CN107515233A - A kind of method of fusion temperature detection high-entropy alloy segregation using heat analysis measure - Google Patents
A kind of method of fusion temperature detection high-entropy alloy segregation using heat analysis measure Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 86
- 239000000956 alloy Substances 0.000 title claims abstract description 86
- 238000005204 segregation Methods 0.000 title claims abstract description 69
- 238000004458 analytical method Methods 0.000 title claims abstract description 35
- 230000004927 fusion Effects 0.000 title claims abstract description 32
- 238000001514 detection method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000000113 differential scanning calorimetry Methods 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000004455 differential thermal analysis Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 31
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 11
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 9
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- 238000005259 measurement Methods 0.000 description 7
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- 238000004453 electron probe microanalysis Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
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- 241001269238 Data Species 0.000 description 2
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- 239000000243 solution Substances 0.000 description 2
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- 238000002076 thermal analysis method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
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- 229910052729 chemical element Inorganic materials 0.000 description 1
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Abstract
The present invention relates to a kind of method of the fusion temperature detection high-entropy alloy segregation using heat analysis measure, belong to material and metallurgical engineering technical field.The method being segregated using the fusion temperature detection high-entropy alloy of heat analysis measure, using the fusion temperature of heat analysis measure high-entropy alloy sample, and subtract each other with the fusion temperature of standard sample, the temperature deviation calculated, when temperature deviation exceedes allowed band, it was demonstrated that the segregation zones of high-entropy alloy product are above standard scope.The present invention uses fusing peak temperature, initial temperature and the final temperature of differential scanning calorimetry high-entropy alloy, comparatively the sample of heat analysis belongs to bulk sample, test is overall performance, if sample interior has part segregation, regardless of whether it is located at surface, or whether the metallographic contrast of segregation is obvious, the skew of fusing peak value, liquidus temperature and solid-state temperature can be all reflected, the segregation of high-entropy alloy can be detected exactly.
Description
Technical field
The present invention relates to a kind of method of the fusion temperature detection high-entropy alloy segregation using heat analysis measure, belong to material
With metallurgical engineering technical field.
Background technology
Conventional alloys be one or two kinds of metals as parent metal, add other elements on a small quantity（Addition generally exists
Below 5at%）.High-entropy alloy is more than four kinds metallic element equimolar mixing, forms the stabilization for there was only a phase or two phases and consolidates
Solution, because after the mixing of multiple element equimolar, the entropy of mixing of whole alloy system is very big, and system randomness is very high, therefore surely
It is qualitative high, so gaining the name " high-entropy alloy ".It is wherein most representational to be：Cr20Mn20Fe20Co20Ni20(at%) FCC faces
The heart cube individual event alloy.Subsequent scientists develop the high-entropy alloy of two-phase on the basis of single-phase high-entropy alloy, such as
Fe80-xMnxCo10Cr10(at%) part HCP martensitic phases are uniformly separated out on FCC matrixes.
The great advantage of high-entropy alloy be exactly in high temperature and low temperature environment can holding structure it is stable, so as to retention property
It is stable, it is to prepare the preferred material in extreme environment, such as manufacture aviation/space flight jet engine turbo blade, therefore pairing
Golden uniformity requirement is high, it is impossible to has small segregation.But F.Otto et al.[1]To CrMnFeCoNi, complete 500 days 900
DEG C high temperature test after point out, such high entropy is also easily segregated in extreme operating environments, therefore is also needed to high-entropy alloy
Further investigate.Therefore, the technology of the small segregation of high-entropy alloy can be detected by, which finding, seems particularly significant.
According to the distribution situation of chemical composition, segregation can be divided into two kinds:The first is macroscopical chemistry segregation, can be passed through
Chemical analysis is sampled, and is readily available scanning electron microscope sem observation, EDX energy disperse spectroscopies and atom-probe EPMA easy to use
Surface scan/line scanning survey segregation bandwidth.Second of segregation is microcosmic faint segregation, can not be by sampling chemical analysis.
And the metallographic contrast of small segregated zone is very faint, it is difficult to be observed by scanning electron microscope sem, EDX and EPMA face are also increased
The difficulty of scanning/line scanning measurement.Spot segregation is common microsegregation, can be observed with SEM.
For microsegregation, EDX and EPMA microscopic analyses must pass through ESEM（SEM）The image of segregation is found, it is right
In high-entropy alloy, the small segregation of many as-cast structures can only occur in the range of very little, if metallographic sample preparation does not select
To the cross section of segregation, it is then not possible to which, it was observed that segregation phenomena, reason has two：The Elemental Concentration difference very little of segregation, point
Distinguish that the EDX equipment of ability can not distinguish Elemental redistribution difference, face surface sweeping and line scanning can not measure concentration difference；Or partially
Cause micro-imaging difficult, the micro-image that can not find segregation also just can not be complete without obvious micro- contrast difference in analysis part
Analyzed into EPMA, therefore the uniform conclusion of high-entropy alloy composition obtained with microcosmic microscopic analysis may be inaccurate.
The thermal conductance of metal is fine, when measuring the fusion temperature of alloy sample using heat analysis, sample quality and purge gass
Flow is all without peak temperature, the fusing initial temperature for significantly affecting melting hump（Solid-state temperature）And final temperature（Liquid phase temperature
Degree）, but heat analysis measurement process is to measure the thermodynamic parameter of sample, the melting hump of most of crystal in dynamic state
Value, liquidus temperature and solid-state temperature are significantly affected by heating rate, and slower heating rate is closer to poised state, measurement
Value is more accurate.The fusing activation of common alloy and crystalline solid can be higher, and fusion temperature is influenceed by heating rate mostly, therefore
Wanting measure fusing peak temperature needs very slow heating rate to make every effort to close to poised state, but heating rate can cause very much partially slowly
The fuel factor unobvious of analysis, therefore the method for melting peak temperature, liquidus temperature and solid-state temperature point of measure alloy can not be used
Analysis segregation, there is no document and technology to be segregated by determining alloy melting temperature detection in the past yet.
But the fusing peak temperature liquidus temperature and the thermal behavior of solid-state temperature and common alloy of high-entropy alloy and different,
Because the entropy of mixing of high-entropy alloy is bigger than conventional alloys, some special dynamic characteristics are shown, such as high-entropy alloy
Fusing activation can very little, in the range of 2~100 DEG C/min heating rate, heating rate is to fusing peak value and liquidus temperature
Influence to be less than 5 DEG C, and influenceed caused by being segregated more than 70 DEG C, it is believed that the now fusing peak value and liquidus temperature of high-entropy alloy
Only influenceed by segregation without being influenceed by heating rate, thus can with the fusing peak value of comparative sample and uniform standard sample or
Liquidus temperature, clearly and succinctly detects segregation defects, and DSC curve is a kind of simple, accurate and cheap analysis method, Ke Yizhun
Fusing peak value, liquidus temperature and the solid-state temperature of true determination sample.
[1]F Otto, A Dlouhý, KG Pradeep, Decomposition of the single-phase
high-entropy alloy CrMnFeCoNi after prolonged anneals at intermediate
temperatures, Volume 112, 15 June 2016, P40–52.
[2]Mathilde Laurent-Brocq, Alfiya Akhatova, Loı¨c Perrie`re,Insights into
the phase diagram of the CrMnFeCoNi high entropy alloy, Acta Materialia,
(2015,p355–365.
[3]Mathilde Laurent-Brocq, Alfiya Akhatova, Loı¨c Perrie`re,Insights into
the phase diagram of the CrMnFeCoNi high entropy alloy, Acta Materialia,
(2015,p355–365。
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of fusing temperature determined using heat analysis
The method of degree detection high-entropy alloy segregation.The present invention is achieved through the following technical solutions.
A kind of method of fusion temperature detection high-entropy alloy segregation using heat analysis measure, high entropy is determined using heat analysis
The fusion temperature of alloy sample, and subtract each other with the fusion temperature of standard sample, the temperature deviation calculated, when temperature deviation exceedes
Allowed band, it was demonstrated that the segregation zones of high-entropy alloy product are above standard scope.
The heat analysis includes differential thermal analysis or differential scanning calorimetry.
The fusion temperature is start temperature, peak temperature or the final temperature of melting hump.
The allowed band is the 3.5% of standard sample fusion temperature.
The high-entropy alloy sample quality is 1~500mg.Fusing peak temperature is easy to identify, easily measured, using peak value
During temperature analysis sample, after sample size is more than 500mg, fusing peak temperature is influenceed too greatly, to cause peak temperature not only by thermal boundary
Influenceed by segregation, also influenceed by sample quality.Comparatively fusing initial temperature is not easy to be influenceed by sample quality, but is not easy to know
Not, although can improve measurement accuracy using extrapolation, measured deviation is still very big.
The temperature deviation and segregation bandwidth that the present invention is obtained correspond, and different segregation species has different correspondences
Relation.
The beneficial effects of the invention are as follows：The present invention uses the fusing peak temperature of differential scanning calorimetry high-entropy alloy, risen
Comparatively beginning temperature and final temperature, the sample of heat analysis belong to bulk sample, test is overall performance, if sample
There is part segregation inside, regardless of whether it is located at surface, or whether the metallographic contrast of segregation is obvious, can all reflect melting hump
The skew of value, liquidus temperature and solid-state temperature, can detect the segregation of high-entropy alloy exactly.
Brief description of the drawings
Fig. 1 is the Cr that the embodiment of the present invention 1 has small segregation20Mn20Fe20Co20Ni20High-entropy alloy as cast condition and uniform formation
DSC curve figure；
Fig. 2 is the Cr that the embodiment of the present invention 1 has small segregation20Mn20Fe20Co20Ni20The as cast condition XRD of high-entropy alloy；
Fig. 3 is the Cr that the embodiment of the present invention 1 has small segregation20Mn20Fe20Co20Ni20The as cast condition SEM figures of high-entropy alloy；
Fig. 4 is the Cr that the embodiment of the present invention 1 has small segregation20Mn20Fe20Co20Ni20The EDX spot scan figures of high-entropy alloy；
Fig. 5 is the Cr that the embodiment of the present invention 2 has spot segregation20Mn20Fe20Co20Ni20The DSC curve of high-entropy alloy and homogeneous state
Figure；
Fig. 6 is the Cr that the embodiment of the present invention 2 has spot segregation20Mn20Fe20Co20Ni20High-entropy alloy SEM image；
Fig. 7 is the Cr that the embodiment of the present invention 2 has spot segregation20Mn20Fe20Co20Ni20The as cast condition XRD of high-entropy alloy.
Embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
The method being segregated using the fusion temperature detection high-entropy alloy of heat analysis measure：Using fusing peak value temperature detection
Cr20Mn20Fe20Co20Ni20The small segregation of high-entropy alloy, microcell segregation refer to the small segregation that occurs in micro-scale, can be with
With SEM, it was observed that, but contrast difference is smaller, is not easy to use EDX analysis measurements.
First using the CrMnFeCoNi high-entropy alloys of cold crucible magnetic suspension stove configuration, CrMnFeCoNi high-entropy alloy as cast conditions
The chemical analysis and Portable X RF analyze datas of tissue are as shown in table 1.The data obtained from table 1 can be seen that chemical composition
Inhomogeneities be less than 0.7%, less than most of document large deviations value, it is believed that chemical composition uniformity is fine.
Table 1
By Cr20Mn20Fe20Co20Ni20High-entropy alloy is surveyed using the synchronous solving NETZSCH STA 449F3 of Nai Chi companies
The DSC curve of amount, detailed process are：Cr20Mn20Fe20Co20Ni20High-entropy alloy sample quality is 45mg, pure Ar purge gass speed
30mL/min, heating rate are 20 DEG C/min, obtain Cr20Mn20Fe20Co20Ni20High-entropy alloy DSC curve, data analysis process
It can be completed by the NETZSCH-Proteus of software Origin and Nai Chi companies.
The Cr that the present embodiment obtains20Mn20Fe20Co20Ni20High-entropy alloy DSC curve and document Plays
Cr20Mn20Fe20Co20Ni20High-entropy alloy DSC curve is as shown in figure 1, as can be seen from Figure 1 the present embodiment
Cr20Mn20Fe20Co20Ni20High-entropy alloy fusing peak value is 1342.3 DEG C, the Cr of standard20Mn20Fe20Co20Ni20High-entropy alloy melts
It is 1405.3 DEG C to change peak value, and the temperature deviation value that both subtract each other to obtain is 63 DEG C, and temperature deviation value is standard sample fusion temperature
4.5%, more than allowed band be standard sample fusion temperature 3.5%, so proving the segregation zones of the high-entropy alloy product
Be above standard scope.
The result of the present embodiment is verified：
The Cr that embodiment is obtained20Mn20Fe20Co20Ni20High-entropy alloy carries out XRD detections, obtains as cast condition XRD such as Fig. 2 institutes
Show, the Cr that as can be seen from Figure 2 the present embodiment obtains20Mn20Fe20Co20Ni20High-entropy alloy as cast condition and document[1]In it is uniform
The XRD picture of tissue does not have near a little gaps, such as 43 degree of 2 θ angles（111）, near 50 degree（200）, near 75 degree
（220）, near 90 degree（311）The diffraction maximum of crystal orientation all with document[2]Value, which is consistent, belongs to single phase solid solution fcc, and XRD is shown
Seem Cr20Mn20Fe20Co20Ni20Segregation is not present in the institutional framework of high-entropy alloy as cast condition sample.
The Cr that embodiment is obtained20Mn20Fe20Co20Ni20High-entropy alloy carries out SEM figure detections, is directly observed using SEM
As cast condition sample metallographic, it is observed that from SE+EDX patterns in Fig. 3 and is generally dispersed with bulk defect, during using EDX spot scan
Fig. 4 is obtained, Mn is 27at%, Cr20at%, Fe15at%, Co17at%, Ni21at% in bulk defect as can be seen from Figure 4, and Mn is first
Plain obvious increase, Fe and Co elements are reduced, and there occurs obvious segregation, therefore bulk defect confirmation is small segregation, but because
Very faint for Elemental redistribution deviation, EDX Surface scans can not clearly distinguish the profile of segregation, can only measure maximum by A points from Fig. 3
Segregation bandwidth ≈ 0.01mm, the temperature deviation value that the present embodiment obtains be standard sample fusion temperature 4.5%, it is believed that
When fusion temperature deviation>When 4.5%, maximum small segregated zone ≈ 0.01mm.
Embodiment 2
The method being segregated using the fusion temperature detection high-entropy alloy of heat analysis measure：Using fusing peak value temperature detection
Cr20Mn20Fe20Co20Ni20Whether high-entropy alloy has spot segregation.Spot segregation refers to by chemical composition analysis and XRF
Spectrum（XRF）It is not easy the microcosmic part differentiated（Such as crystal boundary, cavity）The segregation in region.
The Cr that embodiment 1 is prepared20Mn20Fe20Co20Ni20High-entropy alloy as-cast structure is in 1000 DEG C of high temperings 2
Hour, then water quenching obtains spot segregation tissue, and spot segregation tissue is shown using chemical analysis and Portable X RF analyze datas
The inhomogeneities of chemical composition is less than 0.7%, detects data and the difference very little of table 1.
By the Cr of the present embodiment spot segregation20Mn20Fe20Co20Ni20High-entropy alloy uses the simultaneous thermal analysis of Nai Chi companies
The DSC curve of instrument NETZSCH STA 449F3 measurements, detailed process are：Cr20Mn20Fe20Co20Ni20High-entropy alloy sample quality
Respectively 80mg, 40mg, 50mg, pure Ar purge gass speed 30mL/min, heating rate are 20 DEG C/min, are obtained
Cr20Mn20Fe20Co20Ni20High-entropy alloy DSC curve, data analysis process can be by software Origin and Nai Chi companies
NETZSCH-Proteus is completed.
The Cr that the present embodiment obtains20Mn20Fe20Co20Ni20High-entropy alloy DSC curve and document Plays
Cr20Mn20Fe20Co20Ni20High-entropy alloy DSC curve is as shown in figure 5, as can be seen from Figure 5 the present embodiment
Cr20Mn20Fe20Co20Ni20High-entropy alloy fusing peak value is 1335.5 ± 6.8 DEG C（In the measurement range of common thermal-analysis instrumentation
Peak temperature change is limited in 7 DEG C）, the Cr of standard20Mn20Fe20Co20Ni20High-entropy alloy fusing peak value is 1409 DEG C, both
The temperature deviation value for subtracting each other to obtain is 74 DEG C, and temperature deviation value is the 5.3% of standard sample fusion temperature, is more than allowed band
The 3.5% of standard sample fusion temperature, so proving that the segregation zones of the high-entropy alloy product are above standard scope.
The result of the present embodiment is verified：
The Cr that the present embodiment is obtained20Mn20Fe20Co20Ni20High-entropy alloy carries out XRD detections, and XRD is as shown in fig. 7, from Fig. 7
In can be seen that the Cr that embodiment obtains20Mn20Fe20Co20Ni20High-entropy alloy with it is uniform in Fig. 2 and document of embodiment 1
Tissue XRD picture has the diffraction maximum near some gaps, such as 35 degree of 2 θ angles to differ markedly from document and as-cast structure, it was demonstrated that partially
Analysis is not belonging to the face-centred cubic structure of high-entropy alloy requirement,（111）、（220）、（311）The diffraction maximum and literature value of crystal orientation[3]Phase
Together, illustrate that spot segregation can be found by XRF existing for high tempering sample.Fig. 6 is the SEM metallographics of spot segregation, segregation
At the defects of being generally focused on crystal boundary, hole, deviation is fairly obvious, and chemical element distribution and institutional framework all differ with matrix
Cause, contrast difference is more than 50%, it is easy to by SEM it was observed that the metallographic structure of segregation, is also easy to complete using EDX and EPMA
Into Surface scan and line scanning probe to the size of segregated zone.
What is obtained in Fig. 6 goes out maximum segregation bandwidth ≈ 0.001mm, and the temperature deviation value of the present embodiment melts for standard sample
The 5.3% of temperature, it is believed that when fusion temperature deviation>When 5.3%, maximum spot segregation band ≈ 0.001mm..
Above in association with accompanying drawing to the present invention embodiment be explained in detail, but the present invention be not limited to it is above-mentioned
Embodiment, can also be before present inventive concept not be departed from those of ordinary skill in the art's possessed knowledge
Put that various changes can be made.
Claims (5)
1. a kind of method of fusion temperature detection high-entropy alloy segregation using heat analysis measure, it is characterised in that：Using heat point
The fusion temperature of analysis measure high-entropy alloy sample, and subtract each other with the fusion temperature of standard sample, the temperature deviation calculated, work as temperature
Degree deviation exceedes allowed band, it was demonstrated that the segregation zones of high-entropy alloy product are above standard scope.
2. the method for the fusion temperature detection high-entropy alloy segregation according to claim 1 using heat analysis measure, it is special
Sign is：The heat analysis includes differential thermal analysis or differential scanning calorimetry.
3. the method for the fusion temperature detection high-entropy alloy segregation according to claim 1 using heat analysis measure, it is special
Sign is：The fusion temperature is start temperature, peak temperature or the final temperature of melting hump.
4. the method for the fusion temperature detection high-entropy alloy segregation according to claim 1 using heat analysis measure, it is special
Sign is：The allowed band is the 3.5% of standard sample fusion temperature.
5. the method for the fusion temperature detection high-entropy alloy segregation according to claim 1 using heat analysis measure, it is special
Sign is：The high-entropy alloy sample quality is 1~500mg.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113030166A (en) * | 2021-03-12 | 2021-06-25 | 哈尔滨工业大学 | Measuring device for semi-solid rheological behavior of high-entropy alloy and using method thereof |
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2017
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113030166A (en) * | 2021-03-12 | 2021-06-25 | 哈尔滨工业大学 | Measuring device for semi-solid rheological behavior of high-entropy alloy and using method thereof |
| CN113030166B (en) * | 2021-03-12 | 2022-09-23 | 哈尔滨工业大学 | Measuring device for semi-solid rheological behavior of high-entropy alloy and using method thereof |
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Application publication date: 20171226 |