EP2531850A1 - Zerstörungsfreies verfahren für den nachweis von bearbeitungsbrandstellen von extrem hochfestem stahl und farbtabelle zur kalibrierung von bearbeitungsbrandstellen bei diesem stahl - Google Patents
Zerstörungsfreies verfahren für den nachweis von bearbeitungsbrandstellen von extrem hochfestem stahl und farbtabelle zur kalibrierung von bearbeitungsbrandstellen bei diesem stahlInfo
- Publication number
- EP2531850A1 EP2531850A1 EP11706887A EP11706887A EP2531850A1 EP 2531850 A1 EP2531850 A1 EP 2531850A1 EP 11706887 A EP11706887 A EP 11706887A EP 11706887 A EP11706887 A EP 11706887A EP 2531850 A1 EP2531850 A1 EP 2531850A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- steel
- machining
- burns
- solution
- acid
- 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.)
- Withdrawn
Links
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 34
- 239000010959 steel Substances 0.000 title claims abstract description 34
- 238000003754 machining Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 13
- 229910000922 High-strength low-alloy steel Inorganic materials 0.000 title 1
- 239000000243 solution Substances 0.000 claims abstract description 20
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 16
- 238000007654 immersion Methods 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 14
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 150000007513 acids Chemical class 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000001066 destructive effect Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000004071 soot Substances 0.000 claims description 5
- 238000013021 overheating Methods 0.000 claims description 4
- 230000002747 voluntary effect Effects 0.000 claims description 4
- 238000004040 coloring Methods 0.000 claims description 3
- 239000011260 aqueous acid Substances 0.000 claims description 2
- 230000032683 aging Effects 0.000 abstract description 5
- 238000007669 thermal treatment Methods 0.000 abstract description 2
- 238000000137 annealing Methods 0.000 abstract 1
- 229910045601 alloy Inorganic materials 0.000 description 9
- 239000000956 alloy Substances 0.000 description 9
- 230000007423 decrease Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/204—Structure thereof, e.g. crystal structure
- G01N33/2045—Defects
Definitions
- the invention relates to a method for non-destructive detection of machining burns on stainless steels with very high resistance (abbreviated THR) to corrosion, resulting for example from the final grinding, in particular for the production of landing gear trains. aircraft.
- the steels in particular are alloys based on Cr, Ni, Mo, Al, Ti, for example the steels known under the trade names AMS 5936, MLT 1302, Ma-0650-12 and Ma0600-12.
- the invention also relates to a calibration chart for mill burns of THR steels detected with the method above.
- the present invention relates to the field of quality control of stainless steels after heat treatment and finishing machining or grinding.
- Such control is extremely useful because, during the machining of parts, the material can reach excessive temperatures compared to nominal values and be burned. However, these machining burns generate a significant variation in the mechanical properties of the material, or even possible cracking of the parts.
- Non-destructive testing techniques for low-alloy THR steels such as inspection by etching of acidic composition, such as the alcoholic solution of nitric acid known as NITAL.
- the object of the invention is to enable the detection of machining burns of stainless steels of the THR type in an efficient and industrializable manner.
- a bath of particular acid solution based on hydrofluoric acid provides an indication visual graduated according to the state of burn steels dipped in the bath.
- the subject of the present invention relates to a method for the non-destructive detection of machining burns of stainless steels THR, in which the machined steel is immersed in an aqueous solution of acids comprising acid. hydrofluoric acid and nitric acid, and wherein a calibration scale for burns of steel machining is prepared by immersing samples subjected to deliberate damage in said aqueous acid solution. The samples are classified by their level of gray resulting from the immersion and corresponding to a determined hardness. The steel is then compared to the calibrated color chart.
- the immersion time in the acid solution is at least 5 minutes
- the proportion of all the acids is less than the proportion of water in the solution
- the solution consists, by volume, of 10 to 20%, preferably 15% of hydrofluoric acid, of 10 to 20%, preferably 15% of nitric acid, and 60% to
- the solution is free of hexavalent chromium (Cr6) which is removed by any known means, in particular by exchange of anions in grafted cellulose columns or by addition of a ferric sulphate solution; Cr6 chromium is extremely toxic and its non-proliferation is therefore important for humans and the environment;
- the steel is then immersed in a nitric acid bath for removing the soot produced by the first chemical etching, the soot being formed of residues which risk degrading the reading of the machining burns;
- the acidic solution of the process according to the invention makes it possible to obtain an elemental burn indication of a THR steel corresponding to a reduction of at least 3% in the hardness of the test steel, for an immersion lasting substantially equal to 5 minutes of this steel.
- the color chart is composed of samples subject to damage voluntary, for example by variable abusive rectifications.
- the samples consist of specimen zones subjected to variable rectification of a THR steel to be tested or by pads of this steel subjected to variable overheating heat treatments.
- the same level of gray corresponds to the same level of damage suffered regardless of the type of corrections, real or simulated.
- the samples are sandblasted beforehand in order to homogenize their surface state in order to obtain a better contrast of the coloring after immersion in the acid bath;
- the soot formed is removed by immersion in a nitric acid bath before final rinsing with water.
- the invention also relates to a calibration chart of burns of machining THR steels detected with the method above.
- FIGS. 2a and 2b superior views of the pads of two stainless steels THR having undergone superheating temperatures, corresponding to differentiated simulated rectifications, using different aging temperatures ranging from the standard aging temperature to the solution temperature;
- FIG. 3 a top view of a specimen of a zone-cut THR steel which has undergone voluntary rectifications resulting in differentiated damages
- AMS 5936 Customer 465) and MLT 1302 (MLX17), hereinafter referred to as A1 and A2
- sample pads of each of these steels - respectively P1 to P10 and P1 1 to P18 - are prepared.
- the pads are machined from bars of alloys A1 and A2. These pads have a cylindrical shape, of diameter equal to 15 mm and height equal to 9 mm in the embodiment.
- the pads are first heat treated to overheat at different temperatures, to create faults simulating damage or burn resulting from excessive rectifications.
- the pads are successively introduced into a laboratory furnace at different overheating temperatures.
- the method according to the invention then consists of immersing the pads in a bath containing two strong mineral acids: hydrofluoric acid and nitric acid, in equal proportions in the preferred example.
- the solution comprises 15 ml of each acid and 70 ml of water.
- FIGS. 2a and 2b show the upper face respectively of studs P1 to P10 of alloy A1 and studs P1 1 to P18 of alloy A2 after immersion.
- the pads have different shades according to a contrast gradient of gray level.
- the upper faces have frames whose density of lines reflects the different levels of gray. The figure recalls the corresponding processing temperatures of the pads, ranging respectively from 510 to 950 and from 505 to 850 ° C.
- a top view of a steel specimen A1 is cut into zones Zi having undergone voluntary rectifications of increasing intensity, causing damage also increasing. Hardness measurements HB are made for each zone Zi and the values obtained have been shown in the figure.
- the test piece is then immersed in an acid bath of the same composition as that previously used for simulated rectification pads. Additional immersion stripping and post immersion cleaning treatments are also performed.
- the zones Zi and the plots Pi of the same level of gray bear the same index "i".
- the pads Pi and the zones Zi are classified as abscissa according to their gray level "i”, and the hardness HB of these zones and pads is plotted on the ordinate.
- the correlation of the hardness values of the zones and the plots bearing the same number "i" that is to say having undergone equivalent mechanical (real rectifications) and thermal treatments (simulated rectifications), is corroborated by this graph. A decrease of about 3% in HB hardness is observed between two successive "i" values. The gray level "i” therefore measures a precise degree of damage.
- the invention is not limited to the examples described or represented. It is for example possible to add another acid in the solution, for example hydrochloric acid, in particular in a proportion equivalent to that of other acids.
- the immersion time in the hydrofluoric / nitric acid bath can be extended beyond 5 minutes depending on the steels and the degree of burns, without however exceeding 60 minutes or equivalent for reasons of efficiency.
- Machining modes other than grinding can be used such as for example turning or milling.
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- ing And Chemical Polishing (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR1050670A FR2955937B1 (fr) | 2010-02-01 | 2010-02-01 | Procede de detection non destructif de brulures d'usinage d'un acier a tres haute resistance, procede et nuancier d'etalonnage de brulures d'usinage de cet acier |
| PCT/FR2011/050180 WO2011092438A1 (fr) | 2010-02-01 | 2011-01-28 | Procede de detection non destructif de brulures d'usinage d'un acier a tres haute resistance, et nuancier d'étalonnage de brulures d'usinage de cet acier |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP2531850A1 true EP2531850A1 (de) | 2012-12-12 |
Family
ID=42711799
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP11706887A Withdrawn EP2531850A1 (de) | 2010-02-01 | 2011-01-28 | Zerstörungsfreies verfahren für den nachweis von bearbeitungsbrandstellen von extrem hochfestem stahl und farbtabelle zur kalibrierung von bearbeitungsbrandstellen bei diesem stahl |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US20120288946A1 (de) |
| EP (1) | EP2531850A1 (de) |
| CN (1) | CN102822668A (de) |
| BR (1) | BR112012018009A2 (de) |
| CA (1) | CA2786421A1 (de) |
| FR (1) | FR2955937B1 (de) |
| RU (1) | RU2012137211A (de) |
| WO (1) | WO2011092438A1 (de) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201432261A (zh) * | 2013-02-01 | 2014-08-16 | Univ Chien Hsin Sci & Tech | 鋼筋強度非破壞分析方法及其裝置 |
| RU2698698C1 (ru) * | 2018-12-20 | 2019-08-29 | федеральное государственное бюджетное образовательное учреждение высшего образования "Нижегородский государственный технический университет им. Р.Е. Алексеева" (НГТУ) | Способ количественной оценки пережога в деформируемых термоупрочняемых алюминиевых сплавах с помощью EDS-анализа |
| CN111060670B (zh) * | 2019-12-18 | 2022-06-10 | 江苏隆达超合金股份有限公司 | 酸洗检验镍基合金荒管内表面裂纹缺陷方法 |
| CN112504978A (zh) * | 2020-11-12 | 2021-03-16 | 中国航发中传机械有限公司 | 一种用于耐酸蚀钢制件的磨削烧伤检测方法 |
| FR3129485B1 (fr) * | 2021-11-19 | 2024-08-16 | Commissariat Energie Atomique | Détection de brulures lors de l’usinage d’une pièce mécanique par la méthode de courants de Foucault |
| CN119915990B (zh) * | 2024-12-27 | 2025-10-21 | 昌河飞机工业(集团)有限责任公司 | 金属表面烧伤检测方法及装置 |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5545283B2 (de) * | 1973-06-26 | 1980-11-17 | ||
| GB1486877A (en) * | 1974-06-20 | 1977-09-28 | Mitsubishi Heavy Ind Ltd | Method for analyzing metallic materials |
| SU726149A1 (ru) * | 1977-11-09 | 1980-04-05 | Предприятие П/Я В-8173 | Раствор дл травлени нержавеющей стали и сплавов |
| US4592854A (en) * | 1985-01-09 | 1986-06-03 | Mcdonnell Douglas Corporation | Steel etchant |
| CN1011915B (zh) * | 1986-07-29 | 1991-03-06 | 上海第五钢铁厂 | 一种显示铬轴承钢高倍组织的腐蚀剂 |
| RU2017244C1 (ru) * | 1991-06-10 | 1994-07-30 | Конкин Евгений Дмитриевич | Способ дезактивации поверхностей из нержавеющей стали |
| JPH0520969A (ja) * | 1991-07-15 | 1993-01-29 | Omron Corp | 防滴形スイツチのモ−ルド組立方法 |
| JP3365385B2 (ja) * | 2000-01-31 | 2003-01-08 | 住友金属工業株式会社 | 固体高分子型燃料電池のセパレータ用ステンレス鋼材の製造方法 |
| CN1566920A (zh) * | 2003-07-04 | 2005-01-19 | 孙贤熙 | 钢材腐蚀试剂 |
| JP2008164410A (ja) * | 2006-12-28 | 2008-07-17 | Yokogawa Electric Corp | 鋼材の検査方法 |
-
2010
- 2010-02-01 FR FR1050670A patent/FR2955937B1/fr active Active
-
2011
- 2011-01-28 CN CN2011800066018A patent/CN102822668A/zh active Pending
- 2011-01-28 RU RU2012137211/15A patent/RU2012137211A/ru not_active Application Discontinuation
- 2011-01-28 CA CA2786421A patent/CA2786421A1/fr not_active Abandoned
- 2011-01-28 WO PCT/FR2011/050180 patent/WO2011092438A1/fr not_active Ceased
- 2011-01-28 EP EP11706887A patent/EP2531850A1/de not_active Withdrawn
- 2011-01-28 US US13/574,689 patent/US20120288946A1/en not_active Abandoned
- 2011-01-28 BR BR112012018009A patent/BR112012018009A2/pt not_active IP Right Cessation
Non-Patent Citations (1)
| Title |
|---|
| See references of WO2011092438A1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| US20120288946A1 (en) | 2012-11-15 |
| FR2955937B1 (fr) | 2013-02-08 |
| CA2786421A1 (fr) | 2011-08-04 |
| FR2955937A1 (fr) | 2011-08-05 |
| CN102822668A (zh) | 2012-12-12 |
| RU2012137211A (ru) | 2014-03-10 |
| BR112012018009A2 (pt) | 2017-06-20 |
| WO2011092438A1 (fr) | 2011-08-04 |
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| RIN1 | Information on inventor provided before grant (corrected) |
Inventor name: HUET, LAURENT Inventor name: MENESES, OLIVIER Inventor name: ABERNE, FABRICE |
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| DAX | Request for extension of the european patent (deleted) | ||
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