CN106757301A - A kind of method that intergranular fracture is obtained in austenitic steel and its application - Google Patents
A kind of method that intergranular fracture is obtained in austenitic steel and its application Download PDFInfo
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- CN106757301A CN106757301A CN201611247831.4A CN201611247831A CN106757301A CN 106757301 A CN106757301 A CN 106757301A CN 201611247831 A CN201611247831 A CN 201611247831A CN 106757301 A CN106757301 A CN 106757301A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25F3/00—Electrolytic etching or polishing
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- 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
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Abstract
The invention provides a kind of method that intergranular fracture is obtained in austenitic steel and its application.The present invention carries out electrobrightening in austenitic steel specimen surface, carries out cathodic hydrogen charging to austenitic steel sample afterwards；Then the two ends of clamping austenitic steel sample load surface analysis apparatus for a period of time, then by austenitic steel sample；Under vacuum conditions, after the default incision position of austenitic steel sample carries out multiple first pressing, the default incision position of austenitic steel sample is disposably broken, obtains intergranular fracture.The inventive method process is simple, time-consuming short, operating procedure it is simple it is controllable, be easily achieved；The austenitic steel fracture that the present invention is obtained is typical intergranular fracture, can be prevented effectively from pollution, can provide objective and accurate evidence to crystal ingedient analysis, it is adaptable to which austenitic steel crystal ingedient is analyzed.
Description
Technical field
The present invention relates to ferrous materials analysis technical field, obtained along crystalline substance in austenitic steel in particular to one kind
The method of fracture and its application.
Background technology
Austenitic steel crystal ingedient analysis and research in, especially to the research of Grain Boundary Segregation behavior in, to crystal boundary microcell
What composition was accurately analyzed it is critical only that the acquisition of cleaning intergranular fracture；But in the prior art, for austenitic steel, intergranular fracture
Generation be often only present in it is specific under the conditions of, prior art is difficult to obtain intergranular fracture；Additionally, being prepared using prior art
Intergranular fracture complex process, easily austenitic steel sample contamination is caused in technical process, so as to influence austenitic steel crystal ingedient point
Analyse the accuracy of result, it is difficult to draw accurate, real Grain Boundary Segregation behavioural analysis conclusion.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of method that intergranular fracture is obtained in austenitic steel, the method technique
Simply, take short, operating procedure it is simple it is controllable, be easily achieved, the austenitic steel fracture for being obtained is typical intergranular fracture, energy
Pollution is enough prevented effectively from, objective and accurate evidence can be provided to crystal ingedient analysis.
The second object of the present invention is to provide a kind of answering for above-mentioned method that intergranular fracture is obtained in austenitic steel
With the method is used to analyze austenitic steel crystal ingedient, the austenitic steel intergranular fracture of cleaning is obtained in that, to crystal ingedient
Analysis provides objective and accurate evidence.
In order to realize above-mentioned purpose of the invention, spy uses following technical scheme：
A kind of method that intergranular fracture is obtained in austenitic steel, being included in austenitic steel specimen surface carries out electrolysis throwing
Light, carries out cathodic hydrogen charging to austenitic steel sample afterwards；Then the two ends of clamping austenitic steel sample for a period of time, then by Ovshinsky
Body steel curved beam loads surface analysis apparatus；Under vacuum conditions, the default incision position in austenitic steel sample carries out multiple first pressing
Afterwards, the default incision position of austenitic steel sample is disposably broken, obtains intergranular fracture.
The present invention obtained in austenitic steel the method process is simple of intergranular fracture, time-consuming short, operating procedure it is simple it is controllable,
It is easily achieved；The method that the present invention obtains intergranular fracture in austenitic steel uses special process, and the austenitic steel for being obtained breaks
Mouth is typical intergranular fracture, can be prevented effectively from pollution, can provide objective and accurate evidence to crystal ingedient analysis.
Preferably, electrobrightening is carried out to austenitic steel specimen surface using electrolytic polishing liquid.
It is further preferred that the electrolytic polishing liquid includes the mixed solution of acid and alcohol.
It is highly preferred that the mass ratio of the acid and alcohol is 10-20:80-90, preferably 15-20：80-85, further preferably
It is 15:85.
It is highly preferred that the acid includes one or more in inorganic acid and organic acid, sulfuric acid, phosphoric acid, lemon are preferably included
One kind in lemon acid, hydrofluoric acid, further preferably including sulfuric acid.
It is highly preferred that the alcohol includes one or more in monohydric alcohol, dihydroxylic alcohols and polyalcohol, C1-C3 is preferably included
One or more in alcohol, further preferably including methyl alcohol.
Preferably, the voltage of the electrobrightening is 10-20V, more preferably preferably 15-20V, 15V.
Preferably, the time of the electrobrightening is 5-15s, more preferably preferably 10-15s, 15s.
Preferably, the current density that is flushed with hydrogen of the cathodic hydrogen charging is 300-800mA/cm2, preferably 500-800mA/cm2,
More preferably 500-700mA/cm2。
Preferably, the time that is flushed with hydrogen of the cathodic hydrogen charging is 12-24h, more preferably preferably 18-24h, 18-
20h。
Preferably, it is described clamping austenitic steel sample two ends the clamping time be 2-5h, preferably 3-5h, further it is excellent
Elect 4.5-5h as.
Preferably, the first pressing is to be pressed into 0.5-2mm, preferably 0.8-2mm every time in default incision position, further preferably
It is 0.8-1.5mm.
Preferably, during the multiple first pressing, 2-12min is spaced between adjacent 2 first pressing, preferably by 9-12min,
Further preferably interval 9-10min；
Preferably, the number of times of the first pressing is 2-5 times, preferably 3-5 times, more preferably 3-4 times.
Preferably, the austenitic steel sample is the standard specimen that can be used in surface analysis apparatus detection.
Preferably, the surface analysis apparatus include Auger electron spectrometer.
Preferably, before every step process is carried out, cleaning operation is carried out to austenitic steel sample respectively；
It is further preferred that the cleaning operation includes cleaning austenitic steel sample using washing lotion；
It is highly preferred that the cleaning operation includes being totally submerged austenitic steel sample in washing lotion, cleaned；
It is highly preferred that the cleaning operation includes being cleaned by ultrasonic austenitic steel sample using washing lotion；
It is highly preferred that the washing lotion includes the mixed liquor of ethanol and acetone；
Most preferably, the volume ratio of ethanol and acetone is 1 in the washing lotion:0.5-2, preferably 1:0.5-1, it is further excellent
Elect 1 as:1；
It is further preferred that to carrying out cleaning operation to austenitic steel sample before the electrobrightening, scavenging period is 10-
20min, preferably 15-20min, more preferably 15-18min；
It is further preferred that to carrying out cleaning operation to austenitic steel sample before the cathodic hydrogen charging, scavenging period is 10-
20min, preferably 15-20min, more preferably 18-20min；
It is further preferred that to carrying out cleaning behaviour to austenitic steel sample before the two ends of the clamping austenitic steel sample
Make, scavenging period is 40-60min, preferably 50-60min, more preferably 50-55min.
Preferably, after the two ends of the clamping austenitic steel sample, within 5min, by Ovshinsky preferably within 3min
Body steel curved beam loads the vacuum chamber of surface analysis apparatus, vacuumizes immediately, after vacuum reaches requirement, carries out subsequent technique.
The application of a kind of above-mentioned method that intergranular fracture is obtained in austenitic steel, it is described that edge is obtained in austenitic steel
The method of brilliant fracture is used to analyze austenitic steel crystal ingedient.
The method that the present invention obtains intergranular fracture in austenitic steel is used to analyze austenitic steel crystal ingedient, can obtain
The austenitic steel intergranular fracture that must be cleaned, objective and accurate evidence is provided to crystal ingedient analysis.
Compared with prior art, beneficial effects of the present invention are：
The present invention obtained in austenitic steel the method process is simple of intergranular fracture, time-consuming short, operating procedure it is simple it is controllable,
It is easily achieved；The method that the present invention obtains intergranular fracture in austenitic steel uses special process, and the austenitic steel for being obtained breaks
Mouth is typical intergranular fracture, can be prevented effectively from pollution, can provide objective and accurate evidence to crystal ingedient analysis, fits
For analyzing austenitic steel crystal ingedient.
Brief description of the drawings
In order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art, below will be to specific
The accompanying drawing to be used needed for implementation method or description of the prior art is briefly described, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is a kind of method process chart of specific embodiment of the invention；
The Auger electron spectrometer standard specimen specification schematic diagram that Fig. 2 is used by a kind of specific embodiment of the invention；
Fig. 3 is stereoscan photograph of the gained of the embodiment of the present invention 3 cleaning along brilliant section；
Fig. 4 is stereoscan photograph of the gained of the embodiment of the present invention 4 cleaning along brilliant section；
Fig. 5 is auger electrons spectral line of the gained of the embodiment of the present invention 4 cleaning along brilliant section；
Fig. 6 is the auger electrons spectral line of non-clean intergranular fracture.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with the drawings and specific embodiments, but
It is it will be understood to those of skill in the art that following described embodiment is a part of embodiment of the invention, rather than whole
Embodiment, is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.Based on the embodiment in the present invention, ability
The every other embodiment that domain those of ordinary skill is obtained under the premise of creative work is not made, belongs to guarantor of the present invention
The scope of shield.Unreceipted actual conditions person in embodiment, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same
Or the unreceipted production firm person of instrument, it is the conventional products that can be obtained by commercially available purchase.
In the description of the invention, it is necessary to explanation, term " " center ", " on ", D score, "left", "right", " vertical ",
The orientation or position relationship of the instruction such as " level ", " interior ", " outward " be based on orientation shown in the drawings or position relationship, merely to
Be easy to the description present invention and simplify describe, rather than indicate imply signified device or element must have specific orientation,
With specific azimuth configuration and operation, therefore it is not considered as limiting the invention.Additionally, term " first ", " second ",
" the 3rd " is only used for describing purpose, and it is not intended that indicating or implying relative importance.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Company ", " connection " should be interpreted broadly, for example, it may be being fixedly connected, or being detachably connected, or be integrally connected；Can
Being to mechanically connect, or electrically connect；Can be joined directly together, it is also possible to be indirectly connected to by intermediary, Ke Yishi
Two connections of element internal.For the ordinary skill in the art, with concrete condition above-mentioned term can be understood at this
Concrete meaning in invention.
The invention provides a kind of method that intergranular fracture is obtained in austenitic steel, austenitic steel specimen surface is included in
Electrobrightening is carried out, cathodic hydrogen charging is carried out to austenitic steel sample afterwards；Then during one section of the two ends of clamping austenitic steel sample
Between, then austenitic steel sample is loaded into surface analysis apparatus；Under vacuum conditions, the default incision position in austenitic steel sample enters
After the multiple first pressing of row, the default incision position of austenitic steel sample is disposably broken, obtain intergranular fracture.
The present invention obtained in austenitic steel the method process is simple of intergranular fracture, time-consuming short, operating procedure it is simple it is controllable,
It is easily achieved；The method that the present invention obtains intergranular fracture in austenitic steel uses special process, and the austenitic steel for being obtained breaks
Mouth is typical intergranular fracture, can be prevented effectively from pollution, can provide objective and accurate evidence to crystal ingedient analysis.
In a kind of preferred embodiment of the present invention, electricity is carried out to austenitic steel specimen surface using electrolytic polishing liquid
Solution polishing.
Preferably, the electrolytic polishing liquid includes the mixed solution of acid and alcohol.
It is further preferred that the mass ratio of the acid and alcohol is 10-20:80-90, preferably 15-20：80-85, further
Preferably 15:85.
It is further preferred that the acid includes one or more in inorganic acid and organic acid, sulfuric acid, phosphorus are preferably included
One kind in acid, citric acid, hydrofluoric acid, further preferably including sulfuric acid.
It is further preferred that the alcohol includes one or more in monohydric alcohol, dihydroxylic alcohols and polyalcohol, preferably include
One or more in C1-C3 alcohol, further preferably including methyl alcohol.
Electrobrightening is carried out to austenitic steel specimen surface using specific electrolytic polishing liquid, austenitic steel examination can be dissolved
The deformation layer dislocation on sample surface, hole builds up equipotential tissue, so as to obtain equipotential surface, its corrosion resisting property is carried significantly
It is high, it is to avoid corrosion contact scar is introduced during the acquisition of follow-up fracture, the accurate of austenitic steel crystal ingedient analysis result is improved
Property, make Grain Boundary Segregation behavioural analysis conclusion more accurate, truer.
In a kind of preferred embodiment of the present invention, the voltage of the electrobrightening is 10-20V, preferably 15-
20V, more preferably 15V.
In a kind of preferred embodiment of the present invention, the time of the electrobrightening is 5-15s, preferably 10-
15s, more preferably 15s.
Electrobrightening is carried out to austenitic steel specimen surface using specific electrolytic polishing process condition, Ovshinsky can be dissolved
The deformation layer dislocation on body steel curved beam surface, hole builds up equipotential tissue, so as to obtain equipotential surface, makes its corrosion resisting property big
It is big to improve, it is to avoid corrosion contact scar is introduced during the acquisition of follow-up fracture, austenitic steel crystal ingedient analysis result is improved
Accuracy, makes Grain Boundary Segregation behavioural analysis conclusion more accurate, truer.
In a kind of preferred embodiment of the present invention, the current density that is flushed with hydrogen of the cathodic hydrogen charging is 300-800mA/
cm2, preferably 500-800mA/cm2, more preferably 500-700mA/cm2。
In a kind of preferred embodiment of the present invention, the time that is flushed with hydrogen of the cathodic hydrogen charging is 12-24h, preferably
18-24h, more preferably 18-20h.
Be flushed with hydrogen process conditions using particular cathode carries out cathodic hydrogen charging to austenitic steel sample, it is possible to increase austenitic steel is tried
The fragility of sample, is easy to subsequently smoothly obtain fracture；The toughness due to austenitic steel in itself can be avoided simultaneously, cause it to be difficult to press
It is disconnected, and can not obtain accurately, truly reflecting the intergranular fracture of austenitic steel Grain Boundary Segregation behavior due to generation deformation.
In a kind of preferred embodiment of the present invention, the clamping time at the two ends of the clamping austenitic steel sample is
2-5h, preferably 3-5h, more preferably 4.5-5h.
After cathodic hydrogen charging operation terminates, the two ends special time of austenitic steel sample is clamped, help fully to improve and fill
Hydrogen effect, makes hydrogen fully agglomerate into hydrogen molecule, improves the internal stress of austenitic steel sample, its stress concentration is caused, more than it
Strength degree, further reduces the toughness of austenitic steel sample, be easy to it is follow-up obtain can accurately, truly reflect austenitic steel
The intergranular fracture of Grain Boundary Segregation behavior.
Preferably, the two ends of the austenitic steel sample are clamped using fixture.
It is further preferred that clamping the two ends in the austenitic steel specimen length direction
In a kind of preferred embodiment of the present invention, the first pressing is to be pressed into 0.5-2mm every time in default incision position,
Preferably 0.8-2mm, more preferably 0.8-1.5mm.
In a kind of preferred embodiment of the present invention, during the multiple first pressing, it is spaced between adjacent 2 first pressing
2-12min, preferably by 9-12min, is further preferably spaced 9-10min.
In a kind of preferred embodiment of the present invention, the number of times of the first pressing is 2-5 times, preferably 3-5 times, enters one
Step is preferably 3-4 times.
Austenitic steel sample is broken using the specific mode that breaks, ensure that the accuracy of gained fracture site, and
The mechanical performance of austenitic steel can be fully reduced by multiple first pressing, promotes it once to be broken, obtain accurate edge
Brilliant fracture.
In a kind of preferred embodiment of the present invention, the austenitic steel sample is that can be used in surface analysis apparatus
The standard specimen of detection.
In a kind of preferred embodiment of the present invention, the surface analysis apparatus include Auger electron spectrometer.
Auger spectroscopy analysis occupies highly important status, the standard of its analysis result in material surface constituent analysis work
The whether true objectivity and accuracy that will directly influence constituent analysis conclusion.It is micro- using Auger spectroscopy analysis technical research crystal boundary
Area's composition has turned into a kind of effective means for studying austenitic steel Grain Boundary Segregation behavior.
Preferably, the standard specimen coordinated with Auger electron spectrometer is used in various embodiments of the present invention.
Preferably, can be sampled on austenitic steel, and be processed into the standard specimen of Auger electron spectrometer.
Alternatively, various embodiments of the present invention use the Auger electron spectrometer standard specimen of specification as shown in Figure 2.
In a kind of preferred embodiment of the present invention, before every step process is carried out, respectively to austenitic steel sample
Carry out cleaning operation.
Preferably, the cleaning operation includes cleaning austenitic steel sample using washing lotion.
It is further preferred that the cleaning operation includes being totally submerged austenitic steel sample in washing lotion, cleaned.
It is further preferred that the cleaning operation includes being cleaned by ultrasonic austenitic steel sample using washing lotion.
It is further preferred that the washing lotion includes the mixed liquor of ethanol and acetone.
It is highly preferred that the volume ratio of ethanol and acetone is 1 in the washing lotion:0.5-2, preferably 1:0.5-1, it is further excellent
Elect 1 as:1.
Preferably, to carrying out cleaning operation to austenitic steel sample before the electrobrightening, scavenging period is 10-20min,
Preferably 15-20min, more preferably 15-18min.
Preferably, to carrying out cleaning operation to austenitic steel sample before the cathodic hydrogen charging, scavenging period is 10-20min,
Preferably 15-20min, more preferably 18-20min.
Preferably, cleaned to carrying out cleaning operation to austenitic steel sample before the two ends of the clamping austenitic steel sample
Time is 40-60min, preferably 50-60min, more preferably 50-55min.
Using specific cleaning, help to make the austenitic steel sample keep cleaning in a technical process is earned,
Finally give the intergranular fracture of cleaning, it is to avoid introduce various pollutants, improve the accurate of austenitic steel crystal ingedient analysis result
Property, make Grain Boundary Segregation behavioural analysis conclusion more accurate, truer.
In a kind of preferred embodiment of the present invention, austenitic steel sample samples it by austenitic steel as described
Post-processing is obtained, then before its processing, should carry out cleaning pretreatment.
Preferably, the cleaning pretreatment include austenitic steel sampling eliminated rust, decontamination, grinding process, then carry out
Cleaning operation.
Preferably, the cleaning operation includes cleaning austenitic steel sample using washing lotion.
It is further preferred that the cleaning operation includes being totally submerged austenitic steel sample in washing lotion, cleaned.
It is further preferred that the cleaning operation includes being cleaned by ultrasonic austenitic steel sample using washing lotion.
It is further preferred that the washing lotion includes the mixed liquor of ethanol and acetone.
It is highly preferred that the volume ratio of ethanol and acetone is 1 in the washing lotion:0.5-2, preferably 1:0.5-1, it is further excellent
Elect 1 as:1.
Preferably, the scavenging period is 10-20min, more preferably preferably 12-20min, 15-20min.
In a kind of preferred embodiment of the present invention, after the two ends of the clamping austenitic steel sample, in 5min
Within, austenitic steel sample is loaded the vacuum chamber of surface analysis apparatus preferably within 3min, vacuumize immediately, work as vacuum
After reaching requirement, subsequent technique is carried out.
The intergranular fracture obtained using vacuumizing, fracture surface will not be exposed in working environment, it is not easy to the external world
There is chemical reaction generation fracture attachment and corrosion product in Korrosionsmedium, so as to improve austenitic steel crystal ingedient analysis knot
The accuracy of fruit, makes Grain Boundary Segregation behavioural analysis conclusion more accurate, truer.
The application of a kind of above-mentioned method that intergranular fracture is obtained in austenitic steel, it is described that edge is obtained in austenitic steel
The method of brilliant fracture is used to analyze austenitic steel crystal ingedient.
The method that the present invention obtains intergranular fracture in austenitic steel is used to analyze austenitic steel crystal ingedient, can obtain
The austenitic steel intergranular fracture that must be cleaned, objective and accurate evidence is provided to crystal ingedient analysis.
Embodiment 1
A kind of method that intergranular fracture is obtained in austenitic steel, comprises the following steps：
(1) sampled on Ni-based GH720Li austenitic alloys, be cut into the bar samples of 4 × 32mm of Φ；
(2) step (1) described sample is eliminated rust, decontamination, grinding process, it is 1 that volume ratio is used afterwards:0.5 second
Alcohol and acetone mixture sample submerge sample and carry out ultrasonic wave and clean 10 minutes, are cleaned with deionized water and dried up；
(3) step (2) described sample is processed into Auger electron spectrometer standard specimen；
(4) it is 1 to use volume ratio:0.5 ethanol and acetone mixture sample immersion step (3) sample are simultaneously surpassed
Sound wave is cleaned 10 minutes, is cleaned with deionized water and dried up；
(5) it is 10 to use sulfuric acid and methanol quality ratio:90 sulfuric acid and methyl alcohol mixed liquor is as electrolytic polishing liquid to step
(4) specimen surface carries out electrobrightening, and sample is totally submerged in electrolytic polishing liquid, and electrobrightening voltage is 10V, time
It is 10s；
(6) it is 1 to use volume ratio:0.5 ethanol and acetone mixture sample submergence sample simultaneously carries out ultrasonic wave cleaning 10
Minute, cleaned with deionized water and dried up；
(7) cathodic hydrogen charging is carried out to step (6) described sample using electrolyte solution mode, being flushed with hydrogen current density is
300mA/cm2, the time is flushed with hydrogen for 24 hours；
(8) it is 1 to use volume ratio:0.5 ethanol and acetone mixture ultrasonic wave cleaning step (7) sample 40 minutes
And dry up；
(9) fixture gripping step (7) specimen length direction two ends are used at room temperature, continue 2 hours；
(10) step (9) described sample was loaded the vacuum chamber of Auger electron spectrometer within 5 minutes, when vacuum reaches
During to requirement of experiment, setting Auger hammer is pressed into 0.5mm every time, 2 minutes interval times, after 5 press-ins, the 6th disposable pressure
Disconnected sample, obtains cleaning intergranular fracture.
On the fracture auger electrons spectral line that obtains of reconnaissance analysis show crystal ingedient mainly have Fe, Ni, Cr, C, S, P,
Si and suitable O, N composition of matrix of samples concentration, show that the fracture surface of sample is cleaning intergranular fracture, more can truly reflect crystalline substance
Boundary's composition.
Embodiment 2
A kind of method that intergranular fracture is obtained in austenitic steel, comprises the following steps：
(1) sampled on Ni-based GH536 austenitic alloys, be cut into the bar samples of 4 × 32mm of Φ；
(2) step (1) described sample is eliminated rust, decontamination, grinding process, it is 1 that volume ratio is used afterwards:2 ethanol
Sample is submerged with acetone mixture sample and carry out ultrasonic wave and cleaned 12 minutes, cleaned with deionized water and dried up；
(3) step (2) described sample is processed into Auger electron spectrometer standard specimen；
(4) it is 1 to use volume ratio:2 ethanol and acetone mixture sample immersion step (3) sample simultaneously carry out ultrasound
Ripple is cleaned 20 minutes, is cleaned with deionized water and dried up；
(5) it is 20 to use sulfuric acid and methanol quality ratio:80 sulfuric acid and methyl alcohol mixed liquor is as electrolytic polishing liquid to step
(4) specimen surface carries out electrobrightening, and sample is totally submerged in electrolytic polishing liquid, and electrobrightening voltage is 20V, time
It is 5s；
(6) it is 1 to use volume ratio:2 ethanol and acetone mixture sample submergence sample simultaneously carries out 15 points of ultrasonic wave cleaning
Clock, is cleaned and dried up with deionized water；
(7) cathodic hydrogen charging is carried out to step (6) described sample using electrolyte solution mode, being flushed with hydrogen current density is
800mA/cm2, the time is flushed with hydrogen for 12 hours；
(8) it is 1 to use volume ratio:2 ethanol and acetone mixture ultrasonic wave cleaning step (7) sample 60 minutes are simultaneously
Drying；
(9) fixture gripping step (7) specimen length direction two ends are used at room temperature, continue 5 hours；
(10) step (9) described sample was loaded the vacuum chamber of Auger electron spectrometer within 5 minutes, when vacuum reaches
During to requirement of experiment, setting Auger hammer is pressed into 2mm every time, 12 minutes interval times, after 2 press-ins, disposably breaks for the 3rd time
Sample, obtains cleaning intergranular fracture.
On the fracture auger electrons spectral line that obtains of reconnaissance analysis show crystal ingedient mainly have Fe, Ni, Cr, C, S, P,
Si and suitable O, N composition of matrix of samples concentration, show that the fracture surface of sample is cleaning intergranular fracture, more can truly reflect crystalline substance
Boundary's composition.
Embodiment 3
A kind of method that intergranular fracture is obtained in austenitic steel, comprises the following steps：
(1) sampled on Ni-based GH720Li austenitic alloys, be cut into the bar samples of 4 × 32mm of Φ；
(2) step (1) described sample is eliminated rust, decontamination, grinding process, it is 1 that volume ratio is used afterwards:1 ethanol
Sample is submerged with acetone mixture sample and carry out ultrasonic wave and cleaned 15 minutes, cleaned with deionized water and dried up；
(3) step (2) described sample is processed into Auger electron spectrometer standard specimen；
(4) it is 1 to use volume ratio:1 ethanol and acetone mixture sample immersion step (3) sample simultaneously carry out ultrasound
Ripple is cleaned 15 minutes, is cleaned with deionized water and dried up；
(5) it is 15 to use sulfuric acid and methanol quality ratio:85 sulfuric acid and methyl alcohol mixed liquor is as electrolytic polishing liquid to step
(4) specimen surface carries out electrobrightening, and sample is totally submerged in electrolytic polishing liquid, and electrobrightening voltage is 15V, time
It is 15s；
(6) it is 1 to use volume ratio:1 ethanol and acetone mixture sample submergence sample simultaneously carries out 18 points of ultrasonic wave cleaning
Clock, is cleaned and dried up with deionized water；
(7) cathodic hydrogen charging is carried out to step (6) described sample using electrolyte solution mode, being flushed with hydrogen current density is
500mA/cm2, the time is flushed with hydrogen for 20 hours；
(8) it is 1 to use volume ratio:1 ethanol and acetone mixture ultrasonic wave cleaning step (7) sample 50 minutes are simultaneously
Drying；
(9) fixture gripping step (7) specimen length direction two ends are used at room temperature, continue 3 hours；
(10) step (9) described sample was loaded the vacuum chamber of Auger electron spectrometer within 3 minutes, when vacuum reaches
During to requirement of experiment, setting Auger hammer is pressed into 1.5mm every time, and 10 minutes interval times, after 3 press-ins, the 4th is disposably pressed
Disconnected sample, obtains cleaning intergranular fracture, as shown in Figure 3.
On the fracture auger electrons spectral line that obtains of reconnaissance analysis show crystal ingedient mainly have Fe, Ni, Cr, C, S, P,
Si and suitable O, N composition of matrix of samples concentration, show that the fracture surface of sample is cleaning intergranular fracture, more can truly reflect crystalline substance
Boundary's composition.
Embodiment 4
A kind of method that intergranular fracture is obtained in austenitic steel, comprises the following steps：
(1) sampled on Ni-based GH536 austenitic alloys, be cut into the bar samples of 4 × 33mm of Φ；
(2) step (1) described sample is eliminated rust, decontamination, grinding process, it is 1 that volume ratio is used afterwards:1 ethanol
Sample is submerged with acetone mixture sample and carry out ultrasonic wave and cleaned 20 minutes, cleaned with deionized water and dried up；
(3) step (2) described sample is processed into Auger electron spectrometer standard specimen；
(4) it is 1 to use volume ratio:1 ethanol and acetone mixture sample immersion step (3) sample simultaneously carry out ultrasound
Ripple is cleaned 18 minutes, is cleaned with deionized water and dried up；
(5) it is 15 to use sulfuric acid and methanol quality ratio:85 sulfuric acid and methyl alcohol mixed liquor is as electrolytic polishing liquid to step
(4) specimen surface carries out electrobrightening, and sample is totally submerged in electrolytic polishing liquid, and electrobrightening voltage is 15V, time
It is 15s；
(6) it is 1 to use volume ratio:1 ethanol and acetone mixture sample submergence sample simultaneously carries out 20 points of ultrasonic wave cleaning
Clock, is cleaned and dried up with deionized water；
(7) cathodic hydrogen charging is carried out to step (6) described sample using electrolyte solution mode, being flushed with hydrogen current density is
700mA/cm2, the time is flushed with hydrogen for 18 hours；
(8) it is 1 to use volume ratio:1 ethanol and acetone mixture ultrasonic wave cleaning step (7) sample 55 minutes are simultaneously
Drying；
(9) fixture gripping step (7) specimen length direction two ends are used at room temperature, continue 4.5 hours；
(10) step (9) described sample was loaded the vacuum chamber of Auger electron spectrometer within 3 minutes, when vacuum reaches
During to requirement of experiment, setting Auger hammer is pressed into 0.8mm every time, and 9 minutes interval times, after 4 press-ins, the 5th is disposably pressed
Disconnected sample, obtains cleaning intergranular fracture.As shown in Figure 4.
(random) analysis of reconnaissance is obtained on the gained cleaning intergranular fracture of embodiment 4 auger electrons spectral line as shown in figure 5,
As seen in Figure 5, crystal ingedient is mainly constituted and (had by Fe, Ni, Cr, C, S, P, Si and matrix of samples concentration suitable O, N
A little elements are not marked), show that the fracture surface of sample is cleaning intergranular fracture, more can truly reflect crystal ingedient；As a comparison,
Fig. 6 is that reconnaissance is (random) on non-clean intergranular fracture analyzes the auger electrons spectral line for obtaining, and it uses side same as Example 4
Method obtains intergranular fracture, and difference is to be broken (in normal temperature room) under non-vacuum environment；As can be seen that its base from Fig. 6
The intensity of line impurity peaks is higher compared to the baseline impurity peak intensity of embodiment 4, during follow-up Grain Boundary Segregation analysis, may
The accuracy of meeting impact analysis result.
The present invention obtained in austenitic steel the method process is simple of intergranular fracture, time-consuming short, operating procedure it is simple it is controllable,
It is easily achieved；The method that the present invention obtains intergranular fracture in austenitic steel uses special process, and the austenitic steel for being obtained breaks
Mouth is typical intergranular fracture, can be prevented effectively from pollution, can provide objective and accurate evidence to crystal ingedient analysis, fits
For analyzing austenitic steel crystal ingedient.
Although illustrate and describing the present invention with specific embodiment, but will be appreciated that various embodiments above is only used
To illustrate technical scheme, rather than its limitations；It will be understood by those within the art that：Without departing substantially from this hair
In the case of bright spirit and scope, the technical scheme described in foregoing embodiments can be modified, or to wherein
Some or all of technical characteristic carries out equivalent；And these modifications or replacement, do not make the essence of appropriate technical solution
Depart from the scope of various embodiments of the present invention technical scheme；It is, therefore, intended that including belonging to the present invention in the following claims
In the range of all these substitutions and modifications.
Claims (10)
1. it is a kind of in austenitic steel obtain intergranular fracture method, it is characterised in that be included in austenitic steel specimen surface and enter
Row electrobrightening, carries out cathodic hydrogen charging to austenitic steel sample afterwards；Then the two ends of austenitic steel sample are clamped for a period of time,
Austenitic steel sample is loaded into surface analysis apparatus again；Under vacuum conditions, the default incision position in austenitic steel sample is carried out
After multiple first pressing, the default incision position of austenitic steel sample is disposably broken, obtain intergranular fracture.
2. it is according to claim 1 it is a kind of in austenitic steel obtain intergranular fracture method, it is characterised in that using electricity
Solution polishing fluid carries out electrobrightening to austenitic steel specimen surface；
Preferably, the electrolytic polishing liquid includes the mixed solution of acid and alcohol；
It is further preferred that the mass ratio of the acid and alcohol is 10-20:80-90, preferably 15-20：80-85, further preferably
It is 15:85；
It is further preferred that the acid includes one or more in inorganic acid and organic acid, sulfuric acid, phosphoric acid, lemon are preferably included
One kind in lemon acid, hydrofluoric acid, further preferably including sulfuric acid；
It is further preferred that the alcohol includes one or more in monohydric alcohol, dihydroxylic alcohols and polyalcohol, C1-C3 is preferably included
One or more in alcohol, further preferably including methyl alcohol.
3. it is according to claim 1 it is a kind of in austenitic steel obtain intergranular fracture method, it is characterised in that the electricity
The voltage for solving polishing is 10-20V, more preferably preferably 15-20V, 15V；
Preferably, the time of the electrobrightening is 5-15s, more preferably preferably 10-15s, 15s.
4. it is according to claim 1 it is a kind of in austenitic steel obtain intergranular fracture method, it is characterised in that described the moon
What pole was flushed with hydrogen is flushed with hydrogen current density for 300-800mA/cm2, preferably 500-800mA/cm2, more preferably 500-700mA/
cm2；
Preferably, the time that is flushed with hydrogen of the cathodic hydrogen charging is 12-24h, more preferably preferably 18-24h, 18-20h.
5. it is according to claim 1 it is a kind of in austenitic steel obtain intergranular fracture method, it is characterised in that the folder
The clamping time for holding the two ends of austenitic steel sample is 2-5h, more preferably preferably 3-5h, 4.5-5h.
6. it is according to claim 1 it is a kind of in austenitic steel obtain intergranular fracture method, it is characterised in that it is described just
Pressure is to be pressed into 0.5-2mm, more preferably preferably 0.8-2mm, 0.8-1.5mm every time in default incision position；
Preferably, during the multiple first pressing, 2-12min is spaced between adjacent 2 first pressing, preferably by 9-12min, enters one
Step is preferably by 9-10min；
Preferably, the number of times of the first pressing is 2-5 times, preferably 3-5 times, more preferably 3-4 times.
7. it is according to claim 1 it is a kind of in austenitic steel obtain intergranular fracture method, it is characterised in that described Austria
Family name's body steel curved beam is the standard specimen that can be used in surface analysis apparatus detection；
Preferably, the surface analysis apparatus include Auger electron spectrometer.
8. it is according to claim 1 it is a kind of in austenitic steel obtain intergranular fracture method, it is characterised in that in every step
Before technique is carried out, cleaning operation is carried out to austenitic steel sample respectively；
Preferably, the cleaning operation includes cleaning austenitic steel sample using washing lotion；
It is further preferred that the cleaning operation includes being totally submerged austenitic steel sample in washing lotion, cleaned；
It is further preferred that the cleaning operation includes being cleaned by ultrasonic austenitic steel sample using washing lotion；
It is further preferred that the washing lotion includes the mixed liquor of ethanol and acetone；
It is highly preferred that the volume ratio of ethanol and acetone is 1 in the washing lotion:0.5-2, preferably 1:0.5-1, more preferably
1:1；
Preferably, to carrying out cleaning operation to austenitic steel sample before the electrobrightening, scavenging period is 10-20min, preferably
It is 15-20min, more preferably 15-18min；
Preferably, to carrying out cleaning operation to austenitic steel sample before the cathodic hydrogen charging, scavenging period is 10-20min, preferably
It is 15-20min, more preferably 18-20min；
Preferably, to carrying out cleaning operation, scavenging period to austenitic steel sample before the two ends of the clamping austenitic steel sample
It is 40-60min, preferably 50-60min, more preferably 50-55min.
9. it is according to claim 1 it is a kind of in austenitic steel obtain intergranular fracture method, it is characterised in that the folder
Hold after the two ends of austenitic steel sample, within 5min, austenitic steel sample is loaded into surface analysis preferably within 3min
The vacuum chamber of device, vacuumizes immediately, after vacuum reaches requirement, carries out subsequent technique.
10. a kind of application of the method that intergranular fracture is obtained in austenitic steel as described in claim 1-9 is any, its feature
It is that the method that intergranular fracture is obtained in austenitic steel is used to analyze austenitic steel crystal ingedient.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109682727A (en) * | 2018-12-31 | 2019-04-26 | 盛利维尔（中国）新材料技术股份有限公司 | A method of for showing high-strength steel grain size |
| CN109827817A (en) * | 2017-11-23 | 2019-05-31 | 北京科技大学 | The electrolysis of NiCrCo system nickel base superalloy is flushed with hydrogen process |
| CN112304993A (en) * | 2020-10-28 | 2021-02-02 | 湖南华菱湘潭钢铁有限公司 | Spring steel austenite grain size detection method |
| CN112858359A (en) * | 2020-12-29 | 2021-05-28 | 武汉科技大学 | Method for obtaining peritectic fracture in oriented silicon steel |
| CN114574864A (en) * | 2021-12-08 | 2022-06-03 | 中国科学院金属研究所 | Metallographic corrosive agent for high-silicon austenitic stainless steel and color developing etching method |
-
2016
- 2016-12-29 CN CN201611247831.4A patent/CN106757301B/en active Active
Non-Patent Citations (3)
| Title |
|---|
| 李光福 等: "一种获得清洁沿晶断口的方法", 《理化经验 物理分册》 * |
| 李异 等: "316L不锈钢晶间腐蚀机理的探讨", 《腐蚀科学与防护技术》 * |
| 胡炜 等: "Ni-Fe奥氏体合金的氢脆及成分影响", 《金属学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109827817A (en) * | 2017-11-23 | 2019-05-31 | 北京科技大学 | The electrolysis of NiCrCo system nickel base superalloy is flushed with hydrogen process |
| CN109682727A (en) * | 2018-12-31 | 2019-04-26 | 盛利维尔（中国）新材料技术股份有限公司 | A method of for showing high-strength steel grain size |
| CN112304993A (en) * | 2020-10-28 | 2021-02-02 | 湖南华菱湘潭钢铁有限公司 | Spring steel austenite grain size detection method |
| CN112304993B (en) * | 2020-10-28 | 2022-07-26 | 湖南华菱湘潭钢铁有限公司 | Spring steel austenite grain size detection method |
| CN112858359A (en) * | 2020-12-29 | 2021-05-28 | 武汉科技大学 | Method for obtaining peritectic fracture in oriented silicon steel |
| CN114574864A (en) * | 2021-12-08 | 2022-06-03 | 中国科学院金属研究所 | Metallographic corrosive agent for high-silicon austenitic stainless steel and color developing etching method |
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