JPS5932841A - Adjusting method of sample whose multiple surfaces are simultaneously observed - Google Patents
Adjusting method of sample whose multiple surfaces are simultaneously observedInfo
- Publication number
- JPS5932841A JPS5932841A JP57142468A JP14246882A JPS5932841A JP S5932841 A JPS5932841 A JP S5932841A JP 57142468 A JP57142468 A JP 57142468A JP 14246882 A JP14246882 A JP 14246882A JP S5932841 A JPS5932841 A JP S5932841A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- fracture
- resin
- observation
- observed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
Abstract
Description
【発明の詳細な説明】 に関する。[Detailed description of the invention] Regarding.
従来,機器や構造拐の破損品の事故解析では。Traditionally, this is used in accident analysis of damaged items such as equipment or structural damage.
破面の観察とtill!損部断面損金断面織を観察しで
行うことが,一般に常套手段として行われている。Observation of fracture surface and till! A common practice is to observe the cross-sectional structure of the loss area.
この場合,破面と金属組織の観察はいずれか一力の観察
だけをそれぞれの観察に適した顕微鏡で行うのが盲進で
ある。これらの破面と組織が同一の試料で,同時に観察
することができれば破壊の経路と金属組織との関連等を
解IJiする場合のイ]効なテークが得られる。In this case, it is best to blindly observe either the fracture surface or the metal structure using a microscope suitable for each observation. If these fracture surfaces and structures can be observed simultaneously in the same sample, an effective solution can be obtained for elucidating the relationship between the fracture route and the metal structure.
この[」的のために使用する観察機器としては焦点深度
の大きい走査型電子顕微鏡が適している。しかし1i〔
来は試料の調整が難しいためにほとんどこの破面−金属
組織同時観察の手法は用いられていなかー、た。すなわ
ち、 (jfl来の試料調整方法として考えられている
手段は次のとおりである。A scanning electron microscope with a large depth of focus is suitable as an observation device for this purpose. But 1i [
In the past, this technique of simultaneous observation of fracture surfaces and metallographic structures was rarely used because it was difficult to prepare samples. That is, (jfl) The methods considered as sample preparation methods are as follows.
観.察試料(3)のI Ipl+を第1図に示す。符8
(1)の面が金属組織を現出させた金属組織現出面で。View. FIG. 1 shows I Ipl+ of sample (3). sign 8
The surface (1) is the metal structure-exposing surface where the metal structure is exposed.
符号(2)の曲が破面を示している。図〕、するように
破面Lの(T石、の断面で組織が現出されなければなら
ないためその試料調整においては,θ(の工稈が必要と
なる。The song numbered (2) shows the fractured surface. Since the structure must be exposed in the cross section of the fracture surface L (T stone) as shown in Figure], a culm of θ( is required in preparing the sample.
1)破面−Lの灯、0,の断面の切断
2)上記切断面のG1磨とエッヂンク
II L 1lii記2)の]稈で、観4j≦試料(3
)が小さくで11vり扱いが難しい、非′畠に軟らかい
、非常に1宛い、又は多孔質′ηのものである場合、最
も重要な+IIは破面(2)と研磨の境界部の縁をだれ
させtl:い小である。これをさけるため1通常観察試
料(3)を国事省略の枠に入れて71J(磨するか、第
2図ないし・zl”33図に示すブーラスチック慴の樹
脂(4)。1) Cutting the cross section of the fracture surface - L lamp, 0, 2) G1 polishing and edging of the above cut surface
) is small and difficult to handle, extremely soft, very thin, or porous, the most important +II is the edge at the interface between the fracture surface (2) and the polishing. It's small. In order to avoid this, one normal observation sample (3) should be placed in the frame of 71J (polishing or polishing, or the plastic resin (4) shown in Figure 2 to Figure 33).
(4)で埋込んで研磨する方法がイ″■なわれている。The method of embedding and polishing is described in (4).
今11では1ilf磨が自動的になさ才t −t、−、
tlIt 11“(而も、11′畠に清浄であることか
ら自動ωL磨機によ−、でfilleが行われる例かは
とんとで゛あるが、この場合第2図ないし第3図にンJ
<すように、被研磨試1[(3)は−f 5スチノクや
エボキン等の樹脂(4)、(4’)で成j1トしなけれ
ば何片できない。、−の樹脂(4)、(4)の成Jに試
イ′Jは11(り扱いに便利で、かつ観察試11(、)
)を都かのよいイ☆jHに置くことが出来る利点もある
。Now in 11, 1ilf polishing is not done automatically t -t, -,
tlIt 11" (However, since it is extremely clean, it is quite possible that the filling is performed using an automatic ωL polishing machine, but in this case, it is shown in Figures 2 and 3.)
As shown above, the polished sample 1 [(3) cannot be made into any number of pieces unless it is made of resin (4), (4') such as -f5 Stinoku or Evokin. , - Resin (4), (4) J' J is convenient to handle and observation test 11 (,)
) has the advantage of being able to be placed in a good I☆jH.
なお、プラスチック宿の樹脂(4)、 (4’>で観察
試t1(3)を埋込むlJ法としては、第2図に示す熱
間埋込み(粉イ、状シラーi ニア−:、>″ノカノi
l圧成1ト) ;[=子。In addition, as for the lJ method of embedding observation test t1 (3) with plastic resin resin (4), (4'>), hot embedding (powder I, shape siller i near-:,>'' shown in Fig. 2) is used. Nokano i
lpressure1t) ;[=child.
3図に示を冷間坤1へみ(′・1危1゛(硬化゛・t−
ろ−]゛−1人チック)かある1、
1差−1で、−1記ニジ)のI程は、12りに小−イイ
)、11)。Figure 3 shows the cold hardening ('・1 danger 1゛(hardening)・t-
ro-]゛-1 person tick) is 1, 1 difference is -1, and -1 mark niji) is smaller than 12), 11).
ハ)の渦稈4経る、:とになる5、
f)−1記りの観察1:A: i[(3)の1刀1斯面
(1)夕1戊11つ枠(5)の下面(7接・I−るよう
にil’l゛き、、f−frス−1’−2’、)やエボ
キノの樹脂(4) 、 (4′)t・卸、察試料(3)
を埋込J」・5、〔1〕埋込4/本試月の観′?3面一
ひj)る金属ξI[織IJ出面(1)をfilf磨徘・
J)ブークする。ユバ)プラスデフ化・やエポ4シの樹
脂(4) 、 (45を侶(′!:テ試t’l (3)
の破面(2)から除去し+ +lIk曲 組織間11、
ン観察試1゛[をiする3゜
ところが、二の二1−稈の中で最もφ仔しい点は。C)'s vortex culm passes through 4, becomes: 5, f)-1 Observation 1: A: i Lower surface (7 contacts, I-like ill'l゛,, f-fr-1'-2',) and ebokino resin (4), (4') t wholesale, inspection sample (3)
Embed J'・5, [1] Embed 4/View of this trial month'? Metal ξI [woven IJ exit surface (1) is polished]
J) Book. Yuba) Plus differential / Epo 4 resin (4), (45 ('!: Te test t'l (3)
Removed from the fracture surface (2) + +lIk intertissue 11,
Observation Trial 1゛[3゜However, the most childish point in the culm is 2-21.
・X)のTf−)ノ、チ、りや−r−ボキ〉・′ηの樹
脂(4) 、 (=+3を除去づる点にある。オなわら
、 i+1来の調整/、法では、破面(2)に凹凸かあ
るため樹脂(4)、 (45がIIii単に破面(2)
が1゛、はずれにり(、又機械的にjHBHBIBに樹
脂(4)、(・1′)を取ると(1°し面(2)を傷つ
けるという不具音がある。。・X)'s Tf-)ノ,chi,riya-r-boki〉・'η's resin (4) , (=+3 is removed.Otherwise, in the adjustment /, law from i+1, Because the surface (2) is uneven, the resin (4) (45 is simply a fractured surface (2)
However, when the resin (4) and (・1') are removed mechanically from the HBHBIB, there is a noise caused by the damage to the surface (2).
本発明は一1記ii’r東の多面同時観察試料の調整J
j法におけろ欠点を11ソリ除き、すでに調整の終えた
観察面あるいは調整不要の観察面を傷つけることがない
多面同時観察試料の調整方法を提供することを目的とす
る。−のため本発明のIJ工程で研摩する面以外の多面
同時観察試料の観察面を軟質膜て覆−3た後、1記試料
を樹脂に埋込み成j[5することを特徴とする多面同時
観察試料の調整ljT去を要旨とする。The present invention is based on the preparation of multifaceted simultaneous observation samples of 11.ii'r East.
It is an object of the present invention to provide a method for preparing a sample for simultaneous observation of multiple surfaces without damaging the observation surface that has already been adjusted or the observation surface that does not require adjustment, by eliminating 11 defects in the J method. - Therefore, after covering the observation surface of the sample for multi-surface simultaneous observation other than the surface to be polished in the IJ process of the present invention with a soft film, the sample described in 1 is embedded in a resin and formed [5]. The gist is the preparation of observation samples.
ここで1曲とは観察面を指す。ぼ−、て多面とは、波曲
−金(4組織観察面以外にも、金属組織観察面−金属組
織観察面や金属組織観察面−表面処理層などをも含むも
のである。Here, 1 song refers to the observation side. In addition to the wave-curved gold (four texture observation surfaces), the term "bond and polygon" includes metal structure observation surfaces-metal structure observation surfaces, metal structure observation surfaces-surface treatment layers, and the like.
また1本発明力性は、破面−組織同時観察試事1をi■
るばかりでなくρりえばメッキ等の金属表面処理層の自
由表向との境界を現出するのにも応用でき、従って層の
厚さの同定も可能となる。In addition, the strength of the present invention is that the fracture surface and structure simultaneous observation trial 1 was
In addition to this, it can also be applied to reveal the boundary between the free surface of a metal surface treatment layer such as plating, and thus the thickness of the layer can also be identified.
以T’に図面を用いて本発明の詳細な説明する。The present invention will be described in detail below with reference to the drawings.
ったもの及びさらにプラスチ1.り樹脂に埋め込んだも
のの模式図である。1. FIG.
高強度網のボルトが折損した破1rii (+2と、そ
の起点を通る断面の金属組織現出曲(1)を同時?j1
9にするため観察試料θ葎をrA整した。まず、ボルト
破面(155の観察試料(1罎を観察に適した厚さに切
IJJiし、さらにキ裂の起点を通るv、1血を切断す
る1、次に、第4図に示すように軟質膜と(、・てのア
ルミニウムのn、 II!′!θ樟で破面02を1aう
、この場合アルミニウムの薄膜(119は数枚重ねても
よい。この観察試料(1葎を金属絹織現出面00をFに
して。A fracture caused by a high-strength mesh bolt breaking 1rii (+2 and the metal structure appearance curve (1) of the cross section passing through the origin at the same time? j1
The observation sample θ was adjusted to rA in order to obtain a value of 9. First, cut the bolt fracture surface (155 observation specimens) to a thickness suitable for observation, and then cut through the starting point of the crack. The fracture surface 02 is covered with a soft film (, II!'! Set silk weaving surface 00 to F.
V〜間の成形枠(1つに入れ、粉末状の熱間用プラスチ
ックの樹脂0養を充填し成形を1工う。この場合加熱温
度は150 ’c〜170℃程度、11力は29MI’
a(4,200psi )とした。ここで1.1.’、
+Lアルミニ・°1ノ、の−1す11らy (+8)
は熱間F人形時に塑り、変形し、1彼u7j Uノl!
41 +”+ IT応シT、−、lr+I (d(t
曲(+31: 0: =、り+−)張り(=Iき結局第
5図に小ず如き状態に成形される。A molding frame between V (Put it in one, fill it with powdered hot-use plastic resin, and perform one molding process. In this case, the heating temperature is about 150'C to 170C, and the power of 11 is 29MI'
a (4,200 psi). Here 1.1. ',
+L aluminum・°1ノ, -1s11ray (+8)
is molded and deformed during hot F doll, 1 U7J U Nol!
41 +”+ IT response T, -, lr+I (d(t
The song (+31: 0: =, ri+-) is stretched (=I) and is eventually formed into the shape shown in Figure 5.
二J)ようにし−(、−、411i込まt’した観察試
料(13は金属I11織現出面QI)をrat +(τ
函、上、Fンタを行い観察試1:’+ (1;うの破面
(11)から−ノ゛−!スチ・りの(るJ脂(14)を
取り除々ことによ−> −r 、 h++、 a−誠1
1 IllやかIt)られる3゜二の場合破面Opとゾ
5・ストノ1樹脂(11)の間にj゛ルミJ・′1ノ・
のイ1.り膜(+8)か→トント・′フイ、7−さlし
た仄態に埋込まれ−Cいるため、 1illi面0:e
i、Lアルi二“+y、・′・の−9膜(18)で保
、;((さイtイU 1)<ことはない。しかもアル<
−、:、 7、のIX、り膜08)は′容易にプラス千
ノ9 (I)Nj ’Ifi 1JJ) ’L ヒ(+
j’f 面(Bj J: ’) :’f、’114m
スル:L トかテh/:l5、又、もう一つの効果とし
て、アルミニラ15の−り膜tllj) l;1金)1
バ絹1哉l(1,出向、1υの縁、すなイ)ら破面(1
υとの境Sl、l面かだれるのを1!7III−、する
ため、非′畠にfJ効な観撃試t’+ c++iが7+
、1られる。2J) The observation sample (13 is metal I11 woven surface QI) which was made as follows -(, -, 411i) is rat + (τ
Observation test 1:'+ (1; By removing the J fat (14) from the broken surface (11) of the case -> r, h++, a-Makoto 1
1 Ill or It) In the case of 3゜2, between the fracture surface Op and the resin (11), there is a
A1. Since the film (+8) is embedded in the left side of the film (+8) → 7-1, the -C is 1illi surface 0:e.
i, L Al i 2 "+y, ・'・ maintained by -9 film (18); ((Sai t I U 1)
-, :, 7, IX, ri film 08) is 'easily plus thousand no 9 (I)Nj 'Ifi 1JJ) 'L hi (+
j'f plane (Bj J: ') :'f, '114m
Suru:L Tokateh/:l5, Also, as another effect, the aluminum film tllj)l;1 Gold)1
The fractured surface (1, seconded, edge of 1υ, sunai)
Since the border Sl and l side with υ are 1!7III-, the observation test t'+ c++i with fJ effect on the non' field is 7+
, 1 will be given.
なお・破面(ゆを覆う軟質+v; J−L、では−1′
ルミ−・7〕、の他に銅やスス等の薄膜(18)でも使
用でき。In addition, the fracture surface (soft +v covering the surface; J-L, -1'
In addition to Lumi-7], thin films such as copper and soot (18) can also be used.
筋□Tも同(7−Cある−とは1、う、L−しもなく、
又試イ[の7iII磨面のエノチ二ノノは−j゛−1−
4−f−21!(〕)b’pJ lliイ04)を除去
した後、破面αQをマスキー・′ノし、7たl −(−
[、rツクを?JうJ二うにしてもよい。3tた1記実
施例−rit粉末状の熱間用プラスチ、りの樹脂(M)
l用いたが、かわりに液状の冷間用シー> 7. +
77の樹1’liyを用いる場合は観察試11(13の
破面(121とj′ルミ、r白l、′、9のい、り膜(
1榎J、の間に樹脂が浸+%し・ないように、観察試t
’) +13をF、すp、r+!(+8)で(旦みJΔ
むなとの配Jaをiする6、
−1−述のとおり1本発明の多面同時観察X 14の調
整力法は、そのL稈て(ilF I!i%ず・\き曲以
外の611察而を軟質膜で覆い、樹脂に埋込んて(’l
: 、i’−するので、該観察面近傍の研摩だれを防き
、1該観察面と樹脂との!11離を翁易に行わしめ、該
観、′!I/:曲をキズなどから保護する作用をなし、
よ−、−(3二面同時観察が容易となる。、Muscle □T is the same (7-C is- is 1, U, L- is not,
Also, the enochininono of the 7iIII polished surface of the trial is -j゛-1-
4-f-21! After removing (]) b'pJ lli 04), the fracture surface αQ was masked and
[, r tsuku? You can do J U J two. 3T Example--Rit Powdered Hot-use Plasti, Rino Resin (M)
7. I used liquid cold water instead. +
When using the tree 1'liy of 77, observation sample 11 (fracture surface of 13 (121 and
1. Observation test to prevent resin from soaking between
') +13 to F, sp, r+! (+8) (Danmi JΔ
6. -1- As mentioned above, the adjustment force method of the present invention's multi-faceted simultaneous observation Cover the sensor with a soft membrane and embed it in resin ('l
: , i'-, so that polishing sag near the observation surface is prevented, and 1. between the observation surface and the resin! I made the 11th separation easy, and the view,'! I/: Protects the song from scratches, etc.
Yo-,-(Simultaneous observation of 3 two sides becomes easy.)
第1図はiZ来の破i’、fii ’−組織同時観察試
A[の1(タリを小才斜視図、第2図は(追N(の熱間
埋込み成jしの概略図、第3図は(1束の冷間1!V込
Jシ成1)ユの概略図、;”Xl 4図は本発明のジノ
法に供する破面をイ;々11ψ−c +xi−,た観察
試験片の模式図、第5図は4\°;仁明の/j法に供オ
ろ破曲庖1i=4 ’&λて覆いシーrス千、ツノの樹
脂を、°」里込んだ観察試験ハの模式図を・j、ず。
l、11・・・金属組織検出1iii 、 2 、12
・・破面、3゜+3・・観察試料、4・・・lλ間川用
I゛−)ス千り勺の樹脂。
・1′、l=1・・f・1(開用−メ゛ラス千、′)の
樹脂 5 、 l 5・・13覧1(・枠、6・・・l
−−3,7・・・シラス千、ツノ樹1t!11IIのi
’i、:)号、18・・・アIL/ミニ−ウドの薄膜式
3臭人 土#、 P、U 暇。
(X
21Figure 1 is a small perspective view of fracture i', fii'-structure simultaneous observation test A [1 (Tari) since iZ, Figure 2 is a schematic diagram of hot embedding of (addition N (), Figure 3 is a schematic diagram of (1 bundle of cold 1! Schematic diagram of the test piece, Figure 5 is 4\\^^^^゜゜゜゜゜゜゜゜゜゜゜〕 Schematic diagram of test c. l, 11...Metal structure detection 1iii, 2, 12
...Fracture surface, 3゜+3...Observation sample, 4...lλ Makawa I゛-) Suzuchireki resin.・1', l=1...f・1 (opening - Melas 1,000,') resin 5, l 5...13 List 1 (・frame, 6...l
--3,7...1,000 whitebaits, 1 ton of horn trees! 11II i
'i, :) issue, 18... AIL/Mini-Udo's thin film type 3 odor person Sat #, P, U I'm bored. (X 21
Claims (1)
を軟質膜で覆った後、上記試料を樹脂に埋込み成1[?
することを特徴とする多1hi同時観察試料の調整方法
。After covering the observed surface of the sample with a soft film for simultaneous observation of multiple surfaces outside the chamfered culm (+11), the sample was embedded in resin and formed 1[?
1. A method for preparing samples for multiple 1-hi simultaneous observation.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP57142468A JPS5932841A (en) | 1982-08-17 | 1982-08-17 | Adjusting method of sample whose multiple surfaces are simultaneously observed |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP57142468A JPS5932841A (en) | 1982-08-17 | 1982-08-17 | Adjusting method of sample whose multiple surfaces are simultaneously observed |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS5932841A true JPS5932841A (en) | 1984-02-22 |
Family
ID=15316013
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP57142468A Pending JPS5932841A (en) | 1982-08-17 | 1982-08-17 | Adjusting method of sample whose multiple surfaces are simultaneously observed |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS5932841A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012107683A1 (en) * | 2011-02-11 | 2012-08-16 | Universite De Lorraine | Method for coating a sample |
-
1982
- 1982-08-17 JP JP57142468A patent/JPS5932841A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012107683A1 (en) * | 2011-02-11 | 2012-08-16 | Universite De Lorraine | Method for coating a sample |
FR2971586A1 (en) * | 2011-02-11 | 2012-08-17 | Centre Nat Rech Scient | METHOD FOR COATING A SAMPLE |
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