CN109211628A - A kind of microscopic detection method for cast superalloy level of creep - Google Patents
A kind of microscopic detection method for cast superalloy level of creep Download PDFInfo
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- CN109211628A CN109211628A CN201811033940.5A CN201811033940A CN109211628A CN 109211628 A CN109211628 A CN 109211628A CN 201811033940 A CN201811033940 A CN 201811033940A CN 109211628 A CN109211628 A CN 109211628A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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Abstract
The invention discloses a kind of microscopic detection methods for cast superalloy level of creep, include: the preparation of 1) sample: being randomly selected in measuring samples several, it is cut into sample, then after cleaning removal surface and oil contaminant, it is inlayed again, sample polishing after inlaying, then washes with water, alcohol rinse, drying；The sample that polishing is completed, half are used for microexamination Creep hole and micro-crack；The other half is used for microexamination γ ' phase；2) detection method: 201) emptying hole and micro-crack are detected using optical metallographic microscope；Sample is looked first at, after finding the dotted and linear display of black, continues observation and determines whether display is Creep hole and micro-crack；Creep hole and micro-crack are opened along carbide or eutectic phase and matrix phase boundary edge；202) γ ' phase raftization carries out detecting whether γ ' phase raft using optical metallographic microscope.The present invention is used for the judgement of cast superalloy creep impairment degree, and makes relatively accurate estimate to part service life.
Description
Technical field
The present invention relates to a kind of microscopic detection methods for cast superalloy level of creep, are suitable for casting high temperature and close
Gold is to detect cast superalloy when long using the microscopic method of rear level of creep.
Background technique
Creep is an important feature of mechanics of metal behavior under high temperature, is that metal is made in prolonged constant temperature, constant load
The phenomenon that being plastically deformed with lower slow generation.The parts such as aero-engine turbo blade, guide vane, majority are that high temperature closes
Golden material uses under high temperature, centrifugal force effect for a long time, is also easy to produce creep impairment, and then influence part service life.At present
There is no the determination methods of cast superalloy material creep damage can not define for the part being used for a long time at high temperature
Whether its microscopic structure state can continue normal use to it, and there are certain risks.Therefore this method can be to part structural state
Accurate judgement, and then part service life can be made it is relatively accurate estimate, be not only avoided that cost waste, moreover it is possible in advance
Prevention causes bigger malfunction and failure due to part creep impairment, promotional value and market prospects with higher.
Summary of the invention
The object of the present invention is to provide a kind of microscopic detection methods for cast superalloy level of creep.
The present invention adopts the following technical scheme that realize:
A kind of microscopic detection method for cast superalloy level of creep, comprising the following steps:
1) preparation of sample
It is randomly selected in measuring samples several, sizeable sample is cut into, by the sample ultrasonic wave after cutting
It after cleaning removal surface and oil contaminant, then is inlayed, the side that the sample after inlaying is polished using automatic grind polishing or hand lapping
Formula handles sample, polish completion sample surfaces answer light, no marking, rounding, without not dragging tail, then wash with water, alcohol rushes
It washes, dry up；
The sample that polishing is completed, half are used for microexamination creep by 20% high fluoric acid alcoholic solution electrolytic etching
Cavity and micro-crack；The other half is used for microexamination γ ' phase by 10% phosphate aqueous solution electrolytic etching；
2) detection method
201) emptying hole and micro-crack are detected using optical metallographic microscope；Sample is looked first at, finds black color dots
After shape and linear display, then observe whether judgement display is Creep hole and micro-crack；Creep hole and micro-crack are along carbide
Or eutectic phase and matrix phase boundary edge open；
202) γ ' phase raftization is detected using optical metallographic microscope, and whether observation γ ' mutually grows up along same orientation,
If so, showing γ ' phase raft.
A further improvement of the present invention lies in that in step 1), by the sample after cutting with ultrasonic cleaning 5min~
10min。
A further improvement of the present invention lies in that in step 1), when 20% high fluoric acid alcoholic solution electrolytic etching, electric current 10A,
The electrolytic etching of 10 seconds time.
A further improvement of the present invention lies in that in step 201), first in X200 times of metallography microscope microscopic observation sample, hair
After the existing dotted and linear display of black, determine whether display is Creep hole and micro-crack in X500 times~X1000 times lower observation.
A further improvement of the present invention lies in that in step 202), X500 times~X1000 times lower observation γ ' mutually whether edge
Same orientation is grown up.
A further improvement of the present invention lies in that further including step 3) grade classification, by Creep hole and micro-crack, γ ' phase
Raftization is by slight, medium and serious three kinds of degree classifications.
A further improvement of the present invention lies in that being specifically classified as follows:
A) Creep hole and micro-crack of slight extent；
B) moderate Creep hole and micro-crack；
C) Creep hole and micro-crack of severity；
D) γ ' phase raft of slight extent；
E) moderate γ ' phase raft；
F) γ ' phase raft of severity.
The present invention has following beneficial technical effect:
The present invention can be used for all cast superalloy materials, and the scope of application is wider.It is compacted to have no cast superalloy at present
Become the microscopic detection method of degree of injury, this method has been filled up blank in this respect, can have been made to part structural state accurately
Determine, so part service life can be made it is relatively accurate estimate, effectively cost is avoided to waste, at the same prevent in advance due to
Part creep impairment and cause bigger malfunction and failure, reduce application risk, promotional value and market prospects with higher.
The present invention is used for the judgement of cast superalloy creep impairment degree, and makes to part service life relatively accurate
Estimate.The present invention is operated by above-mentioned experimental procedure, is determined part creep impairment degree, is estimated service life, with
Take corresponding measure.
Detailed description of the invention
Fig. 1 and Fig. 2 is respectively the dotted and linear display figure of black.
Fig. 3 and Fig. 4 is respectively Creep hole and micro-crack figure.
Fig. 5 is γ ' mutually normal microstructure figure.
Fig. 6 is γ ' phase raft microstructure figure.
Fig. 7 is the Creep hole and micro-crack figure of slight extent.
Fig. 8 is moderate Creep hole and micro-crack figure.
Fig. 9 is the Creep hole and micro-crack figure of severity.
Figure 10 is the normal microstructure figure of γ '.
Figure 11 is the γ ' phase raft figure of slight extent.
Figure 12 is moderate γ ' phase raft figure.
Figure 13 is the γ ' phase raft figure of severity.
Figure 14 is Creep hole figure.
Figure 15 is micro-crack figure.
Figure 16 is γ ' phase raft figure.
Specific embodiment
The present invention is made further instructions below in conjunction with drawings and examples.
A kind of microscopic detection method for cast superalloy level of creep provided by the invention, comprising the following steps:
1) preparation of sample
6 are randomly selected in measuring samples, are cut into sizeable sample, it is general using with cooling device and cutting heat
The lesser mode in the zone of influence cuts sample, and heat affected area should completely remove after cutting, and the section after cutting should hang down with face to be detected
Directly.
By the ultrasonic cleaning 5min~10min of the sample after cutting, after removing surface and oil contaminant, then inlayed, sample
Detection side is placed on as far as possible inlays mold center position, to guarantee that detection side is complete, avoids rounding.
Sample after inlaying handles sample by the way of automatic grind polishing or hand lapping polishing, and when grinding and polishing should be noted that
The integrality on protection detection side, avoids rounding.Polishing complete sample surfaces answer light, no marking, rounding, nothing do not drag tail, so
After wash with water, alcohol rinse, drying.
The sample that polishing is completed, 3 pass through 20% high fluoric acid alcoholic solution electrolytic etching, electric current 10A, 10 seconds time electricity
Solution corrosion, is used for microexamination Creep hole and micro-crack；Another 3, by 10% phosphate aqueous solution electrolytic etching, are used for micro-
Observe γ ' phase.
101) hand lapping polishes
It is recommended to use pre-grinding test sample of gold phase machine, is ground using P120, P320, P600, P1000 or P1200 sand paper, is ground every time
Mill should completely remove cutting and upper one of grinding damage, be rinsed with water with water lubrication, and after grinding clean；Then it is tried using metallographic
Sample polishing machine, on short flannel cloth successively with 5 μm, 2.5 μm of diamond polishing cream or with other equigranular polishing materials to examination
Sample is finally polished, and in polishing plus water lubrication, is then rinsed with water, with drying up after alcohol rinse.
102) automatic grind polishing
The symmetrical clamping of sample will be inlayed on sample holder disk, with the smoothing of pressure weighing apparatus, clamped, it is ensured that grinding surface is in same water
Plane；Using automatic grinding and polishing device, sample preparation parameter can refer to standard ASTM E3, and when preparation should be noted that sand paper turntable and sample
Clamping disk rotating Vortex, every time grinding replacement sand paper when be rinsed with water abrasive disk fall off sand grains, polishing cloth select non-felt；Preparation
After the completion, it is rinsed with water, dried up after alcohol rinse.
2) detection method
201) emptying hole and micro-crack are detected using optical metallographic microscope.In X200 times of metallography microscope microscopic observation
Sample after finding the dotted and linear display of black as depicted in figs. 1 and 2, determines that display is in X500 times~X1000 times lower observation
No is Creep hole and micro-crack.Creep hole and micro-crack are opened along carbide or eutectic phase and matrix phase boundary edge, such as Fig. 3
With shown in Fig. 4.
202) γ ' phase raftization is detected using optical metallographic microscope.In X500 times~X1000 times lower observation γ ' phase
Whether grow up along same orientation, as shown in Figure 5, Figure 6.Fig. 6 shows γ ' phase raft.
3) grade classification
By Creep hole and micro-crack, γ ' phase raftization by slight, medium and serious three kinds of degree classifications.
A) Creep hole and micro-crack of slight extent, as shown in Figure 7.
B) moderate Creep hole and micro-crack, as shown in Figure 8.
C) Creep hole and micro-crack of severity, as shown in Figure 9.
Mutually normal microstructure is as shown in Figure 10 by γ '.
D) γ ' phase raft of slight extent, as shown in figure 11.
E) moderate γ ' phase raft, as shown in figure 12.
F) γ ' phase raft of severity, as shown in figure 13.
Embodiment
After the turbo blade use of DZ125 directional casting high-temperature alloy material, for creep impairment deciding degree, tool
Body implementation steps are as follows:
(1) sample is prepared
6 blades are extracted, sizeable sample is cut into, with ultrasonic cleaning 10min, sample detection side is placed on and is inlayed
It is inlayed the center of mould.
Sample after inlaying carries out the sand of P120, P320, P600 and P1200 by the way of hand lapping polishing respectively
Paper grinding, sample are rinsed with water completely；Then metallographic-sample polisher is used, successively with 5 μm, 2.5 μm of gold on short flannel cloth
Hard rock antiscuffing paste finally polishes sample, final rinse water, with drying up after alcohol rinse.
The sample that polishing is completed, 3 pass through 20% high fluoric acid alcoholic solution electrolytic etching, electric current 10A, 10 seconds time electricity
Solution corrosion, is used for microexamination Creep hole and micro-crack；Another 3, by 10% phosphate aqueous solution electrolytic etching, are used for micro-
Observe γ ' phase.
(2) it detects
Optical microphotograph sem observation, there are Creep hole and micro-cracks for sample, as shown in Figure 14 and Figure 15.
Optical microphotograph sem observation, sample γ ' phase raft, as shown in figure 16.
(3) classify
On inspection, by Creep hole, micro-crack and the γ ' phase raft of inspection turbo blade discovery severity.
It is required according to turbo blade relevant criterion, there is the Creep hole more than slight extent, micro-crack and γ ' phase raft
Change, needs to change blade.
Claims (10)
1. a kind of microscopic detection method for cast superalloy level of creep, which comprises the following steps:
1) preparation of sample
It is randomly selected in measuring samples several, sizeable sample is cut into, by the sample ultrasonic cleaning after cutting
It after removing surface and oil contaminant, then is inlayed, the sample after inlaying is by the way of automatic grind polishing or hand lapping polishing
Manage sample, polish completion sample surfaces answer light, no marking, rounding, nothing do not drag tail, then wash with water, alcohol rinse, blow
It is dry；
The sample that polishing is completed, half are used for microexamination Creep hole by 20% high fluoric acid alcoholic solution electrolytic etching
And micro-crack；The other half is used for microexamination γ ' phase by 10% phosphate aqueous solution electrolytic etching；
2) detection method
201) emptying hole and micro-crack are detected using optical metallographic microscope；Look first at sample, discovery black it is dotted and
After linear display, then observe whether judgement display is Creep hole and micro-crack；Creep hole and micro-crack are along carbide or altogether
Crystal phase and matrix phase boundary edge open；
202) γ ' phase raftization is detected using optical metallographic microscope, and whether observation γ ' mutually grows up along same orientation, if
It is to show γ ' phase raft.
2. a kind of microscopic detection method for cast superalloy level of creep according to claim 1, feature exist
In in step 1), by the ultrasonic cleaning 5min~10min of the sample after cutting.
3. a kind of microscopic detection method for cast superalloy level of creep according to claim 1, feature exist
In, in step 1), when 20% high fluoric acid alcoholic solution electrolytic etching, electric current 10A, the electrolytic etching of 10 seconds time.
4. a kind of microscopic detection method for cast superalloy level of creep according to claim 1, feature exist
In first in X200 times of metallography microscope microscopic observation sample, being confirmed whether there is the dotted and linear display of black in step 201).
5. a kind of microscopic detection method for cast superalloy level of creep according to claim 4, feature exist
In showing whether be Creep hole and micro- in X500 times~X1000 times lower observation judgement after finding the dotted and linear display of black
Crackle.
6. a kind of microscopic detection method for cast superalloy level of creep according to claim 1, feature exist
In in step 202), whether observation γ ' mutually grows up along same orientation under X500 times~X1000 times.
7. a kind of microscopic detection method for cast superalloy level of creep according to claim 1, feature exist
In in step 202), whether observation γ ' mutually grows up along same orientation under X500 times.
8. a kind of microscopic detection method for cast superalloy level of creep according to claim 1, feature exist
In in step 202), whether observation γ ' mutually grows up along same orientation under X1000 times.
9. a kind of microscopic detection method for cast superalloy level of creep according to claim 1, feature exist
In further including step 3) grade classification, by Creep hole and micro-crack, γ ' phase raftization by slight, medium and serious three kinds of degree
Classification.
10. a kind of microscopic detection method for cast superalloy level of creep according to claim 9, feature exist
In being specifically classified as follows:
A) Creep hole and micro-crack of slight extent；
B) moderate Creep hole and micro-crack；
C) Creep hole and micro-crack of severity；
D) γ ' phase raft of slight extent；
E) moderate γ ' phase raft；
F) γ ' phase raft of severity.
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Cited By (3)
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| CN110806357A (en) * | 2019-11-13 | 2020-02-18 | 中国石油大学(华东) | Method for evaluating high-temperature creep damage based on low-temperature fracture |
| CN111272506A (en) * | 2020-02-28 | 2020-06-12 | 鞍钢股份有限公司 | Preparation method of metallographic sample of oriented silicon steel continuous casting billet |
| CN112903385A (en) * | 2021-01-19 | 2021-06-04 | 大冶特殊钢有限公司 | Preparation method of high-temperature alloy metallographic specimen |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110806357A (en) * | 2019-11-13 | 2020-02-18 | 中国石油大学(华东) | Method for evaluating high-temperature creep damage based on low-temperature fracture |
| CN111272506A (en) * | 2020-02-28 | 2020-06-12 | 鞍钢股份有限公司 | Preparation method of metallographic sample of oriented silicon steel continuous casting billet |
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| CN112903385A (en) * | 2021-01-19 | 2021-06-04 | 大冶特殊钢有限公司 | Preparation method of high-temperature alloy metallographic specimen |
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Application publication date: 20190115 |