CN105181727A - Identification method of axle workpiece fracture failure crack initiation - Google Patents
Identification method of axle workpiece fracture failure crack initiation Download PDFInfo
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- CN105181727A CN105181727A CN201510595884.4A CN201510595884A CN105181727A CN 105181727 A CN105181727 A CN 105181727A CN 201510595884 A CN201510595884 A CN 201510595884A CN 105181727 A CN105181727 A CN 105181727A
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Abstract
The invention discloses an identification method of axle workpiece fracture failure crack initiation. The identification method comprises the following steps: (1) pretreating a sample, namely cutting the sample, cleaning the fracture of the sample, and protecting the surface of the fracture from being damaged; and (2) carrying out back scattering image acquisition on the fracture of the sample by utilizing an electronic probe X ray microscopic analyzer; carrying out wave spectrum element qualitative analysis on regions with different gray levels reflected by a back scattering image, thus determining the main components of different characteristic regions of the surface nearby the fracture crack initiation region; carrying out micro-domain element distribution analysis on the suspected crack initiation position of the surface of the fracture according to the back scattering image and the element qualitative analysis; and identifying the accurate position and the reason of the crack point of the fracture according to the back scattering image and the ion element distribution analysis result of the fracture of the workpiece. According to the identification method, the position of the crack initiation of the surface of the fracture can be accurately distinguished; the element segregation or inclusion defects at the crack initiation position of the surface of the fracture can be clearly reflected, so that the reason of the crack initiation can be judged.
Description
Technical field
The present invention relates to a kind of engineering key member Analysis of Fracture Failure method, particularly relate to a kind of recognition methods of shaft-like workpiece fracture failure formation of crack.
Background technology
Shaft-like workpiece is the important component in kinematic train.The fracture failure of such workpiece can cause the fault of whole machine usually.Especially for main equipment, the fracture failure of shaft-like workpiece may cause serious accident.Therefore, failure analysis is carried out to the shaft-like workpiece of fracture, and proposes measure on this basis, prevent the generation of this type of accident, to the qualification of failure accidents reason, accident prevention, ensure that industrial normal operation etc. has important function and significance.Because shaft-like workpiece can be subject to the effect (being generally alternating bending and torsional load) of alternate load in normal conditions, the fatigue break caused by this class load becomes the modal a kind of failure mode of shaft-like workpiece.Fatigue break was lost efficacy, and referred to that workpiece is under the repeated action of alternate load, at nominal stress far below the behavior that rupture failure occurs when material yield strength.Fatigue Failure Process generally comprises crack initiation, Crack Extension and last hit three phases, is that a kind of accumulated damage destroys.A knick point of fatigue crack is often positioned at the fault location of surface of the work (conventional cycle fatigure failure) or inner (super high cycle fatigue destruction), discriminating to workpiece fracture failure basic reason is related to the analysis in the type inefficacy workpiece crack source, because of but important step in failure analysis.But due in crack propagation process, workpiece keeps running status, the antithesis section of fracture can grind mutually, make crackle source region under normal circumstances occur serious grinding marks, thus cover the vestige that crackle expands at first, make the accurate location of formation of crack be difficult to differentiate.
At present, in the failure analysis field of shaft-like workpiece, check that the technological means of fracture is generally and rely on scanning electron microscope (Scanningelectronmicroscope, the ultimate analysis of secondary electron image SEM) and energy dispersion X ray spectrum (EnergydispersiveX-rayspectroscopy, EDS).The combination of two kinds of technology can realize the judgement to fracture breaking property preferably.Secondary electron image can present the microscopic appearance that sample surfaces has height to rise and fall clearly, (such as, is rock-candy structure or plastic fracture to the judgement of fracture character; Grain boundary fracture or transgranular fracture etc.) there is very important effect.But for subjected to the crackle source region of grinding damage, its microscopic appearance feature that surface height rises and falls originally is polished all, has been difficult to by secondary electron image the accurate location tracking formation of crack.Energy dispersion X ray spectrum can assist analytical review to shaft-like workpiece fracture from the angle of ultimate analysis.If the crackle source region of fracture is by the segregation of element and the phenomenon such as is mingled with and causes, then can be distinguished by ultimate analysis, to find the basic reason causing this type of workpiece to rupture.But, the resolution of spectroscopy detection device is lower, be about 160eV, and the measurement of ultra-light elements because of the beryllium window limit of Si (Li) detecting device in energy spectrometer, therefore analysis result atomic number being less than to the element such as carbon (C), nitrogen (N), oxygen (O) of 11 is inaccurate, and these elements element that snotter contains in shaft-like workpiece often.Therefore, rely on secondary electron image and power spectrum ultimate analysis well cannot determine the position in shaft-like workpiece fatigue break fracture crack source and crack the reason in source, this is key issue to be solved by this invention just.
Document " Fatigue-Fracture Mechanism of Main Bearing Cage for Aircraft Engine " can only provide doubtful crackle source region from the secondary electron image of workpiece fracture, is difficult to the accurate location finding formation of crack.Document " analysis of 35CrMo Tempered Gear bending fatigue broken tooth failure " can only provide doubtful crackle source region from the macro morphology picture of workpiece fracture and secondary electron image, is difficult to the accurate location finding formation of crack.Though indicate in literary composition that formation of crack place exists snotter and provides EDS ultimate analysis to prove, but do not show the position of snotter existence intuitively.
In sum, the accurate location differentiating shaft-like workpiece fracture surface crackle source region does not also have effective scheme, and development more effectively, intuitively method to differentiate the accurate location in shaft-like workpiece fracture surface crackle source region and to analyze its producing cause, not only there is necessity but also there is urgency.
In prior art, nobody utilizes electro probe-X-ray microanalysis to identify shaft-like workpiece fracture failure formation of crack; our known electron probe utilizes the high-power electron beam bombardment solid surface focused on; the element by bombarding is made to inspire characteristic X-ray; qualitative and quantitative chemical analysis is carried out by its wavelength and intensity and solid surface microcell; be mainly used to fine particle or the tiny area of analyzing solid surface, have bigger difference with workpiece fracture crack identifing source.In addition, the instrumental method can analyzing fracture in prior art is a lot, those skilled in the art are difficult to electron probe and the identification of workpiece fracture failure formation of crack to connect, one is because nobody utilizes electron probe to carry out similar test, two is because those skilled in the art cannot predict the effect in this instrument identification workpiece fracture crack source, different classes of material demand arranges different conditions of work, also must carry out a series of correction, correctly could measure the content of element.The Accurate Determining of various parameter, the accuracy of last recognition result can be ensured, and the mensuration process need inventor of various parameter relies on the experience of its years of work constantly to be revised, continuous exploration, best measuring condition could be determined, this needs to pay creative work, and institute is not apparent with the inventive method.
Beneficial effect of the present invention is:
1, electron probe (electro probe-X-ray microanalysis (ElectronProbeMicroanalyzer, EPMA)) fine focusing electron beam can be utilized, the characteristic X-ray of element is excited in the microcell of sample top layer, according to wavelength and the intensity of characteristic X-ray, carry out the qualitative or quantitative test of micro-area chemical.Its resolution exceeds at least one order of magnitude than energy spectrum analysis, and especially electron probe is to the measurement of ultra-light elements without any restriction, and it can measure atomic number from all elements between 4 to 92.If again in conjunction with the backscatter images of fracture, then can reach the accurate judgement to shaft-like workpiece fracture crack source position and producing cause.
2, the ultimate analysis of electron probe and the combination of backscatter images can reflect the information in the formation of crack region of shaft-like workpiece fracture well.Backscatter images is by backscattered electron imaging, and backscattered electron refers to a part of incident electron reflected by solid sample atom, comprising elasticity backscattered electron and non-resilient backscattered electron.The quantity of backscattered electron increases with the increase of atomic number, so, utilize backscattered electron can not only analyze shape characteristic as imaging signal, also can be used for tracer atom ordinal number contrast, carry out qualitative constituent analysis.
3, because the formation of crack of fracture shaft-like workpiece fracture surface often exists element aggregation, the defect such as to be mingled with, electron probe is utilized to carry out element Surface scan to crackle source region, clearly can differentiate the accurate location in fracture crack source, and can help to judge formation of crack Producing reason.
Summary of the invention
The present invention, in order to solve Shortcomings in prior art, provides a kind of recognition methods of shaft-like workpiece fracture failure formation of crack, and that it has is accurate, clear, intuitively, do not damage sample and operate easy advantage.
To achieve these goals, technical scheme of the present invention is:
Electron probe X-ray microanalysis method is detecting the application in shaft-like workpiece fracture failure formation of crack.
A recognition methods for shaft-like workpiece fracture failure formation of crack, comprises the steps:
1) sample pre-treatments: after cutting sample, cleans sample fracture, and protection fracture surface is not destroyed;
2) electro probe-X-ray microanalysis is utilized to carry out backscatter images collection to sample fracture; Wave spectrum qualitative elementary analysis is carried out in the region that the gray scale reflected backscatter images is different, determines that fracture plays the principal ingredient in surperficial different characteristic region near split plot; According to backscatter images and qualitative elementary analysis result, microregion element surface analysis is carried out to the doubtful crack initiation zone position of fracture surface; According to backscatter images and the element surface analysis result of workpiece fracture, identify that fracture plays accurate location and the producing cause of knick point.
Preferably, step 1) in, the thickness of pretreated sample is 10-15mm, the length of sample and be widely all less than 50mm.The sample of well cutting can be placed on the monitor station of instrument, convenient detection.
Preferably, step 1) in, to the method that sample fracture cleans, comprise the steps: first to carry out ultrasonic cleaning 10-15min with organic solvent to fracture surface.Fracture after cleaning more easily identifies.
Preferred further, if sample fracture surface is corroded, after fracture being cleaned with organic solvent, then use 2-5% watery hydrochloric acid, Ultrasonic Cleaning 1-3min, when the corrosion product of fracture surface many places is cleaned, stops cleaning, carry out fracture surface examination; If cleaning performance is not obvious, then uses 6-10% watery hydrochloric acid instead and clean.
If fracture surface is corroded, when corrosion product is cleaned, all for fracture surface corrosion products all can not be cleaned up, because if thoroughly cleaned up by corrosion product, then the microscopic feature of fracture surface is totally disrupted, can not reach the object of formation of crack identification.
Shaft-like workpiece, owing to needing the protection of lubricating oil under its nominal situation, can cause fracture surface to be subject to the pollution of oily substance after fracture.After this, fracture surface is placed in atmosphere owing to exposing, and surface is very easy to the pollution being subject to dust-like material.Have in the atmospheric environment of corrosive elements if be in, fracture surface also can be corroded destruction, and this adds difficulty to the identification of fracture surface formation of crack undoubtedly.So cleaned fracture surface before fracture surface examination.
Preferably, step 2) in, the condition of work of electro probe-X-ray microanalysis is: filament current: 28 ~ 35 μ A; Accelerating potential: 10 ~ 25KV; Electronic beam current: 50 ~ 100nA; Beam spot diameter: 1 μm ~ 20 μm; Crystal is arranged: passage one: RAP; Passage two: PBST; Passage three: PET; Passage four: LIF.This optimum configurations both can ensure the quality of backscatter images imaging, when can ensure again ultimate analysis, and the shooting conditions of complete period element.
Preferred further, the condition of work of described electro probe-X-ray microanalysis is: filament current: 32 μ A; Accelerating potential: 15KV; When qualitative elementary analysis, electronic beam current is 100nA; When element surface analysis, electronic beam current is 50nA.
Preferably, step 2) in, optimum configurations when backscatter images gathers is: enlargement factor: 100x ~ 2000x; Backward scattering accepts scope: Range2 ~ Range3; Image scanning speed: Slow1 ~ Slow3.
The image gathered under this optimum configurations can clean the pattern reflecting sample fracture.
Preferably, step 2) in, the optimum configurations of surface analysis scanning is: Surface scan single point signals acquisition time :≤30.00ms; Surface scan step-length: 0.2 ~ 0.5 μm; Surface scan area size: >=100 μm × 100 μm; Surface scan data point: >=200 × 200.
This optimum configurations can ensure fracture rise split plot carry out element surface analysis time, wave spectrum detector can obtain enough semaphores, and element surface analysis region is enough to cover split plot.
Preferably, step 2) in, when qualitative elementary analysis, electronic beam current is 100nA, and the single-spot testing time is greater than 6min, tests several diverse locations, average at the same area.This optimum configurations can ensure when qualitative elementary analysis, the shooting conditions of complete period element, and wave spectrum detector can obtain enough semaphores.
Preferred further, step 2) in, when qualitative elementary analysis, test 3 diverse locations at the same area, average.
Principle of work of the present invention is as follows:
The doubtful formation of crack region of the fine focusing beam bombardment shaft-like workpiece fracture surface utilizing tungsten filament to launch, by the interaction of electronics and fracture surface material, produce and reflect the be excited chemical composition in district and the various physical messages of physical property profile, by detection display, data processing supervisor, thus obtain the physics in fracture crack source region, the data information of chemical property aspect, with the accurate location in identification fracture crack source and characteristic information.
Through the high energy electron beam bombardment fracture surface that focuses on according to Moseley law, square being directly proportional of the Atom of Elements of the wavelength of characteristic X-ray and generation X ray.Therefore, according to wavelength and the intensity of characteristic X-ray, just can determine it is which kind of element and content thereof.But in analytic process, require that the energy of incident beam must be greater than the critical ionization excitation energy of inner electron of certain Elements Atom.Different classes of material demand arranges different conditions of work, also must carry out a series of correction, correctly could measure the content of element.
The ultimate analysis of electron probe and the combination of backscatter images can reflect the information in the formation of crack region of shaft-like workpiece fracture well.Backscatter images is by backscattered electron imaging, and backscattered electron refers to a part of incident electron reflected by solid sample atom, comprising elasticity backscattered electron and non-resilient backscattered electron.The quantity of backscattered electron increases with the increase of atomic number, so, utilize backscattered electron can not only analyze shape characteristic as imaging signal, also can be used for tracer atom ordinal number contrast, carry out qualitative constituent analysis.
Because the formation of crack of fracture shaft-like workpiece fracture surface often exists element aggregation, the defect such as to be mingled with, backscatter images is utilized to carry out element Surface scan in conjunction with electron probe to crackle source region, clearly can differentiate the accurate location in fracture crack source, and can help to judge formation of crack Producing reason.
Accompanying drawing explanation
In Fig. 1 (a) embodiment 1 shaft-like workpiece fracture surface rise the backscatter images 100 of split plot ×;
In Fig. 1 (b) embodiment 1 shaft-like workpiece fracture surface rise the backscatter images 1000 of split plot ×;
In Fig. 1 (c) embodiment 1, shaft-like workpiece fracture surface plays the electron probe surface analysis image of split plot aluminium (Al) element;
In Fig. 1 (d) embodiment 1, shaft-like workpiece fracture surface plays the electron probe surface analysis image of split plot oxygen (O) element;
In Fig. 2 (a) embodiment 1 shaft-like workpiece fracture surface rise the secondary electron image 1000 of split plot ×;
In Fig. 2 (b) embodiment 1, shaft-like workpiece fracture surface plays the power spectrum surface analysis image of split plot aluminium (Al) element;
In Fig. 2 (c) embodiment 1, shaft-like workpiece fracture surface plays the power spectrum surface analysis image of split plot oxygen (O) element;
In Fig. 3 (a) embodiment 2 shaft-like workpiece fracture surface rise the backscatter images 1000 of split plot ×;
In Fig. 3 (b) embodiment 2, shaft-like workpiece fracture surface plays the electron probe surface analysis image of split plot carbon (C) element;
In Fig. 3 (c) embodiment 2, shaft-like workpiece fracture surface plays the electron probe surface analysis image of split plot iron (Fe) element.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention will be described in detail, can be easy to be readily appreciated by one skilled in the art, thus make more explicit defining to protection scope of the present invention to make advantages and features of the invention.
Embodiment 1
(1) certain shaft-like workpiece (manufactured materials is ferrous alloy) ruptured is sampled, utilize analytically pure acetone to carry out Ultrasonic Cleaning 15 minutes to fracture sample.
(2) adjustment of electron beam centering is carried out to electron probe (Japanese Shimadzu EPMA-1600).Utilization can send the material of fluorescence (as standard model ZrO
2) be placed in beam bombardment under, observe the position of beam bombardment point.Electron beam current is detected, makes electric current reach best saturation point position.Regulate beam spot, be located on screen graticule point of crossing, adjustment beam spot is a full circle.Arranging electron probe condition of work is filament current: 32 μ A; Accelerating potential: 15KV; Electronic beam current: 100nA; Beam spot diameter: 1 μm.
(3) sample on the broken edge through pre-treatment is put into electron probe sample bin, carry out the backscatter images collection (see Fig. 1 (a) and 1 (b)) near the doubtful crackle source region of fracture surface.Clearly can be seen the accurate location in crackle source region by Fig. 1 (a), present black by central area, Fig. 1 (b) visible crack source region, peripheral region presents grey, illustrates that this crackle is the snotter crack initiation being different from matrix from an elemental composition.
(4) electron probe wave spectrum is utilized to carry out qualitative elementary analysis respectively to the regions of different colours playing (Fig. 1 (b)) in knick point place backscatter images, in the middle of finding, black region principal ingredient is aluminium (Al), oxygen (O) element, and surrounding gray region principal ingredient is Fe element.
(5) carry out EDS maps analysis with electron probe to the Al element in this fracture crack source region and O element, analysis result is shown in Fig. 1 (c) and 1 (d), causes the snotter of this crackle crack initiation to be alumina type snotter as seen.The existence of snotter can cause the stress of regional area to concentrate, and very easily produces fine crack and further expands, finally cause shaft-like workpiece to rupture under alternate load.Electron probe element Surface scan optimum configurations: Surface scan single point signals acquisition time: 30.00ms; Surface scan step-length: 0.2 μm; Surface scan area size: 100 μm × 100 μm; Surface scan data point: 500 × 500.
(6) compare with secondary electron image Momentum profiles element analysis technology.
The formation of crack position of the same workpiece fracture that Fig. 2 (a) shows for secondary electron image.According to this picture, by the height fluctuating shape characteristic of fracture surface, the doubtful position of formation of crack substantially can be judged.But the accurate location of knick point can not be shown, and the snotter situation that crackle crack initiation is caused in this region cannot have been shown.Fig. 2 (b) and 2 (c) are respectively the mapping being analyzed crackle source region Al element and the O element obtained by EDS.As seen from the figure, utilize EDS can see the gathering playing split plot Al element and O element at crackle reluctantly, but its resolving effect is far short of what is expected relative to the results of elemental analyses of electron probe.Embodiment 2
(1) certain shaft-like workpiece (manufactured materials is GCr15) ruptured is sampled, utilize analytically pure acetone to carry out Ultrasonic Cleaning 15 minutes to fracture sample.
(2) adjustment of electron beam centering is carried out to electron probe (Japanese Shimadzu EPMA-1600).Arranging electron probe condition of work is filament current: 30 μ A; Accelerating potential: 20KV; Electronic beam current: 50nA; Beam spot diameter: 1 μm.
(3) sample on the broken edge through pre-treatment is put into electron probe sample bin, carry out the backscatter images collection (see Fig. 3 (a)) near the doubtful crackle source region of fracture surface.Clearly can be seen near crackle source region by Fig. 3 (a), except the outside surface of this workpiece has breakage, also can find that many places regional area presents black, and all the other most of regions present brilliant white.This illustrates that this region exists the gathering of certain element.
(4) electron probe wave spectrum is utilized to carry out qualitative elementary analysis respectively to the regions of different colours playing (Fig. 3 (a)) in knick point place backscatter images, find that black region principal ingredient is carbon (C) element, and surrounding gray region principal ingredient is iron (Fe) element.
(5) carrying out EDS maps analysis with electron probe to the C element in this fracture crack source region and Fe element, there is carbon and assembles (Fig. 3 (b) and 3 (c)) in the split plot that rises of visible crack.The gathering of carbon can cause this type of material regional area fragility to increase, thus reduces the fatigue strength of material, increases the risk of workpiece fracture.Surface scan single point signals acquisition time: 40.00ms; Surface scan step-length: 0.5 μm; Surface scan area size: 100 μm × 100 μm; Surface scan data point: 200 × 200.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but the restriction not to invention protection domain; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still in protection scope of the present invention.
Claims (10)
1. electron probe X-ray microanalysis method is detecting the application in shaft-like workpiece fracture failure formation of crack.
2. a recognition methods for shaft-like workpiece fracture failure formation of crack, is characterized in that: comprise the steps:
1) sample pre-treatments: after cutting sample, cleans sample fracture, and protection fracture surface is not destroyed;
2) electro probe-X-ray microanalysis is utilized to carry out backscatter images collection to sample fracture; Wave spectrum qualitative elementary analysis is carried out in the region that the gray scale reflected backscatter images is different, determines that fracture plays the principal ingredient in surperficial different characteristic region near split plot; According to backscatter images and qualitative elementary analysis result, microregion element surface analysis is carried out to the doubtful crack initiation zone position of fracture surface; According to backscatter images and the element surface analysis result of workpiece fracture, identify that fracture plays accurate location and the producing cause of knick point.
3. recognition methods according to claim 2, is characterized in that: step 1) in, the thickness of pretreated sample is 10-15mm, the length of sample and be widely all less than 50mm.
4. recognition methods according to claim 2, is characterized in that: step 1) in, to the method that sample fracture cleans, comprise the steps: first to carry out ultrasonic cleaning 10-15min with organic solvent to fracture surface.
5. recognition methods according to claim 4, it is characterized in that: if sample fracture surface is corroded, after fracture being cleaned with organic solvent, use 2-5% watery hydrochloric acid again, Ultrasonic Cleaning 1-3min, when the corrosion product of fracture surface many places is cleaned, stops cleaning, carry out fracture surface examination; If cleaning performance is not obvious, then uses 6-10% watery hydrochloric acid instead and clean.
6. recognition methods according to claim 2, is characterized in that: step 2) in, the condition of work of electro probe-X-ray microanalysis is: filament current: 28 ~ 35 μ A; Accelerating potential: 10 ~ 25KV; Electronic beam current: 50 ~ 100nA; Beam spot diameter: 1 μm ~ 20 μm; Crystal is arranged: passage one: RAP; Passage two: PBST; Passage three: PET; Passage four: LIF.
7. recognition methods according to claim 2, is characterized in that: step 2) in, optimum configurations when backscatter images gathers is: enlargement factor: 100x ~ 2000x; Backward scattering accepts scope: Range2 ~ Range3; Image scanning speed: Slow1 ~ Slow3.
8. recognition methods according to claim 2, is characterized in that: step 2) in, the optimum configurations of surface analysis scanning is: Surface scan single point signals acquisition time: >=30.00ms; Surface scan step-length: 0.2 ~ 0.5 μm; Surface scan area size: >=100 μm × 100 μm; Surface scan data point: >=200 × 200.
9. recognition methods according to claim 2, is characterized in that: step 2) in, when qualitative elementary analysis, electronic beam current is 100nA, and the single-spot testing time is greater than 6min, tests several diverse locations, average at the same area.
10. recognition methods according to claim 2, is characterized in that: step 2) in, when qualitative elementary analysis, test 3 diverse locations at the same area, average.
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| CN105866120A (en) * | 2016-03-24 | 2016-08-17 | 山东省分析测试中心 | Failure analysis method for suspended structural member of subway power supply network and application thereof |
| CN106840675A (en) * | 2017-03-17 | 2017-06-13 | 复旦大学 | A kind of synthetic determination method of nuclear power generating equipment sluice gate reducer shaft failure cause |
| CN108796514A (en) * | 2018-06-28 | 2018-11-13 | 武钢集团昆明钢铁股份有限公司 | A kind of failure fracture cleaning solution and the preparation method and application thereof |
| CN108857302A (en) * | 2018-07-28 | 2018-11-23 | 国营芜湖机械厂 | A kind of deployment method of metal parts crackle |
| CN113533406A (en) * | 2021-08-11 | 2021-10-22 | 宁波锦越新材料有限公司 | Method for detecting impurity elements in high-purity aluminum ingot |
| CN113655079A (en) * | 2021-07-30 | 2021-11-16 | 宁波锦越新材料有限公司 | Method for detecting 6061 aluminum alloy precipitate |
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| CN108796514A (en) * | 2018-06-28 | 2018-11-13 | 武钢集团昆明钢铁股份有限公司 | A kind of failure fracture cleaning solution and the preparation method and application thereof |
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| CN113655079A (en) * | 2021-07-30 | 2021-11-16 | 宁波锦越新材料有限公司 | Method for detecting 6061 aluminum alloy precipitate |
| CN113533406A (en) * | 2021-08-11 | 2021-10-22 | 宁波锦越新材料有限公司 | Method for detecting impurity elements in high-purity aluminum ingot |
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Application publication date: 20151223 |