CN104502166A - Method of preparing sample wafer capable of representing grain sliding of steel and iron materials - Google Patents
Method of preparing sample wafer capable of representing grain sliding of steel and iron materials Download PDFInfo
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- CN104502166A CN104502166A CN201410779391.1A CN201410779391A CN104502166A CN 104502166 A CN104502166 A CN 104502166A CN 201410779391 A CN201410779391 A CN 201410779391A CN 104502166 A CN104502166 A CN 104502166A
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Abstract
The invention discloses a method of preparing sample wafer capable of representing the grain sliding of steel and iron materials, and belongs to the technical field of corrosion of steel and iron materials. The process steps and control technical parameters are as follows: carrying out solution annealing on metal materials in a heating furnace at a temperature of 1050 DEG C for 30min, and cooling by means of water cooling; carrying out cold-machining material cold deformation by using a micro-type rolling mill in a machining workshop under the conditions of a pass number of 5, a thickness reduction of 20% every time, a room temperature and a unidirection; sensitizing at a temperature of 650 DEG C for 24h, and cooling with the furnace; and carrying out scratch treatment, namely preparing scratch lines slantwise penetrating through grains on the surface of a test sample, in this way, after stretching in a high-temperature furnace, representing the grain sliding by the scratch lines, so as to obtain the sample wafer enabling stress corrosion cracking to be observed under SEM. The method has the advantage of qualitatively obtaining the inhibition effect of two-phase grains on the prevention of the stress corrosion cracking.
Description
Technical field
The invention belongs to ferrous materials corrosion technology field, in particular, provide a kind of being used for and prepare the method that can characterize the print of ferrous materials grain sliding.
Background technology
Stress corrosion crack is a kind of common metal material failure mode, and this inefficacy is common in automobile tail gas pipe, in the metal material under the rugged surroundings such as Oil/Gas Pipe and High Temperature High Pressure.In use, owing to being subject to rugged surroundings and heavily stressed collaborative impact, easily there is transcrystalline at grain boundaries place and prolong brilliant fracture, thus greatly reduce the time limit of material military service in metal material, and can cause the generation of accident due to catastrophic failure.
In order to suppress the generation of this accident from material angle, form Secondary phase particle by special thermal treatment at iron and steel grain boundaries, but be difficult to prove Secondary phase particle on earth to the inhibiting effect of material stress corrosion cracking.So find a kind of method to prepare the print that can characterize ferrous materials grain sliding thus prove that Secondary phase particle is necessary to the inhibiting effect of material stress corrosion cracking on earth.And this method is simple to operate, economical and practical.
Summary of the invention
The object of the invention is to provide a kind of being used for prepare the method that can characterize the print of ferrous materials grain sliding, effectively can prepare and can be used for observing the inhibiting print of metal material sediment counter stress corrosion cracking.
Then by groping to find, a series of process being carried out to drawing by high temperature sample, making the inhibiting effect being easy to observe Secondary phase particle counter stress corrosion cracking at optics and SEM microscope norma basilaris.
The present invention includes: print thermal treatment, preparation score line.Wherein thermal treatment comprises solution annealing, cold working sensitized treatment.The technical parameter of concrete technology step and control is as follows:
(1) metal material is carried out solution annealing in heating furnace.Parameter: temperature 1050 DEG C, time 30min, the type of cooling is water-cooled.
(2) then using job shop micro-type rolling mill to carry out cold working is material cold deformation.Parameter: road number of times 5, each Reducing thickness 20%, temperature is room temperature, and direction is single direction.
(3) sensibilization.Temperature 650 DEG C, time 24h, the type of cooling cools with stove.
(4) scratching: adopt a kind of method simply and easily to prepare the score line of crystal grain athwart at specimen surface, like this after stretching at high temperature furnace, can characterize grain sliding with this cut fine rule.Characterizing grain sliding by drawing by high temperature is the main way explaining stress corrosion crack, and the groove preparing tiny crystal grain is athwart crucial.Although there is people also well can prepare cut at almag crystal grain place with FIB milling-FEI Nova 600 abroad, expend time in and money.
The invention has the advantages that there is applicability widely, the requirement of various metals material tests grain sliding can be met; and it is simply easy; namely people can operate and required item price is simple, and expense and cycle are far smaller than FIB, have very high economy and efficiency meaning.
Accompanying drawing explanation
Fig. 1 is inventive samples schematic diagram.
Fig. 2 is micrograph after print process of the present invention.
Embodiment
Further describe below in conjunction with accompanying drawing:
Object of the present invention with a kind of method being used for preparing the print that can characterize ferrous materials grain sliding is provided, can prepare simply efficiently and can be used for the print that SEM observes the impact of Secondary phase particle counter stress corrosion cracking.
For print thermal treatment and cold working:
1) solution annealing, heats 30 minutes then water-cooleds at 1050 °;
2) sensitization: be incubated 24 hours under 650 °, then air cooling.3) cold treatment, it is cold rolling to carry out one direction five passage under room temperature.
For preparing cut and etching:
Characterizing grain sliding by drawing by high temperature is the main way explaining stress corrosion crack, and the groove preparing tiny crystal grain is athwart crucial.The present invention adopts dry sanding paper to carry out manual operations preparation line.Concrete steps are as follows:
1, polish, must practical to roughly grind and that print is polished by fine grinding is very bright.Wherein roughly grind: can be mainly that print is smooth and by dirty for specimen surface removal, the highlyest use P2400 sand paper.Fine grinding: use fine grinding dish to use diamond grinding fluid 3 μm 10 minutes, 1 μm 5 minutes and 1/4 μm 1 minute.
2, preparation line, multiple sand paper can prepare line, but must adjust sand paper thickness according to grain size, and principle is that a crystal grain is rule by 4-8 bar.For example this time operation uses 600grit sand paper to be good.Angle is horizontal along print or longitudinal 45° angle.
3, etch, etching uses strong acid to make the display of the situation of metal material surface clear.Ultimate principle be grain boundaries have high density dislocation can be corroded by highly concentrated solution thus color very heavy thus under the microscope face can show out.Basic process is: use the oxalic acid of 10% and 6 voltaisms to compress into capable etching, often excessively take out observation 5 seconds and once prevent overetch.
Like this, crystal grain and the groove through it can be observed out very much clearly under an optical microscope, thus observe grain sliding through effect of stress.Due to employing is laboratory normal experiment instrument, the present invention, the expensive instruments such as practical FIB can be avoided, and can rapidly, circulation operation, simple and effectively can prepare sample, thus provide convenient and cost-effective experimental technique for a lot of researcher characterizes Grain Boundary Sliding thus stress corrosion crack is discussed further.
Claims (1)
1. be used for preparing the method that can characterize the print of ferrous materials grain sliding, it is characterized in that, the technical parameter of processing step and control is as follows:
(1) metal material is carried out solution annealing in heating furnace, temperature 1050 DEG C, time 30min, the type of cooling is water-cooled;
(2) use job shop micro-type rolling mill to carry out the cold deformation of cold working formula material, road number of times 5, each Reducing thickness 20%, temperature is room temperature, and direction is single direction;
(3) sensitization: temperature 650 DEG C, time 24h, the type of cooling cools with stove;
(4) scratching: the score line preparing crystal grain athwart at specimen surface, like this after stretching at high temperature furnace, characterizes grain sliding with this cut fine rule.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410779391.1A CN104502166A (en) | 2014-12-15 | 2014-12-15 | Method of preparing sample wafer capable of representing grain sliding of steel and iron materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410779391.1A CN104502166A (en) | 2014-12-15 | 2014-12-15 | Method of preparing sample wafer capable of representing grain sliding of steel and iron materials |
Publications (1)
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| CN104502166A true CN104502166A (en) | 2015-04-08 |
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| CN201410779391.1A Pending CN104502166A (en) | 2014-12-15 | 2014-12-15 | Method of preparing sample wafer capable of representing grain sliding of steel and iron materials |
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Citations (8)
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| JP3756722B2 (en) * | 2000-04-27 | 2006-03-15 | 日鉱金属加工株式会社 | Titanium copper alloy material and heat treatment method for titanium copper alloy |
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| DE102009013631B3 (en) * | 2009-03-18 | 2010-08-19 | Burkhard Weiss | Method for the production of high-hardness, high-grade mold part from rust resistant and/or high manganese-containing austenitic or austenitic-martensitic steel, by producing a final contour raw part of high-alloyed cast steel |
| CN101871084A (en) * | 2009-04-24 | 2010-10-27 | 中国钢铁股份有限公司 | Method for manufacturing low ductility anisotropy rolling aluminum alloy sheet |
| CN101995378A (en) * | 2009-08-14 | 2011-03-30 | 中国科学院金属研究所 | Method for quantitatively measuring contribution of grain boundary sliding in superplastic deformation of superfine material |
| CN102094238A (en) * | 2010-09-28 | 2011-06-15 | 常州天合光能有限公司 | Method for reducing internal stress defect of ingot polycrystal |
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2014
- 2014-12-15 CN CN201410779391.1A patent/CN104502166A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3150969A (en) * | 1962-12-17 | 1964-09-29 | Brush Beryllium Co | Beryllium-bronze alloy |
| JP3756722B2 (en) * | 2000-04-27 | 2006-03-15 | 日鉱金属加工株式会社 | Titanium copper alloy material and heat treatment method for titanium copper alloy |
| CN101012519A (en) * | 2000-08-09 | 2007-08-08 | 奥林公司 | Silver containing copper alloy |
| EP1479786A1 (en) * | 2003-05-20 | 2004-11-24 | Corus Aluminium N.V. | Wrought aluminium alloy |
| DE102009013631B3 (en) * | 2009-03-18 | 2010-08-19 | Burkhard Weiss | Method for the production of high-hardness, high-grade mold part from rust resistant and/or high manganese-containing austenitic or austenitic-martensitic steel, by producing a final contour raw part of high-alloyed cast steel |
| CN101871084A (en) * | 2009-04-24 | 2010-10-27 | 中国钢铁股份有限公司 | Method for manufacturing low ductility anisotropy rolling aluminum alloy sheet |
| CN101995378A (en) * | 2009-08-14 | 2011-03-30 | 中国科学院金属研究所 | Method for quantitatively measuring contribution of grain boundary sliding in superplastic deformation of superfine material |
| CN102094238A (en) * | 2010-09-28 | 2011-06-15 | 常州天合光能有限公司 | Method for reducing internal stress defect of ingot polycrystal |
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