JPH01280236A - Method of taking replica of metal defect - Google Patents
Method of taking replica of metal defectInfo
- Publication number
- JPH01280236A JPH01280236A JP10769388A JP10769388A JPH01280236A JP H01280236 A JPH01280236 A JP H01280236A JP 10769388 A JP10769388 A JP 10769388A JP 10769388 A JP10769388 A JP 10769388A JP H01280236 A JPH01280236 A JP H01280236A
- Authority
- JP
- Japan
- Prior art keywords
- transfer agent
- agent
- transfer
- coated
- inspected
- 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
- 230000007547 defect Effects 0.000 title claims abstract description 24
- 239000002184 metal Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 47
- 239000003822 epoxy resin Substances 0.000 claims abstract description 8
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000005498 polishing Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 abstract description 13
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 150000001247 metal acetylides Chemical class 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 2
- 238000000576 coating method Methods 0.000 abstract 2
- 238000005530 etching Methods 0.000 abstract 2
- 238000012360 testing method Methods 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000007689 inspection Methods 0.000 description 3
- 239000006082 mold release agent Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- SMEGJBVQLJJKKX-HOTMZDKISA-N [(2R,3S,4S,5R,6R)-5-acetyloxy-3,4,6-trihydroxyoxan-2-yl]methyl acetate Chemical compound CC(=O)OC[C@@H]1[C@H]([C@@H]([C@H]([C@@H](O1)O)OC(=O)C)O)O SMEGJBVQLJJKKX-HOTMZDKISA-N 0.000 description 1
- 229940081735 acetylcellulose Drugs 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000113 methacrylic resin Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000013518 transcription Methods 0.000 description 1
- 230000035897 transcription Effects 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【発明の詳細な説明】
〔発明の目的〕
（産業上の利用分野）
この発明は、例えばタービンや配管等の孔内周面の金属
欠陥を転写剤に転写させる金属欠陥レプリカ採取方法に
関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial Application Field) The present invention relates to a metal defect replica collection method for transferring metal defects on the inner circumferential surface of a hole, such as a turbine or a pipe, to a transfer agent.
（従来の技術）
例えば、蒸気タービンやガスタービン等大形原動機には
材質検査のために検査孔が回転体の中心部に穿設されて
おり、この検査孔を利用して例えば磁粉探傷検査、浸透
探傷検査、超音波探傷検査等の非破壊検査を状況に応じ
て使いわけ、目視検査とともに行なわれている。(Prior art) For example, in large-scale prime movers such as steam turbines and gas turbines, an inspection hole is drilled in the center of the rotating body for material inspection. Non-destructive tests such as penetrant testing and ultrasonic testing are used depending on the situation and are carried out along with visual inspections.
ところで、蒸気タービンロータの中心孔等では高温長時
間使用中に炭化物の粗大化やクリープ損傷によるヴオイ
ドの発生があり、材料劣化の要因になっている。Incidentally, in the center hole of a steam turbine rotor, etc., during long-term use at high temperatures, voids are generated due to coarsening of carbides and creep damage, which causes material deterioration.
このため、最近では高度な品質管理が要求されており、
大形回転体については上述慣用的検査方法に加えて１回
転体のすみずみまで金属欠陥を検鏡し、材料の長時間使
用後の経年劣化の傾向を容易にして正確に把握する手法
が採られている。For this reason, advanced quality control has recently been required.
For large rotating bodies, in addition to the conventional inspection methods mentioned above, a method is adopted in which metal defects are inspected in every corner of the rotating body to easily and accurately grasp the tendency of aging of materials after long-term use. It is being
その一つに、被検体の一部をじかに剥ぎ取り。One of them is to directly strip away a part of the subject.
そのテストピースを電子顕微鏡を用いて金属欠陥を検鏡
して材料の経年劣化を予測する手法がある。There is a method to predict the aging of the material by examining the test piece for metal defects using an electron microscope.
しかし、この手法は、廃材を用いて検鏡するならともか
く、実機適用の材料をじかに剥ぎ取り、それをテストピ
ースに使用すれば正確な金属欠陥を検鏡する点で最も好
ましいものの、実機の強、度低下をまねき、ひいては実
機の損壊につながる点で好ましくない。However, although this method is most preferable in that it allows you to inspect metal defects directly by directly stripping off the material used in the actual machine and using it as a test piece, it does not require the strength of the actual machine. , which is undesirable because it leads to a decrease in performance, which in turn leads to damage to the actual machine.
（発明が解決しようとする課題）
最近になって、実機適用の材料をテストピースとして剥
ぎ取らず、実機適用材のまま金属欠陥を検鏡する手法と
してレプリカ方式がこの種分野で採用されている。(Problem to be solved by the invention) Recently, the replica method has been adopted in this type of field as a method for inspecting metal defects using the actual material without peeling it off as a test piece. .
レプリカ方式は、被゛検体の表面に有機剤を塗布し、そ
の塗布膜に金属欠陥を転写させ、転写後、電子顕微鏡で
検鏡するものである。レプリカ方式には一段法と二段法
とがあり、それぞれの用途に使いわけられているものの
、一長一短がある。すなわち、前者は、第３図にも見ら
れるように、被検体２の表面を腐食液で腐食させておき
、この腐食面に、例えばアセチルセルロースとフィルム
（転写紙）との転写剤４を塗布し、その被膜である転写
剤４を手作業等機械的に剥し、その転写面に電気伝導性
の高い金属、例えばＡｕを用いて蒸着層５にするもので
ある。こうして形成された転写剤を走査形電子顕微鏡で
金属入感を検鏡する。In the replica method, an organic agent is applied to the surface of the specimen, metal defects are transferred to the applied film, and after the transfer, the specimen is examined using an electron microscope. There are two types of replica methods: a one-stage method and a two-stage method, each of which is used for different purposes, but each has its advantages and disadvantages. That is, in the former case, as shown in FIG. 3, the surface of the specimen 2 is corroded with a corrosive liquid, and a transfer agent 4 of, for example, acetyl cellulose and a film (transfer paper) is applied to this corroded surface. Then, the transfer agent 4, which is the film, is peeled off mechanically, such as manually, and a metal with high electrical conductivity, for example, Au, is used on the transfer surface to form a vapor deposited layer 5. The thus formed transfer agent is examined for metal sensitivity using a scanning electron microscope.
しかし、このようなレプリカ方法は、簡易式であるため
適用の利便性は高いものの、転写面にＡｕ等の蒸着層５
を形成する工程もあって、設備の費用点て経済的効果が
うすれ、蒸着作業に伴う作業時間的効率の点でも好まし
くないことはもとより、転写面に蒸着層を形成するため
極微な金属欠陥は正確に転写できない不具合がある。However, although such a replica method is simple and convenient to apply, it does not require a vapor deposition layer 5 of Au or the like on the transfer surface.
There is also a step of forming a vapor deposited layer on the transfer surface, which is less economical in terms of equipment costs and unfavorable in terms of work time efficiency associated with vapor deposition work.In addition, since the vapor deposited layer is formed on the transfer surface, minute metal defects are eliminated. There is a problem that the image cannot be transferred accurately.
他方、後者は、第４図にも見られるように、エツチング
した被検体２の表面に、例えば半液状のプラスチック等
の転写剤６を塗布被膜させ、そのまま乾燥凝固させた後
、手作業等機械的に剥し、その転写面のうち一部（図で
は転写突部の斜面）にＡｕ等を用いた蒸着層７を形成す
るためのシャドウィングを行う、こうして形成された転
写剤６の蒸着層７の表面にカーボン等を用いて蒸着する
モールディング層８を形成し、そのモールディング層８
を溶解剥離後、透過電子顕微鏡で金属欠陥を検鏡する。On the other hand, as shown in FIG. 4, in the latter case, a transfer agent 6 such as semi-liquid plastic is coated on the surface of the etched object 2, dried and solidified, and then manually or mechanically applied. The vapor deposited layer 7 of the transfer agent 6 formed in this way is removed to form a vapor deposited layer 7 using Au or the like on a part of the transfer surface (in the figure, the slope of the transfer protrusion). A molding layer 8 is formed by vapor-depositing carbon or the like on the surface of the molding layer 8.
After dissolving and peeling off, examine the metal defects using a transmission electron microscope.
しかし、この手法では、転写剤の電気導電性が高いので
透過電子顕微鏡によく適合できる反面。However, this method is well suited for transmission electron microscopy due to the high electrical conductivity of the transfer agent.
転写剤を作製する上であまりにも作業工程を多く要する
不都合があるに
の発明は、転写剤を作製する上で多くの作業工程を必要
とし、くわえて従来の転写剤では極微の金属欠陥を転写
できない等の不具合・不都合に鑑み、その作製工程の少
ない、しかも電気導電性の高い転写剤を用いた金属欠陥
レプリカ採取方法を提供することを目的″とする。The invention has the disadvantage of requiring too many work steps to create a transfer agent.In addition, the invention requires too many work steps to create a transfer agent, and in addition, conventional transfer agents cannot transfer minute metal defects. In view of the problems and inconveniences such as not being able to do so, the object of the present invention is to provide a method for collecting metal defect replicas that requires fewer manufacturing steps and uses a transfer agent with high electrical conductivity.
（課題を解決するための手段）
上記目的に沿って、この発明では、研摩後、腐食液で腐
食させた被検体の表面に離型剤を塗布し、しかる後、０
５０〜７０重量％、エポキシ樹脂５０〜３０重量％から
なるレプリカ剤を塗布する構成にする。(Means for Solving the Problems) In accordance with the above object, in the present invention, after polishing, a mold release agent is applied to the surface of the specimen corroded with a corrosive solution, and then
The structure is such that a replica agent consisting of 50 to 70% by weight and 50 to 30% by weight of epoxy resin is applied.
（作用）
上記構成では、被検体の表面を腐食させると、被検体に
形成されているクリープ損傷によるヴオイド、炭化物の
析出、極微な欠陥きずが明瞭にあられれる。こうした表
面処理工程を行った被検体上に離型剤を塗布しておけば
転写剤を塗布しても容易に剥れる。転写剤は、カーボン
およびエポキシ樹脂からなる混融剤であるが、この混融
剤にはカーボン５０〜７０重量％も含まれているので、
電気導電性は比較的高まる。(Function) In the above configuration, when the surface of the test object is corroded, the precipitation of voids and carbides due to creep damage and minute defects formed on the test object are clearly seen. If a mold release agent is applied on the specimen that has been subjected to such a surface treatment step, even if a transfer agent is applied, it will be easily peeled off. The transfer agent is a blending agent made of carbon and epoxy resin, and since this blending agent contains 50 to 70% by weight of carbon,
Electrical conductivity is relatively increased.
このように転写剤を用いて被検体の金属欠陥を転写させ
、その転写剤を電子顕微鏡で検鏡すれば。In this way, if you use a transfer agent to transfer metal defects on the object, and then examine the transfer agent using an electron microscope.
転写剤からＸ線１反射電子、二次電子線が検鏡に好まし
く出るので金属欠陥は明瞭に検鏡できる。Since X-rays, reflected electrons, and secondary electron beams are preferably emitted from the transfer agent to the microscope, metal defects can be clearly observed under the microscope.
したがって、従来の転写剤の作製上、その作業工程の短
縮と相まって被検体の金属欠陥が正確にして確実に検鏡
できる。Therefore, in addition to shortening the process for producing conventional transfer agents, metal defects in the specimen can be accurately and reliably examined using a microscope.
（実施例）
この発明にかかる金属欠陥レプリカ採取方法につき、図
を参照しながら実施例を説明する。(Example) An example of the metal defect replica collecting method according to the present invention will be described with reference to the drawings.
転写剤は、下表にも示されるように、Ｃ５０〜７０重量
％、エポキシ樹脂５０〜３０重量％からなる混融物であ
る。As shown in the table below, the transfer agent is a mixed melt consisting of 50 to 70% by weight of C and 50 to 30% by weight of epoxy resin.
表
このような組成にすれば、混融物にカーボンの手助を受
けて立体的な網状組織ができるので導電性が高くなる。With such a composition, a three-dimensional network structure is formed in the mixed melt with the help of carbon, resulting in high conductivity.
また、混融物中のエポキシ樹脂は。Also, the epoxy resin in the mixture.
転写効果を高めるに寄与する。Contributes to enhancing the transcription effect.
上記構成の転写剤を用いて被検体から金属欠陥を転写す
るには次の工程を採る。The following steps are taken to transfer metal defects from the object using the transfer agent having the above structure.
第２図は、その作業手順を示すもので、先ず、例えばＣ
ｒ−Ｍｏ−Ｖ製のタービンケーシング材等である被検体
２の表面を、パフ研摩した後、洗浄し。Figure 2 shows the work procedure. First, for example, C
The surface of the test object 2, which is a turbine casing material made of r-Mo-V, is powder-polished and then washed.
乾燥させ、つづいてナイタール等の腐食液で腐食させる
。こうすると、被検体２のクリープ損傷によるジオイド
１１．炭化物１２の析出、極微なきず１３が明瞭にあら
れれる。Dry and then corrode with a corrosive solution such as nital. In this way, the geoid 11. due to creep damage to the object 2. Precipitation of carbide 12 and minute flaws 13 are clearly visible.
次に、被検体２の表面にシリコン系の離型剤３を塗布し
、しかる後上記組成の転写剤１を塗布被膜する。転写剤
１は被検体２の表面に離型剤３が塗布されているので容
易に剥れる。Next, a silicone-based mold release agent 3 is applied to the surface of the object 2, and then a transfer agent 1 having the above composition is coated. The transfer agent 1 can be easily peeled off because the release agent 3 is applied to the surface of the subject 2.
最後に、被検体２から転写した転写剤１は、電子顕微鏡
で金属欠陥が検鏡され、こうして検鏡後の結果から材料
の劣化度合を予測し、その寿命を推定する。Finally, the transfer agent 1 transferred from the subject 2 is examined for metal defects using an electron microscope, and the degree of deterioration of the material is predicted from the results after the examination, and its lifespan is estimated.
ところで、転写剤は、上記組成のものを用いて金属欠陥
を転写することで、この発明では説明しであるが、この
実施例に限らず、例えば銀、銅、フロム等やウィスカ等
で混融物中に立体的網状組織を形成することもできる。By the way, the transfer agent is described in this invention by transferring metal defects using the composition described above, but is not limited to this embodiment. It is also possible to form a three-dimensional network within the object.
また、合成樹脂としては、メタクリル樹脂などの熱可塑
性樹脂および共重合体、熱硬化型エポキシ樹脂でもよい
。Furthermore, the synthetic resin may be a thermoplastic resin such as methacrylic resin, a copolymer, or a thermosetting epoxy resin.
このようにすれば、立体的網状組織に基づく高い導電性
と１合成樹脂が有する固有特性とが相マツチしてすぐれ
た転写剤が作製される。In this way, an excellent transfer agent can be produced in which the high conductivity based on the three-dimensional network structure and the unique properties of one synthetic resin are compatible.
以上の説明の通り、この発明は転写剤としてカーボン５
０〜７０重量％、エポキシ樹脂５０〜３０重量％の組成
し、この転写剤を用いて被検体の金属欠陥を転写し、検
鏡するもので、従来の転写剤作製工程が一段と節約され
、しかも、転写率も高く、転写像も明瞭になる等の効果
がある。As explained above, this invention uses carbon 5 as a transfer agent.
This transfer agent has a composition of 0 to 70% by weight and 50 to 30% by weight of epoxy resin, and this transfer agent is used to transfer metal defects on the specimen and examine it with a microscope.The conventional transfer agent preparation process is further reduced, and , the transfer rate is high and the transferred image becomes clear.
第１図はこの発明のレプリカ採取工程を示す作業手順図
、第２図および第３図は従来のレプリカ採取工程を示す
作業手順図である。
１．４．６・・・転写剤 ２・・・被検体３・・・離
型剤 ５，７・・・蒸着層８・・・モールデ
ィング層
代理人 弁理士 則 近 憲 佑
同 第子丸 健
第１図
第２図 第３図FIG. 1 is a work procedure diagram showing a replica collection process of the present invention, and FIGS. 2 and 3 are work procedure diagrams showing a conventional replica collection process. 1.4.6...Transfer agent 2...Test 3...Release agent 5,7...Vapor deposited layer 8...Molding layer agent Patent attorney Noriyoshi Chika Yudo Ken Daishimaru Figure 1 Figure 2 Figure 3
Claims (1)
塗布し、しかる後、Ｃ５０〜７０重量％、エポキシ樹脂
５０〜３０重量％からなる転写剤を塗布することを特徴
とする金属欠陥レプリカ採取方法。After polishing, a release agent is applied to the surface of the specimen corroded with a corrosive liquid, and then a transfer agent consisting of 50 to 70% by weight of C and 50 to 30% by weight of epoxy resin is applied. Method for collecting metal defect replicas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10769388A JPH01280236A (en) | 1988-05-02 | 1988-05-02 | Method of taking replica of metal defect |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10769388A JPH01280236A (en) | 1988-05-02 | 1988-05-02 | Method of taking replica of metal defect |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01280236A true JPH01280236A (en) | 1989-11-10 |
Family
ID=14465562
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10769388A Pending JPH01280236A (en) | 1988-05-02 | 1988-05-02 | Method of taking replica of metal defect |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01280236A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103439156A (en) * | 2013-07-30 | 2013-12-11 | 国家电网公司 | Preparation method of laminating film for on-site metallographic examination of tower material |
-
1988
- 1988-05-02 JP JP10769388A patent/JPH01280236A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103439156A (en) * | 2013-07-30 | 2013-12-11 | 国家电网公司 | Preparation method of laminating film for on-site metallographic examination of tower material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107727663A (en) | It is a kind of that the method for carrying out failure detection is characterized to LED chip | |
| US10753884B2 (en) | Nondestructive inspection of composite materials | |
| CN112525735A (en) | Replica method for detecting fatigue small crack condition | |
| JP3631652B2 (en) | Non-destructive inspection method using X-ray | |
| JPH01280236A (en) | Method of taking replica of metal defect | |
| JP2001116746A (en) | Method for assessment of quality of coating treatment and assembly for it | |
| Rokhlin et al. | Quantitative ultrasonic characterization of environmental degradation of adhesive bonds | |
| JPH08159745A (en) | Nondestructive property judgement of surface state of part | |
| CN110702497B (en) | Method for predicting crack initiation position or propagation direction of metal surface | |
| JPS60140729A (en) | Method of detecting defect of semiconductor element film | |
| CN115078086A (en) | Method for measuring bonding force between metal matrix and oxide film by using SEM (scanning electron microscope) in-situ tensile instrument | |
| US5317901A (en) | Nondestructive test for coated carbon-carbon composite articles | |
| Watts et al. | The failure mode of adhesively bonded aluminium following aqueous exposure | |
| JPH0313861A (en) | Method for detecting damage in metal | |
| JPH0381638A (en) | Method for obtaining replica of metallic structure | |
| Luo et al. | Application of ultrasonic testing technology to fretting wear detection of electrical connectors | |
| JPH08160008A (en) | Non-destructive inspecting method for defect | |
| JPS63238448A (en) | Pellicle evaluating apparatus | |
| JPS6266138A (en) | Preparation of replica | |
| Harris | Damage Evaluation by Laminate Deply | |
| JPH09178044A (en) | Method for evaluating piping performance and analyzer | |
| WO2023188535A1 (en) | Piping life prediction method | |
| Madani et al. | Evaluation of polyimide coatings integrity by positron annihilation lifetime spectroscopy and electrochemical impedance spectroscopy | |
| JP2006294904A (en) | Method for evaluating delamination characteristics | |
| GB2027544A (en) | Testing brazed metal joints |