CN106757301B - A kind of method and its application obtaining intergranular fracture in austenitic steel - Google Patents
A kind of method and its application obtaining intergranular fracture in austenitic steel Download PDFInfo
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- CN106757301B CN106757301B CN201611247831.4A CN201611247831A CN106757301B CN 106757301 B CN106757301 B CN 106757301B CN 201611247831 A CN201611247831 A CN 201611247831A CN 106757301 B CN106757301 B CN 106757301B
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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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- 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 present invention provides a kind of in austenitic steel obtains the method and its application of intergranular fracture.The present invention carries out electrobrightening in austenitic steel specimen surface, carries out cathodic hydrogen charging to austenitic steel sample later；Then the both ends for clamping austenitic steel sample for a period of time, then by austenitic steel sample are packed into surface analysis apparatus；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, intergranular fracture is obtained.The method of the present invention simple process, time-consuming short, operating procedure is simply controllable, is easily achieved；Present invention austenitic steel fracture obtained is typical intergranular fracture, can effectively be avoided pollution, and can analyze to crystal ingedient and provide objective and accurate evidence, is suitable for analyzing austenitic steel crystal ingedient.
Description
Technical field
The present invention relates to steel material analysis technical fields, obtain in austenitic steel along crystalline substance in particular to one kind
The method and its application of fracture.
Background technique
In the analysis and research of austenitic steel crystal ingedient, especially in the research of crystal boundary segregation behavior, to crystal boundary microcell
The key that ingredient is accurately analyzed is to clean the acquisition of 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, the prior art is difficult to obtain intergranular fracture；In addition, using prior art preparation
Intergranular fracture complex process easily causes austenitic steel sample contamination in technical process, to influence austenitic steel crystal ingedient point
Analyse the accuracy of result, it is difficult to obtain accurate, true crystal boundary segregation behavioural analysis conclusion.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of method for obtaining intergranular fracture in austenitic steel, this method technique
Simply, time-consuming short, operating procedure is simply controllable, is easily achieved, and austenitic steel fracture obtained is typical intergranular fracture, energy
It is enough effectively to avoid pollution, it can be analyzed to crystal ingedient and provide objective and accurate evidence.
The second object of the present invention is to provide a kind of answering for above-mentioned method for obtaining intergranular fracture in austenitic steel
With this method is used to analyze austenitic steel crystal ingedient, can obtain clean austenitic steel intergranular fracture, gives crystal ingedient
Analysis provides objective and accurate evidence.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A method of it obtaining intergranular fracture in austenitic steel, is included in austenitic steel specimen surface and carries out electrolysis throwing
Light carries out cathodic hydrogen charging to austenitic steel sample later；Then the both ends of austenitic steel sample are clamped for a period of time, then by Ovshinsky
Body steel curved beam is packed into surface analysis apparatus；Under vacuum conditions, multiple first pressing is carried out in the default incision position of austenitic steel sample
Afterwards, the default incision position of austenitic steel sample is disposably broken, obtains intergranular fracture.
The method and process that the present invention obtains intergranular fracture in austenitic steel is simple, time-consuming short, operating procedure is simply controllable,
It is easily achieved；The present invention obtains the method for intergranular fracture using special process in austenitic steel, and austenitic steel obtained is disconnected
Mouth is typical intergranular fracture, can effectively be avoided pollution, and can analyze to crystal ingedient and provide objective and accurate evidence.
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 it is described acid and alcohol mass ratio be 10-20:80-90, preferably 15-20:80-85, further preferably
For 15:85.
It is highly preferred that the acid includes one of inorganic acid and organic acid or a variety of, sulfuric acid, phosphoric acid, lemon are preferably included
One of lemon acid, hydrofluoric acid further preferably include sulfuric acid.
It is highly preferred that the alcohol includes one of monohydric alcohol, dihydric alcohol and polyalcohol or a variety of, C1-C3 is preferably included
One of alcohol is a variety of, further preferably includes methanol.
Preferably, the voltage of the electrobrightening is 10-20V, preferably 15-20V, further preferably 15V.
Preferably, the time of the electrobrightening is 5-15s, preferably 10-15s, further preferably 15s.
Preferably, the current density that is flushed with hydrogen of the cathodic hydrogen charging is 300-800mA/cm2, preferably 500-800mA/cm2,
Further preferably 500-700mA/cm2。
Preferably, the time that is flushed with hydrogen of the cathodic hydrogen charging is 12-24h, preferably 18-24h, further preferably 18-
20h。
Preferably, it is described clamping austenitic steel sample both ends the clamping time be 2-5h, preferably 3-5h, further it is excellent
It is selected as 4.5-5h.
Preferably, the first pressing is to be pressed into 0.5-2mm, preferably 0.8-2mm every time in default incision position, further preferably
For 0.8-1.5mm.
Preferably, during the multiple first pressing, it is spaced 2-12min between adjacent 2 first pressing, preferably by 9-12min,
Further preferably interval 9-10min；
Preferably, the number of the first pressing is 2-5 times, preferably 3-5 times, further preferably 3-4 times.
Preferably, the austenitic steel sample is the standard sample that can be used in surface analysis apparatus detection.
Preferably, the surface analysis apparatus includes Auger electron spectrometer.
Preferably, before the progress of every step process, cleaning operation is carried out to austenitic steel sample respectively；
It is further preferred that the cleaning operation includes being cleaned using washing lotion to austenitic steel sample；
It is highly preferred that the cleaning operation includes that austenitic steel sample is totally submerged in washing lotion, cleaned；
It is highly preferred that the cleaning operation includes being cleaned by ultrasonic using washing lotion to austenitic steel sample；
It is highly preferred that the washing lotion includes the mixed liquor of ethyl alcohol and acetone；
Most preferably, in the washing lotion volume ratio of ethyl alcohol and acetone be 1:0.5-2, preferably 1:0.5-1, further it is excellent
It is selected as 1:1；
It is further preferred that carrying out cleaning operation, scavenging period 10- to austenitic steel sample before the electrobrightening
20min, preferably 15-20min, further preferably 15-18min；
It is further preferred that carrying out cleaning operation, scavenging period 10- to austenitic steel sample before the cathodic hydrogen charging
20min, preferably 15-20min, further preferably 18-20min；
It is further preferred that carrying out cleaning behaviour to austenitic steel sample before the both ends of the clamping austenitic steel sample
Make, scavenging period 40-60min, preferably 50-60min, further preferably 50-55min.
Preferably, after the both ends of the clamping austenitic steel sample, within 5min, by Ovshinsky preferably within 3min
Body steel curved beam is packed into the vacuum chamber of surface analysis apparatus, vacuumizes immediately, after vacuum degree 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
Clean austenitic steel intergranular fracture is obtained, provides objective and accurate evidence to crystal ingedient analysis.
Compared with prior art, the invention has the benefit that
The method and process that the present invention obtains intergranular fracture in austenitic steel is simple, time-consuming short, operating procedure is simply controllable,
It is easily achieved；The present invention obtains the method for intergranular fracture using special process in austenitic steel, and austenitic steel obtained is disconnected
Mouth is typical intergranular fracture, can effectively be avoided pollution, and can analyze to crystal ingedient and provide objective and accurate evidence, fit
For analyzing austenitic steel crystal ingedient.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is a kind of method and process flow chart of specific embodiment of the present invention；
Fig. 2 is Auger electron spectrometer standard sample specification schematic diagram used by a kind of specific embodiment of the present invention；
Fig. 3 is cleaning obtained by the embodiment of the present invention 3 along the stereoscan photograph of brilliant section；
Fig. 4 is cleaning obtained by the embodiment of the present invention 4 along the stereoscan photograph of brilliant section；
Fig. 5 is cleaning obtained by the embodiment of the present invention 4 along the auger electrons spectral line of brilliant section；
Fig. 6 is the auger electrons spectral line of non-clean intergranular fracture.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with the drawings and specific embodiments, but
Be it will be understood to those of skill in the art that it is following described embodiments are some of the embodiments of the present invention, rather than it is whole
Embodiment is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.Based on the embodiments of the present invention, ability
Domain those of ordinary skill every other embodiment obtained without making creative work, belongs to guarantor of the present invention
The range of shield.The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same
Or production firm person is not specified in instrument, is the conventional products that can be obtained by commercially available purchase.
In the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to
Convenient for description the present invention and simplify description, rather than the device or element of indication or suggestion meaning must have a particular orientation,
It is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.In addition, term " first ", " second ",
" third " is used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, can also can be indirectly connected through an intermediary
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood at this with concrete condition
Concrete meaning in invention.
The method that the present invention provides a kind of to obtain intergranular fracture in austenitic steel, is included in austenitic steel specimen surface
Electrobrightening is carried out, cathodic hydrogen charging is carried out to austenitic steel sample later；When then clamping one section of the both ends of austenitic steel sample
Between, then by austenitic steel sample be packed into surface analysis apparatus；Under vacuum conditions, the default incision position of austenitic steel sample into
After the multiple first pressing of row, the default incision position of austenitic steel sample is disposably broken, intergranular fracture is obtained.
The method and process that the present invention obtains intergranular fracture in austenitic steel is simple, time-consuming short, operating procedure is simply controllable,
It is easily achieved；The present invention obtains the method for intergranular fracture using special process in austenitic steel, and austenitic steel obtained is disconnected
Mouth is typical intergranular fracture, can effectively be avoided pollution, and can analyze to crystal ingedient and provide objective and accurate evidence.
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 it is described acid and alcohol mass ratio be 10-20:80-90, preferably 15-20:80-85, further
Preferably 15:85.
It is further preferred that the acid includes one of inorganic acid and organic acid or a variety of, sulfuric acid, phosphorus are preferably included
One of acid, citric acid, hydrofluoric acid further preferably include sulfuric acid.
It is further preferred that the alcohol includes one of monohydric alcohol, dihydric alcohol and polyalcohol or a variety of, preferably include
One of C1-C3 alcohol is a variety of, further preferably includes methanol.
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, equipotential tissue is built up in hole mentions its corrosion resisting property significantly to obtain equipotential surface
Height avoids introducing corrosion contact scar during subsequent fracture obtains, and improves the accurate of austenitic steel crystal ingedient analysis result
Property, keep crystal boundary segregation behavioural analysis conclusion more acurrate, truer.
In a kind of preferred embodiment of the present invention, the voltage of the electrobrightening is 10-20V, preferably 15-
20V, further preferably 15V.
In a kind of preferred embodiment of the present invention, the time of the electrobrightening is 5-15s, preferably 10-
15s, further 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, equipotential tissue is built up in hole keeps its corrosion resisting property big to obtain equipotential surface
It is big to improve, it avoids introducing corrosion contact scar during subsequent fracture obtains, improves austenitic steel crystal ingedient analysis result
Accuracy keeps crystal boundary segregation behavioural analysis conclusion more acurrate, 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, further 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, further preferably 18-20h.
Process conditions are flushed with hydrogen using particular cathode, cathodic hydrogen charging is carried out to austenitic steel sample, can be improved austenitic steel examination
The brittleness of sample smoothly obtains fracture convenient for subsequent；It can be avoided the toughness due to austenitic steel itself simultaneously, it caused to be difficult to press
It is disconnected, and the intergranular fracture that can accurately, really reflect austenitic steel crystal boundary segregation behavior cannot be obtained due to generating deformation.
In a kind of preferred embodiment of the present invention, the clamping time at the both ends of the clamping austenitic steel sample is
2-5h, preferably 3-5h, further preferably 4.5-5h.
After cathodic hydrogen charging operation, the both ends specific time of austenitic steel sample is clamped, helps sufficiently to improve and fill
Hydrogen effect makes hydrogen sufficiently agglomerate into hydrogen molecule, improves the internal stress of austenitic steel sample, its stress is caused to concentrate, and is more than it
Strength degree further decreases the toughness of austenitic steel sample, convenient for it is subsequent obtain can accurately, really reflect austenitic steel
The intergranular fracture of crystal boundary segregation behavior.
Preferably, the both ends of the austenitic steel sample are clamped using fixture.
It is further preferred that clamping the both ends in 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, further 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, further preferably interval 9-10min.
In a kind of preferred embodiment of the present invention, the number of the first pressing is 2-5 times, preferably 3-5 times, into one
Step preferably 3-4 times.
It breaks mode using specific and breaks austenitic steel sample, can guarantee the accuracy of gained fracture site, and
The mechanical performance that austenitic steel can be sufficiently reduced by multiple first pressing promotes it that can once be broken, obtains 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 sample of detection.
In a kind of preferred embodiment of the present invention, the surface analysis apparatus includes Auger electron spectrometer.
Auger spectroscopy analysis occupies highly important status in material surface constituent analysis work, analyzes the standard of result
The objectivity and accuracy of constituent analysis conclusion will be directly influenced whether really.It is micro- using Auger spectroscopy analysis technical research crystal boundary
Area's ingredient has become a kind of effective means for studying the segregation behavior of austenitic steel crystal boundary.
Preferably, using the standard sample cooperated with Auger electron spectrometer in various embodiments of the present invention.
Preferably, it can be sampled on austenitic steel, and be processed into the standard sample of Auger electron spectrometer.
Optionally, various embodiments of the present invention use the Auger electron spectrometer standard sample of specification as shown in Figure 2.
In a kind of preferred embodiment of the present invention, before the progress of every step process, respectively to austenitic steel sample
Carry out cleaning operation.
Preferably, the cleaning operation includes being cleaned using washing lotion to austenitic steel sample.
It is further preferred that the cleaning operation includes that austenitic steel sample is totally submerged in washing lotion, cleaned.
It is further preferred that the cleaning operation includes being cleaned by ultrasonic using washing lotion to austenitic steel sample.
It is further preferred that the washing lotion includes the mixed liquor of ethyl alcohol and acetone.
It is highly preferred that in the washing lotion volume ratio of ethyl alcohol and acetone be 1:0.5-2, preferably 1:0.5-1, further it is excellent
It is selected as 1:1.
Preferably, before the electrobrightening to austenitic steel sample carry out cleaning operation, scavenging period 10-20min,
Preferably 15-20min, further preferably 15-18min.
Preferably, before the cathodic hydrogen charging to austenitic steel sample carry out cleaning operation, scavenging period 10-20min,
Preferably 15-20min, further preferably 18-20min.
Preferably, cleaning operation, cleaning are carried out to austenitic steel sample before the both ends of the clamping austenitic steel sample
Time is 40-60min, preferably 50-60min, further preferably 50-55min.
Using specific cleaning process, help that the austenitic steel sample is made to keep cleaning in earning a technical process,
Clean intergranular fracture is finally obtained, avoids introducing various pollutants, improves the accurate of austenitic steel crystal ingedient analysis result
Property, keep crystal boundary segregation behavioural analysis conclusion more acurrate, truer.
In a kind of preferred embodiment of the present invention, such as austenitic steel sample is by sampling it in austenitic steel
Post-processing obtains, then before its processing, should carry out cleaning pretreatment.
Preferably, the cleaning pretreatment include austenitic steel sampling derusted, decontamination, grinding process, then carry out
Cleaning operation.
Preferably, the cleaning operation includes being cleaned using washing lotion to austenitic steel sample.
It is further preferred that the cleaning operation includes that austenitic steel sample is totally submerged in washing lotion, cleaned.
It is further preferred that the cleaning operation includes being cleaned by ultrasonic using washing lotion to austenitic steel sample.
It is further preferred that the washing lotion includes the mixed liquor of ethyl alcohol and acetone.
It is highly preferred that in the washing lotion volume ratio of ethyl alcohol and acetone be 1:0.5-2, preferably 1:0.5-1, further it is excellent
It is selected as 1:1.
Preferably, the scavenging period is 10-20min, preferably 12-20min, further preferably 15-20min.
In a kind of preferred embodiment of the present invention, after the both ends of the clamping austenitic steel sample, in 5min
Within, austenitic steel sample is packed into the vacuum chamber of surface analysis apparatus preferably within 3min, vacuumizes immediately, works as vacuum degree
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
Corrosive media occurs chemical reaction and generates fracture attachment and corrosion product, to improve austenitic steel crystal ingedient analysis knot
The accuracy of fruit keeps crystal boundary segregation behavioural analysis conclusion more acurrate, 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
Clean austenitic steel intergranular fracture is obtained, provides objective and accurate evidence to crystal ingedient analysis.
Embodiment 1
A method of it obtaining intergranular fracture in austenitic steel, includes the following steps:
(1) it is sampled on Ni-based GH720Li austenitic alloy, is cut into the bar samples of 4 × 32mm of Φ；
(2) it is derusted to step (1) described sample, decontamination, grinding process, uses volume ratio for the second of 1:0.5 later
Pure and mild acetone mixture sample submerges sample and carries out ultrasonic cleaning 10 minutes, is cleaned and is dried up with deionized water；
(3) step (2) described sample is processed into Auger electron spectrometer standard sample；
(4) volume ratio is used as the ethyl alcohol of 1:0.5 and acetone mixture sample immersion step (3) sample and is surpassed
Sound wave cleans 10 minutes, is cleaned and is dried up with deionized water；
(5) use sulfuric acid and methanol quality than for the sulfuric acid of 10:90 and methyl alcohol mixed liquor 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
For 10s；
(6) volume ratio is used as the ethyl alcohol of 1:0.5 and acetone mixture sample submergence sample and carries out ultrasonic cleaning 10
Minute, it is cleaned and is dried up with deionized water；
(7) cathodic hydrogen charging is carried out to step (6) sample using electrolyte solution mode, being flushed with hydrogen current density is
300mA/cm2, being flushed with hydrogen the time is 24 hours；
(8) use volume ratio for the ethyl alcohol of 1:0.5 and acetone mixture ultrasonic cleaning step (7) sample 40 minutes
And it dries up；
(9) fixture gripping step (7) specimen length direction both ends are used at room temperature, it is for 2 hours；
(10) step (9) described sample is packed into the vacuum chamber of Auger electron spectrometer within 5 minutes, when vacuum degree reaches
When to requirement of experiment, setting Auger hammer is pressed into 0.5mm every time, and interval time 2 minutes, after 5 indentations, the 6th disposable pressure
Disconnected sample obtains cleaning intergranular fracture.
The auger electrons spectral line that reconnaissance is analyzed on the fracture show crystal ingedient mainly and have Fe, Ni, Cr, C, S, P,
Si and comparable O, N composition of matrix of samples concentration show that the fracture surface of sample for cleaning intergranular fracture, can more be truly reflected crystalline substance
Boundary's ingredient.
Embodiment 2
A method of it obtaining intergranular fracture in austenitic steel, includes the following steps:
(1) it is sampled on Ni-based GH536 austenitic alloy, is cut into the bar samples of 4 × 32mm of Φ；
(2) it is derusted to step (1) described sample, decontamination, grinding process, uses volume ratio for the ethyl alcohol of 1:2 later
Sample is submerged with acetone mixture sample and carries out ultrasonic cleaning 12 minutes, is cleaned and is dried up with deionized water；
(3) step (2) described sample is processed into Auger electron spectrometer standard sample；
(4) volume ratio is used as the ethyl alcohol of 1:2 and acetone mixture sample immersion step (3) sample and carries out ultrasound
Wave cleans 20 minutes, is cleaned and is dried up with deionized water；
(5) use sulfuric acid and methanol quality than for the sulfuric acid of 20:80 and methyl alcohol mixed liquor 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
For 5s；
(6) volume ratio is used to submerge sample for the ethyl alcohol of 1:2 and acetone mixture sample and carry out ultrasonic cleaning 15 and divide
Clock is cleaned and is dried up with deionized water；
(7) cathodic hydrogen charging is carried out to step (6) sample using electrolyte solution mode, being flushed with hydrogen current density is
800mA/cm2, being flushed with hydrogen the time is 12 hours；
(8) use volume ratio for the ethyl alcohol of 1:2 and acetone mixture ultrasonic cleaning step (7) sample 60 minutes simultaneously
Drying；
(9) fixture gripping step (7) specimen length direction both ends are used at room temperature, it is for 5 hours；
(10) step (9) described sample is packed into the vacuum chamber of Auger electron spectrometer within 5 minutes, when vacuum degree reaches
When to requirement of experiment, setting Auger hammer is pressed into 2mm every time, interval time 12 minutes, after 2 indentations, disposably breaks for the 3rd time
Sample obtains cleaning intergranular fracture.
The auger electrons spectral line that reconnaissance is analyzed on the fracture show crystal ingedient mainly and have Fe, Ni, Cr, C, S, P,
Si and comparable O, N composition of matrix of samples concentration show that the fracture surface of sample for cleaning intergranular fracture, can more be truly reflected crystalline substance
Boundary's ingredient.
Embodiment 3
A method of it obtaining intergranular fracture in austenitic steel, includes the following steps:
(1) it is sampled on Ni-based GH720Li austenitic alloy, is cut into the bar samples of 4 × 32mm of Φ；
(2) it is derusted to step (1) described sample, decontamination, grinding process, uses volume ratio for the ethyl alcohol of 1:1 later
Sample is submerged with acetone mixture sample and carries out ultrasonic cleaning 15 minutes, is cleaned and is dried up with deionized water；
(3) step (2) described sample is processed into Auger electron spectrometer standard sample；
(4) volume ratio is used as the ethyl alcohol of 1:1 and acetone mixture sample immersion step (3) sample and carries out ultrasound
Wave cleans 15 minutes, is cleaned and is dried up with deionized water；
(5) use sulfuric acid and methanol quality than for the sulfuric acid of 15:85 and methyl alcohol mixed liquor 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
For 15s；
(6) volume ratio is used to submerge sample for the ethyl alcohol of 1:1 and acetone mixture sample and carry out ultrasonic cleaning 18 and divide
Clock is cleaned and is dried up with deionized water；
(7) cathodic hydrogen charging is carried out to step (6) sample using electrolyte solution mode, being flushed with hydrogen current density is
500mA/cm2, being flushed with hydrogen the time is 20 hours；
(8) use volume ratio for the ethyl alcohol of 1:1 and acetone mixture ultrasonic cleaning step (7) sample 50 minutes simultaneously
Drying；
(9) fixture gripping step (7) specimen length direction both ends are used at room temperature, it is for 3 hours；
(10) step (9) described sample is packed into the vacuum chamber of Auger electron spectrometer within 3 minutes, when vacuum degree reaches
When to requirement of experiment, setting Auger hammer is pressed into 1.5mm every time, and interval time 10 minutes, after 3 indentations, the 4th was disposably pressed
Disconnected sample obtains cleaning intergranular fracture, as shown in Figure 3.
The auger electrons spectral line that reconnaissance is analyzed on the fracture show crystal ingedient mainly and have Fe, Ni, Cr, C, S, P,
Si and comparable O, N composition of matrix of samples concentration show that the fracture surface of sample for cleaning intergranular fracture, can more be truly reflected crystalline substance
Boundary's ingredient.
Embodiment 4
A method of it obtaining intergranular fracture in austenitic steel, includes the following steps:
(1) it is sampled on Ni-based GH536 austenitic alloy, is cut into the bar samples of 4 × 33mm of Φ；
(2) it is derusted to step (1) described sample, decontamination, grinding process, uses volume ratio for the ethyl alcohol of 1:1 later
Sample is submerged with acetone mixture sample and carries out ultrasonic cleaning 20 minutes, is cleaned and is dried up with deionized water；
(3) step (2) described sample is processed into Auger electron spectrometer standard sample；
(4) volume ratio is used as the ethyl alcohol of 1:1 and acetone mixture sample immersion step (3) sample and carries out ultrasound
Wave cleans 18 minutes, is cleaned and is dried up with deionized water；
(5) use sulfuric acid and methanol quality than for the sulfuric acid of 15:85 and methyl alcohol mixed liquor 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
For 15s；
(6) volume ratio is used to submerge sample for the ethyl alcohol of 1:1 and acetone mixture sample and carry out ultrasonic cleaning 20 and divide
Clock is cleaned and is dried up with deionized water；
(7) cathodic hydrogen charging is carried out to step (6) sample using electrolyte solution mode, being flushed with hydrogen current density is
700mA/cm2, being flushed with hydrogen the time is 18 hours；
(8) use volume ratio for the ethyl alcohol of 1:1 and acetone mixture ultrasonic cleaning step (7) sample 55 minutes simultaneously
Drying；
(9) fixture gripping step (7) specimen length direction both ends are used at room temperature, continue 4.5 hours；
(10) step (9) described sample is packed into the vacuum chamber of Auger electron spectrometer within 3 minutes, when vacuum degree reaches
When to requirement of experiment, setting Auger hammer is pressed into 0.8mm every time, and interval time 9 minutes, after 4 indentations, the 5th was disposably pressed
Disconnected sample obtains cleaning intergranular fracture.As shown in Figure 4.
(random) the obtained auger electrons spectral line of analysis of reconnaissance on the cleaning intergranular fracture obtained by embodiment 4 as shown in figure 5,
As seen in Figure 5, crystal ingedient is mainly made of Fe, Ni, Cr, C, S, P, Si and matrix of samples concentration comparable O, N and (has
A little elements do not mark), show that the fracture surface of sample for cleaning intergranular fracture, can more be truly reflected crystal ingedient；As a comparison,
Fig. 6, which is that reconnaissance is (random) on non-clean intergranular fracture, analyzes obtained auger electrons spectral line, uses side same as Example 4
Method obtains intergranular fracture, and difference is under non-vacuum environment to be broken (in room temperature room)；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, may in subsequent crystal boundary segregation analytic process
It will affect precision of analysis.
The method and process that the present invention obtains intergranular fracture in austenitic steel is simple, time-consuming short, operating procedure is simply controllable,
It is easily achieved；The present invention obtains the method for intergranular fracture using special process in austenitic steel, and austenitic steel obtained is disconnected
Mouth is typical intergranular fracture, can effectively be avoided pollution, and can analyze to crystal ingedient and provide objective and accurate evidence, fit
For analyzing austenitic steel crystal ingedient.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that the above various embodiments is only used
To illustrate technical solution of the present invention, rather than its limitations；Those skilled in the art should understand that: without departing substantially from this hair
It in the case where bright spirit and scope, is possible to modify the technical solutions described in the foregoing embodiments, or to wherein
Some or all of technical characteristic is equivalently replaced；And these are modified or replaceed, and do not make the essence of corresponding technical solution
It departs from the scope of the technical solutions of the embodiments of the present invention；It is, therefore, intended that in the following claims including belonging to the present invention
All these substitutions and modifications in range.
Claims (58)
1. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel, which is characterized in that be included in Ni-based austenitic steel examination
Sample surface carries out electrobrightening, carries out cathodic hydrogen charging to Ni-based austenitic steel sample later；Then Ni-based austenitic steel examination is clamped
The both ends of sample for a period of time, then by Ni-based austenitic steel sample are packed into surface analysis apparatus；Under vacuum conditions, in Ni-based Ovshinsky
After the default incision position of body steel curved beam carries out multiple first pressing, the default incision position of Ni-based austenitic steel sample is disposably broken,
Obtain intergranular fracture.
2. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that adopt
Electrobrightening is carried out to Ni-based austenitic steel specimen surface with electrolytic polishing liquid.
3. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 2, which is characterized in that institute
State the mixed solution that electrolytic polishing liquid includes acid and alcohol.
4. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that institute
The mass ratio for stating acid and alcohol is 10-20:80-90.
5. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that institute
The mass ratio for stating acid and alcohol is 15-20:80-85.
6. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that institute
The mass ratio for stating acid and alcohol is 15:85.
7. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that institute
Stating acid includes one of inorganic acid and organic acid or a variety of.
8. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that institute
Stating acid includes one of sulfuric acid, phosphoric acid, citric acid, hydrofluoric acid.
9. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that institute
Stating acid includes sulfuric acid.
10. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that
The alcohol includes one of monohydric alcohol, dihydric alcohol and polyalcohol or a variety of.
11. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that
The alcohol includes one of C1-C3 alcohol or a variety of.
12. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that
The alcohol includes methanol.
13. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that
The voltage of the electrobrightening is 10-20V.
14. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that
The voltage of the electrobrightening is 15-20V.
15. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that
The voltage of the electrobrightening is 15V.
16. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that
The time of the electrobrightening is 5-15s.
17. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that
The time of the electrobrightening is 10-15s.
18. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 3, which is characterized in that
The time of the electrobrightening is 15s.
19. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The current density that is flushed with hydrogen of the cathodic hydrogen charging is 300-800mA/cm2。
20. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The current density that is flushed with hydrogen of the cathodic hydrogen charging is 500-800mA/cm2。
21. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The current density that is flushed with hydrogen of the cathodic hydrogen charging is 500-700mA/cm2。
22. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 19, which is characterized in that
The time that is flushed with hydrogen of the cathodic hydrogen charging is 12-24h.
23. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 19, which is characterized in that
The time that is flushed with hydrogen of the cathodic hydrogen charging is 18-24h.
24. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 19, which is characterized in that
The time that is flushed with hydrogen of the cathodic hydrogen charging is 18-20h.
25. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The clamping time at the both ends of the Ni-based austenitic steel sample of clamping is 2-5h.
26. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The clamping time at the both ends of the Ni-based austenitic steel sample of clamping is 3-5h.
27. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The clamping time at the both ends of the Ni-based austenitic steel sample of clamping is 4.5-5h.
28. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The first pressing is to be pressed into 0.5-2mm every time in default incision position.
29. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The first pressing is to be pressed into 0.8-2mm every time in default incision position.
30. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The first pressing is to be pressed into 0.8-1.5mm every time in default incision position.
31. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
During the multiple first pressing, 2-12min is spaced between adjacent 2 first pressing.
32. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
During the multiple first pressing, 9-12min is spaced between adjacent 2 first pressing.
33. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
It is spaced during the multiple first pressing, is spaced 9-10min between adjacent 2 first pressing.
34. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The number of the first pressing is 2-5 times.
35. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The number of the first pressing is 3-5 times.
36. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The number of the first pressing is 3-4 times.
37. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The Ni-based austenitic steel sample is the standard sample that can be used in surface analysis apparatus detection.
38. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
The surface analysis apparatus includes Auger electron spectrometer.
39. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
Before the progress of every step process, cleaning operation is carried out to Ni-based austenitic steel sample respectively.
40. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 39, which is characterized in that
The cleaning operation includes being cleaned using washing lotion to Ni-based austenitic steel sample.
41. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 39, which is characterized in that
The cleaning operation includes that Ni-based austenitic steel sample is totally submerged in washing lotion, is cleaned.
42. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 39, which is characterized in that
The cleaning operation includes being cleaned by ultrasonic using washing lotion to Ni-based austenitic steel sample.
43. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 39, which is characterized in that
The washing lotion includes the mixed liquor of ethyl alcohol and acetone.
44. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 43, which is characterized in that
The volume ratio of ethyl alcohol and acetone is 1:0.5-2 in the washing lotion.
45. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 43, which is characterized in that
The volume ratio of ethyl alcohol and acetone is 1:0.5-1 in the washing lotion.
46. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 43, which is characterized in that
The volume ratio of ethyl alcohol and acetone is 1:1 in the washing lotion.
47. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 39, which is characterized in that
Cleaning operation, scavenging period 10-20min are carried out to Ni-based austenitic steel sample before the electrobrightening.
48. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 39, which is characterized in that
Cleaning operation, scavenging period 15-20min are carried out to Ni-based austenitic steel sample before the electrobrightening.
49. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
Cleaning operation, scavenging period 15-18min are carried out to Ni-based austenitic steel sample before the electrobrightening.
50. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 39, which is characterized in that
Cleaning operation, scavenging period 10-20min are carried out to Ni-based austenitic steel sample before the cathodic hydrogen charging.
51. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 39, which is characterized in that
Cleaning operation, scavenging period 15-20min are carried out to Ni-based austenitic steel sample before the cathodic hydrogen charging.
52. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 39, which is characterized in that
Cleaning operation, scavenging period 18-20min are carried out to Ni-based austenitic steel sample before the cathodic hydrogen charging.
53. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
Cleaning operation is carried out to Ni-based austenitic steel sample before the both ends of the Ni-based austenitic steel sample of clamping, scavenging period is
40-60min。
54. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
Cleaning operation is carried out to Ni-based austenitic steel sample before the both ends of the Ni-based austenitic steel sample of clamping, scavenging period is
50-60min。
55. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
Cleaning operation is carried out to Ni-based austenitic steel sample before the both ends of the Ni-based austenitic steel sample of clamping, scavenging period is
50-55min。
56. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
After the both ends of the Ni-based austenitic steel sample of clamping, Ni-based austenitic steel sample is packed into surface analysis dress within 5min
The vacuum chamber set, vacuumizes immediately, after vacuum degree reaches requirement, carries out subsequent technique.
57. a kind of method for obtaining intergranular fracture in Ni-based austenitic steel according to claim 1, which is characterized in that
After the both ends of the Ni-based austenitic steel sample of clamping, Ni-based austenitic steel sample is packed into surface analysis dress within 3min
The vacuum chamber set, vacuumizes immediately, after vacuum degree reaches requirement, carries out subsequent technique.
58. a kind of application of method that intergranular fracture is obtained in Ni-based austenitic steel as described in claim 1-57 is any,
It is characterized in that, the method for obtaining intergranular fracture in Ni-based austenitic steel is used for Ni-based austenitic steel crystal ingedient point
Analysis.
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