such as a rubber mold or a can, and are required to obtain final dimensional accuracy. Since machining is required, the entire manufacturing process becomes complicated.
【０００６】したがって、本発明は、高エネルギの負荷
が加わったときにマトリックスとの反応生成物を形成せ
ず、所望のＴｉ−Ｎｉ合金が充分に形成されるととも
に、製造工程を簡略化することができる亀裂進展抑止部
材を提供することを目的としている。Accordingly, the present invention does not form a reaction product with a matrix when a high energy load is applied, allows a desired Ti-Ni alloy to be sufficiently formed, and simplifies a manufacturing process. It is an object of the present invention to provide a crack growth suppressing member capable of cracking.
【０００７】[0007]
【課題を解決するための手段】本発明の亀裂進展抑止部
材は、マトリックス中に、Ｔｉ：４５〜６５体積％で残
部がＮｉであって、ＴｉとＮｉが微細な層状組織または
非晶質組織であるＴｉＮｉ相が全体の１０〜５０体積％
分散することを特徴としている。以下、本発明の数値限
定の根拠を本発明の作用とともに説明する。According to the present invention, there is provided a crack growth suppressing member comprising: a matrix having 45 to 65% by volume of Ti and the balance of Ni; Is 10 to 50% by volume of the whole
It is characterized by being dispersed. Hereinafter, the basis of the numerical limitation of the present invention will be described together with the operation of the present invention.
【０００８】ＴｉＮｉ相：全体の１０〜５０体積％ マトリックス中のＴｉＮｉ相の体積比が１０％未満で
は、衝突による亀裂進展を防止するように機能するＴｉ
−Ｎｉ合金の生成量が少なく、亀裂進展抑止の効果が得
られない。ＴｉＮｉ相の体積比の増加に伴いＴｉ−Ｎｉ
合金の形成量が多くなり亀裂進展抑止の効果は向上する
が、ＴｉＮｉ相の体積比が５０％を超えると亀裂進展抑
止の効果は高まるものの構造部材としての強度が低下す
る。よって、マトリックス中のＴｉＮｉ相の体積比は１
０〜５０％とした。[0008] TiNi phase: The volume ratio of TiNi phase in total 10 to 50 volume percent matrix is less than 10%, functions to prevent crack growth by collision Ti
-The amount of Ni alloy generated is small, and the effect of suppressing crack growth cannot be obtained. As the volume ratio of the TiNi phase increases, Ti-Ni
Although the formation amount of the alloy increases and the effect of suppressing crack growth is improved, when the volume ratio of the TiNi phase exceeds 50%, the effect of suppressing crack growth increases but the strength as a structural member decreases. Therefore, the volume ratio of the TiNi phase in the matrix is 1
0 to 50%.
【０００９】ＴｉＮｉ相中のＴｉ：４５〜６５体積％ ＴｉＮｉ相中のＴｉが４５体積％未満の場合は、残部の
Ｎｉが多くなり過ぎてＮｉとマトリックスとの各種反応
生成物の形成が多くなる。一方、ＴｉＮｉ相中のＴｉが
６５体積％を超えるとＴｉが多くなるためＴｉとマトリ
ックスとの各種反応生成物の形成が多くなる。よって、
ＴｉＮｉ相中のＴｉは４５〜６５体積％とした。[0009] Ti in the TiNi phase: 45 to 65% by volume When the Ti in the TiNi phase is less than 45% by volume, the remaining Ni becomes too large, and the formation of various reaction products between Ni and the matrix increases. . On the other hand, if the Ti in the TiNi phase exceeds 65% by volume, the amount of Ti increases, so that the formation of various reaction products between Ti and the matrix increases. Therefore,
Ti in the TiNi phase was 45 to 65% by volume.
【００１０】ただし、ＴｉＮｉ相中のＴｉとＮｉとが予
め合金化していると、Ｔｉ−Ｎｉ合金生成によるエネル
ギーの吸収が行われず亀裂進展抑止の効果がなくなるの
で、ＴｉとＮｉは独立して存在している必要がある。さ
らに、ＴｉとＮｉが近接していないとＴｉ−Ｎｉ合金だ
けでなくＴｉもしくはＮｉとマトリックスとの反応生成
物が形成されることとなる。したがってＴｉＮｉ相は、
ＴｉとＮｉが交互に重なり合った微細な層状組織または
ＴｉとＮｉが混合された非晶質組織であることが必要で
ある。However, if Ti and Ni in the TiNi phase are pre-alloyed, energy is not absorbed by the formation of the Ti—Ni alloy and the effect of suppressing crack propagation is lost, so that Ti and Ni exist independently. Need to be. Further, if Ti and Ni are not close to each other, not only a Ti-Ni alloy but also a reaction product of Ti or Ni with a matrix will be formed. Therefore, the TiNi phase is
It is necessary to have a fine layered structure in which Ti and Ni alternately overlap or an amorphous structure in which Ti and Ni are mixed.
【００１１】微細な層状組織のＴｉＮｉ相は、ＴｉとＮ
ｉとが常に近接した状態で維持できるため、高エネルギ
ーの負荷が加わった際、Ｔｉ−Ｎｉ合金の生成が容易と
なるとともにマトリックスとの反応生成物の形成を防止
でき、亀裂進展抑止の効果を高くすることができる。ま
た非晶質組織のＴｉＮｉ相では、高エネルギーの負荷が
加わった際、結晶質のＴｉ−Ｎｉ合金が晶出することに
よりエネルギーを吸収し亀裂進展を抑止する。The TiNi phase having a fine layered structure is composed of Ti and N
i can always be kept in close proximity to each other, so that when a high energy load is applied, it becomes easy to form a Ti-Ni alloy, and it is possible to prevent the formation of a reaction product with the matrix, and to suppress the crack growth. Can be higher. In addition, in a TiNi phase having an amorphous structure, when a high energy load is applied, a crystalline Ti—Ni alloy is crystallized, thereby absorbing energy and suppressing crack propagation.
【００１２】次に、本発明の亀裂進展抑止部材の製造方
法は、Ｔｉ：４５〜６５体積％および残部：Ｎｉであっ
て、ＴｉとＮｉが微細な層状組織または非晶質組織であ
るＴｉＮｉ粉：１０〜５０体積％にマトリックス粉：残
部を混合して圧縮成形し、焼結することを特徴としてい
る。Next, the method for producing a crack growth suppressing member according to the present invention is directed to a TiNi powder in which Ti: 45 to 65% by volume and the balance: Ni, wherein Ti and Ni have a fine layered structure or an amorphous structure. : 10 to 50% by volume, the matrix powder: the remainder is mixed, compression-molded, and sintered.
【００１３】微細な層状組織または非晶質組織を有する
ＴｉＮｉ粉は、Ｔｉ粉：４５〜６５体積％およびＮｉ
粉：残部からなる混合粉に対して２０分〜５時間メカニ
カルアロイング処理を施すことで製造することができ
る。The TiNi powder having a fine layered structure or amorphous structure is composed of 45 to 65% by volume of Ti powder and Ni powder.
Powder: The powder can be produced by subjecting a mixed powder consisting of the remainder to mechanical alloying treatment for 20 minutes to 5 hours.
【００１４】上記製造方法によれば、メカニカルアロイ
ング処理により、ＴｉとＮｉが層状に微細に分散する組
織または非晶質合金の組織を得ることができ、また、粉
末スプレー積層法やＣＩＰ、ＨＩＰと比べて極めて簡便
である。ただし、メカニカルアロイング処理の時間が短
すぎるとＴｉとＮｉの層状組織が得られず、Ｔｉまたは
Ｎｉのみの部分が残留した偏析の多いものとなり、亀裂
進展抑止の効果が乏しくなる。一方、処理時間が長い
と、ＴｉとＮｉが合金化してしまい亀裂進展抑止の効果
が乏しくなる。このような観点から、処理時間は２０分
〜５時間が望ましく、３０分〜４時間であればさらに好
適である。According to the above-described manufacturing method, a structure in which Ti and Ni are finely dispersed in a layer or a structure of an amorphous alloy can be obtained by a mechanical alloying treatment. It is extremely simple compared to. However, if the time of the mechanical alloying treatment is too short, a layered structure of Ti and Ni cannot be obtained, and a portion of only Ti or Ni remains and a large amount of segregation occurs, and the effect of suppressing crack growth is poor. On the other hand, if the treatment time is long, Ti and Ni are alloyed, and the effect of suppressing crack growth becomes poor. From such a viewpoint, the processing time is preferably 20 minutes to 5 hours, and more preferably 30 minutes to 4 hours.
【００１５】[0015]
【発明の実施の形態】以下、本発明の好ましい実施の形
態を説明する。ＴｉＮｉ相の組織状態は、ＴｉＮｉ相、
およびＴｉ粉末とＮｉ粉末を混合しただけの混合粉末に
ついて、Ｘ線回折を行った際のＴｉおよびＮｉのピーク
強度を比較することで調べることができる。Ｘ線回折に
よるピーク強度の比較は、ＴｉもしくはＮｉの各々の元
素のピーク全てについて比較することが望ましいが、ピ
ーク強度の高い３つの線（３強線）のピーク強度のみで
比較しても差し支えない。DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, preferred embodiments of the present invention will be described. The structure state of the TiNi phase is TiNi phase,
It can be examined by comparing peak intensities of Ti and Ni when X-ray diffraction is performed on a mixed powder obtained by mixing Ti powder and Ni powder only. It is desirable to compare the peak intensities by X-ray diffraction for all peaks of each element of Ti or Ni, but it is also possible to compare only the peak intensities of three lines (three strong lines) having high peak intensities. Absent.
【００１６】Ｔｉ粉末とＮｉ粉末の混合粉末のＴｉおよ
びＮｉの各々の３強線のピーク強度合計に対するＴｉＮ
ｉ相のＴｉおよびＮｉの各々の３強線のピーク強度合計
の比（以下、ピーク強度比と称する）が５０％を超えて
いる場合は、ＴｉもしくはＮｉの偏析が残留している状
態を示しており、高エネルギーの負荷が加わった際、効
率よくＴｉ−Ｎｉ合金の反応生成が行われないばかり
か、偏析したＴｉもしくはＮｉとマトリックスとの反応
生成物が形成されることとなる。また、ピーク強度比が
５％に満たない場合は、ＴｉとＮｉの合金化が進行して
いる状態を示しており、亀裂進展抑止の効果が乏しくな
る。したがって、ピーク強度比は、５〜５０％であるこ
とが望ましい。TiN with respect to the total peak intensity of the three strong lines of Ti and Ni of the mixed powder of Ti powder and Ni powder
When the ratio of the peak intensity sum of the three strong lines of each of the i-phase Ti and Ni (hereinafter, referred to as peak intensity ratio) exceeds 50%, it indicates that the segregation of Ti or Ni remains. Therefore, when a high energy load is applied, not only is the reaction generation of the Ti—Ni alloy not performed efficiently, but also a reaction product of the segregated Ti or Ni and the matrix is formed. Further, when the peak intensity ratio is less than 5%, it indicates that alloying of Ti and Ni is in progress, and the effect of suppressing crack growth is poor. Therefore, the peak intensity ratio is desirably 5 to 50%.
【００１７】本発明の亀裂進展抑止部材は、粉末冶金法
により製造することができる。すなわち、原料粉末とし
てＴｉ粉末、Ｎｉ粉末およびマトリックス粉末の混合粉
を用い、混合粉を金型内で上下方向より圧縮成形した成
形体を焼結する方法、混合粉をラバー等に封入して静水
圧成形した成形体を焼結する方法、混合粉を缶等に封入
して高温静水圧成形した後缶材を除去する方法、粉末押
出し法により混合粉を押出し成形した成形体を焼結する
方法等が挙げられる。The crack growth suppressing member of the present invention can be manufactured by a powder metallurgy method. That is, a method of using a mixed powder of Ti powder, Ni powder and matrix powder as raw material powder, sintering a compact obtained by compressing the mixed powder in a vertical direction in a mold, enclosing the mixed powder in a rubber or the like, and statically A method of sintering a compact formed by hydraulic molding, a method of enclosing a mixed powder in a can or the like, removing a can material after high-temperature isostatic pressing, and a method of sintering a molded body formed by extruding a mixed powder by powder extrusion. And the like.
【００１８】本発明の亀裂進展抑止部材のマトリックス
としては、軽量かつ高強度で、加工性の良好なものが好
ましく、ＣｕもしくはＣｕ合金、またはＡｌもしくはＡ
ｌ合金が好適である。たとえば、ＪＩＳ３３００「銅お
よび銅合金継目無管」に規定される建築配管用銅管の無
酸素銅・りん脱酸銅などの純Ｃｕ系、各種プラントの熱
交換器管用のアドミラルティ黄銅（Ｃ４４３０）、アル
ミニウム黄銅（Ｃ６８７０）、キュプロニッケル（Ｃ７
０６０，Ｃ７１５０，Ｃ７１６４）等のＣｕおよびＣｕ
合金、また加工性に優れる純Ａｌ（ＪＩＳ１０００
系）、耐熱性・強度に優れるＡｌ−Ｃｕ系（２０００
系）、耐食性・加工性に優れるＡｌ−Ｍｇ系（３０００
系）、耐食性・押し出し性に優れるＡｌ−Ｍｇ−ｓｉ系
（６０００系）、溶接性・強度に優れるＡｌ−Ｚｎ−Ｍ
ｇ系（７０００系）等のＡｌおよびＡｌ合金が挙げられ
る。The matrix of the member for inhibiting crack growth of the present invention is preferably a lightweight, high-strength material having good workability, such as Cu or Cu alloy, or Al or A.
1 alloy is preferred. For example, pure Cu-based materials such as oxygen-free copper and phosphorous deoxidized copper for copper pipes for building piping specified in JIS 3300 "Copper and copper alloy seamless pipes", and Admiralty brass for heat exchanger tubes of various plants (C4430) , Aluminum brass (C6870), cupronickel (C7
060, C7150, C7164) and the like.
Alloy and pure Al with excellent workability (JIS1000
System), Al-Cu system (2000)
System), Al-Mg system (3000) with excellent corrosion resistance and workability
System), Al-Mg-si system (6000 system) with excellent corrosion resistance and extrudability, Al-Zn-M with excellent weldability and strength
Al and Al alloys such as g-based (7000-based) are exemplified.
【００１９】[0019]
【実施例】以下、具体的な実施例を参照して本発明をさ
らに詳細に説明する。 ［実施例１］原料粉として、Ｔｉ粉（平均粒度：３０μ
ｍ）、カーボニルＮｉ粉（平均粒度：１μｍ）を使用
し、５０体積％のＴｉ粉をＮｉ粉に配合して混合した
後、メカニカルアロイング処理を行った。メカニカルア
ロイング処理は、凝着防止のためメタノールを添加した
Ａｒ雰囲気中で、原料粉の投入量を５００ｇ、処理時間
を０．１〜４時間として行った。得られたＴｉＮｉ相お
よびメカニカルアロイング処理前の混合粉について、そ
れぞれＸ線回折を行い、ＴｉとＮｉの３強線のピーク強
度の合計を測定した結果を表１に示す。また、ＴｉＮｉ
相の組織状態の評価を表１に併せて示す。さらに、図１
および図２に、メカニカルアロイング処理時間が２時間
および４時間のＴｉＮｉ相の組織写真を示す。Hereinafter, the present invention will be described in more detail with reference to specific examples. [Example 1] Ti powder (average particle size: 30 µ
m) and carbonyl Ni powder (average particle size: 1 μm), and after mixing and mixing 50% by volume of Ti powder with Ni powder, a mechanical alloying treatment was performed. The mechanical alloying treatment was performed in an Ar atmosphere to which methanol was added to prevent adhesion, with the amount of the raw material powder charged being 500 g and the treatment time being 0.1 to 4 hours. Table 1 shows the results obtained by performing X-ray diffraction on the obtained TiNi phase and the mixed powder before the mechanical alloying treatment, and measuring the total peak intensity of the three strong lines of Ti and Ni. Also, TiNi
Table 1 also shows the evaluation of the phase structure. Further, FIG.
2 and FIG. 2 show microstructure photographs of the TiNi phase when the mechanical alloying treatment time is 2 hours and 4 hours.
【００２０】[0020]
【表１】 [Table 1]
【００２１】図１および図２から判るように、処理時間
が２時間では、未反応のＴｉとＮｉが層状および非晶質
の状態で微細に分散した組織、処理時間が４時間では、
ＴｉとＮｉが非晶質の状態で微細に分散した組織が得ら
れた。また、図示は省略したが、処理時間が３０分では
未反応のＴｉとＮｉが層状に微細に分散した組織が得ら
れた。この結果により、メカニカルアロイング処理の時
間を３０分〜４時間とすることで、層状組織または非晶
質組織からなる所望のＴｉＮｉ相が得られることが確認
された。なお、メカニカルアロイング処理の時間を２０
分〜５時間とすることでも層状組織または非晶質組織か
らなるＴｉＮｉ相が得られるものと推測される。As can be seen from FIGS. 1 and 2, when the processing time is 2 hours, the structure in which unreacted Ti and Ni are finely dispersed in a layered and amorphous state, and when the processing time is 4 hours,
A structure in which Ti and Ni were finely dispersed in an amorphous state was obtained. Although not shown in the drawing, a structure in which unreacted Ti and Ni were finely dispersed in a layered manner was obtained in a processing time of 30 minutes. From these results, it was confirmed that a desired TiNi phase composed of a layered structure or an amorphous structure was obtained by setting the mechanical alloying treatment time to 30 minutes to 4 hours. The time of the mechanical alloying process is set to 20.
It is presumed that a TiNi phase composed of a layered structure or an amorphous structure can be obtained even when the time is from 5 minutes to 5 hours.
【００２２】また、表１の結果から、ＴｉＮｉ相の粉末
Ｘ線回折の３強線のピーク強度の合計が、メカニカルア
ロイング処理前の単純混合物の３強線のピーク強度の合
計の５〜５０％の強度比となるようにメカニカルアロイ
ングを行うことにより、ＴｉとＮｉが層状に微細に分散
する組織または非晶質合金の組織を呈し、合金化が不完
全なＴｉＮｉ相が得られることが判った。Also, from the results in Table 1, the sum of the peak intensities of the three strong lines in the powder X-ray diffraction of the TiNi phase is 5 to 50 times the sum of the peak intensities of the three strong lines of the simple mixture before the mechanical alloying treatment. % By mechanical mechanical alloying so as to obtain a structure in which Ti and Ni are finely dispersed in a layer or an amorphous alloy structure, and a TiNi phase incompletely alloyed can be obtained. understood.
【００２３】［実施例２］粒度：８８μｍ以下の電解Ｃ
ｕ粉末に、実施例１において２時間のメカニカルアロイ
ング処理を行ったＴｉＮｉ相からなる粉末を体積比で１
０％、３０％、５０％をそれぞれ配合し、混合した後、
ホットプレスを用い焼結固化した。素材の形状は直径５
０ｍｍで高さが５ｍｍの円板状とし、ホットプレス条件
は、ＣｕマトリックスとＴｉＮｉ相が著しく反応しない
温度範囲の６５０℃、保持時間３０分間、雰囲気５×１
０−２Ｔｏｒｒの真空中で、加圧力４００ｋｇｆ／ｃｍ
２で行った。試料の評価は、素材から切り出した１０×
１０×５ｍｍの試験片表面に電流３０〜３５Ａ、照射時
間が１〜４秒の範囲で高エネルギーのレーザを照射した
後、照射部の切断面におけるＴｉＮｉ合金の形成状況を
Ｘ線回折により分析した。Example 2 Electrolytic C having a particle size of 88 μm or less
The powder composed of the TiNi phase subjected to the mechanical alloying treatment for 2 hours in Example 1 was added to the u powder at a volume ratio of 1
After blending 0%, 30% and 50% respectively, and mixing,
It was sintered and solidified using a hot press. The shape of the material is diameter 5
0 mm and a disk shape with a height of 5 mm. The hot pressing conditions were 650 ° C. in a temperature range where the Cu matrix and the TiNi phase did not significantly react, a holding time of 30 minutes, and an atmosphere of 5 × 1.
Pressure of 400 kgf / cm in a vacuum of 0 -2 Torr
2 was performed. The evaluation of the sample is 10 ×
After irradiating a high-energy laser to a 10 × 5 mm specimen surface with a current of 30 to 35 A and an irradiation time of 1 to 4 seconds, the formation state of the TiNi alloy on the cut surface of the irradiated portion was analyzed by X-ray diffraction. .
【００２４】図３〜図５は、上記試料のレーザ照射部分
周辺のＸ線回折パターンを示すチャートである。これら
のチャートから明らかなように、何れの試料についても
ＣｕマトリックスとＴｉおよびＮｉとの反応物は観察さ
れなかった。また、いずれの試料についても、ＴｉＮｉ
相がレーザのエネルギーにより合金化したＴｉ−Ｎｉ合
金（◎印）が認められ、本発明におけるＴｉＮｉ相の効
果が確認された。FIGS. 3 to 5 are charts showing X-ray diffraction patterns around the laser-irradiated portion of the sample. As is clear from these charts, no reaction products of the Cu matrix with Ti and Ni were observed in any of the samples. In addition, for all samples, TiNi
A Ti—Ni alloy in which the phase was alloyed by the energy of the laser (marked with ◎) was recognized, and the effect of the TiNi phase in the present invention was confirmed.
【００２５】[0025]
【発明の効果】以上説明したように本発明によれば、マ
トリックス中に、ＴｉとＮｉが微細な層状組織または非
晶質組織であるＴｉＮｉ相が分散したものであるから、
衝突等の高エネルギー負荷が発生した際、ＴｉとＮｉが
確実に反応してＴｉ−Ｎｉ合金を形成し、上記エネルギ
ーを吸収するとともに、ＴｉもしくはＮｉとマトリック
スの反応生成物の形成を防止でき、効率よく亀裂進展を
防止することができる。As described above, according to the present invention, since Ti and Ni are dispersed in a matrix, a TiNi phase having a fine layered structure or an amorphous structure is dispersed.
When a high energy load such as a collision occurs, Ti and Ni surely react to form a Ti-Ni alloy, absorb the energy, and prevent the formation of a reaction product of Ti or Ni and the matrix, Crack growth can be efficiently prevented.
【図１】 本発明の実施例の金属組織を示す図であっ
て、２時間のメカニカルアロイング処理を行ったときの
ＴｉＮｉ相を示すものである。FIG. 1 is a view showing a metal structure of an example of the present invention, showing a TiNi phase when a mechanical alloying process is performed for 2 hours.
【図２】 本発明の実施例の金属組織を示す図であっ
て、４時間のメカニカルアロイング処理を行ったときの
ＴｉＮｉ相を示すものである。FIG. 2 is a view showing a metal structure of an example of the present invention, showing a TiNi phase when a mechanical alloying process is performed for 4 hours.
【図３】 本発明の実施例における試料のレーザ照射部
分周辺のＸ線回折パターンである。FIG. 3 is an X-ray diffraction pattern around a laser-irradiated portion of a sample in an example of the present invention.
【図４】 本発明の実施例における試料のレーザ照射部
分周辺のＸ線回折パターンである。FIG. 4 is an X-ray diffraction pattern around a laser-irradiated portion of a sample in an example of the present invention.
【図５】 本発明の実施例における試料のレーザ照射部
分周辺のＸ線回折パターンである。FIG. 5 is an X-ray diffraction pattern around a laser-irradiated portion of a sample in an example of the present invention.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 四方 英雄 千葉県松戸市大金平１−48−１ Ｆターム(参考） 4K018 AA03 AA14 BA02 BA03 BA04 BA08 BC16 KA61 KA62 ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Hideo Shikata 1-48-1, Daikindaira, Matsudo-shi, Chiba F-term (reference) 4K018 AA03 AA14 BA02 BA03 BA04 BA08 BC16 KA61 KA62
Claims (5)
積％および残部：Ｎｉであって、ＴｉとＮｉが微細な層
状組織または非晶質組織であるＴｉＮｉ相が、全体の１
０〜５０体積％分散することを特徴とする亀裂進展抑止
部材。1. A TiNi phase in which 45 to 65% by volume of Ti and the balance: Ni in which Ti and Ni are a fine layered structure or an amorphous structure is contained in a matrix.
A crack growth suppressing member characterized by being dispersed in 0 to 50% by volume.
金、またはＡｌもしくはＡｌ合金であることを特徴とす
る請求項１に記載の亀裂進展抑止部材。2. The member according to claim 1, wherein the matrix is Cu or a Cu alloy, or Al or an Al alloy.
およびＮｉの各々の３強線のピーク強度の合計は、その
原料粉末であるＴｉ粒子およびとＮｉ粒子の混合粉末の
Ｘ線回折におけるＴｉおよびＮｉの各々の３強線のピー
ク強度の合計に対し５〜５０％であることを特徴とする
請求項１または２に記載の亀裂進展抑止部材。3. An X-ray diffraction of the TiNi phase
Is the sum of the peak intensities of the three strong lines of Ti and Ni in the X-ray diffraction of the mixed powder of the Ti particles and the Ni particles as the raw material powder. The crack growth suppressing member according to claim 1 or 2, wherein the content is 5 to 50%.
ｉであって、ＴｉとＮｉが微細な層状組織または非晶質
組織であるＴｉＮｉ粉：１０〜５０体積％にマトリック
ス粉：残部を混合して圧縮成形し、焼結することを特徴
とする亀裂進展抑止部材の製造方法。4. Ti: 45 to 65% by volume and balance: N
i, a crack characterized by mixing TiNi powder having a fine layered structure or amorphous structure with Ti and Ni: 10 to 50% by volume, matrix powder: remainder, compression molding, and sintering. A method for manufacturing a progress inhibiting member.
体積％およびＮｉ粉：残部からなる混合粉に対して２０
分〜５時間メカニカルアロイング処理を施した粉末であ
ることを特徴とする請求項４に記載の亀裂進展抑止部材
の製造方法。5. The method according to claim 1, wherein the TiNi powder is Ti powder: 45 to 65.
Volume% and Ni powder: 20 based on the mixed powder consisting of the balance
The method for producing a crack growth suppressing member according to claim 4, wherein the powder is a powder that has been subjected to a mechanical alloying treatment for minutes to 5 hours.
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|---|---|---|---|
| JP2000343571A JP4535601B2 (en) | 2000-11-10 | 2000-11-10 | Crack growth inhibiting member and manufacturing method thereof |
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| JP4535601B2 JP4535601B2 (en) | 2010-09-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002332506A (en) * | 2001-05-07 | 2002-11-22 | Central Res Inst Of Electric Power Ind | Structure material having function of suppressing propagation of cracking |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63118002A (en) * | 1986-11-05 | 1988-05-23 | Mitsui Eng & Shipbuild Co Ltd | Production of fine amorphous particle |
| JPH0565584A (en) * | 1991-09-05 | 1993-03-19 | Yoshida Kogyo Kk <Ykk> | Production of high strength aluminum alloy powder |
| JPH09111313A (en) * | 1995-10-17 | 1997-04-28 | Masumoto Takeshi | Production of aluminum alloy powder for high-strength aluminum alloy molding and production of high-strength aluminum alloy molding |
| JPH1150102A (en) * | 1998-05-26 | 1999-02-23 | Japan Storage Battery Co Ltd | Production of hydrogen storage alloy powder for battery |
-
2000
- 2000-11-10 JP JP2000343571A patent/JP4535601B2/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63118002A (en) * | 1986-11-05 | 1988-05-23 | Mitsui Eng & Shipbuild Co Ltd | Production of fine amorphous particle |
| JPH0565584A (en) * | 1991-09-05 | 1993-03-19 | Yoshida Kogyo Kk <Ykk> | Production of high strength aluminum alloy powder |
| JPH09111313A (en) * | 1995-10-17 | 1997-04-28 | Masumoto Takeshi | Production of aluminum alloy powder for high-strength aluminum alloy molding and production of high-strength aluminum alloy molding |
| JPH1150102A (en) * | 1998-05-26 | 1999-02-23 | Japan Storage Battery Co Ltd | Production of hydrogen storage alloy powder for battery |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002332506A (en) * | 2001-05-07 | 2002-11-22 | Central Res Inst Of Electric Power Ind | Structure material having function of suppressing propagation of cracking |
| JP4591985B2 (en) * | 2001-05-07 | 2010-12-01 | 財団法人電力中央研究所 | Structural material |
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| Publication number | Publication date |
|---|---|
| JP4535601B2 (en) | 2010-09-01 |
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