CN107607567A - The quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder - Google Patents
The quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder Download PDFInfo
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- CN107607567A CN107607567A CN201710896251.6A CN201710896251A CN107607567A CN 107607567 A CN107607567 A CN 107607567A CN 201710896251 A CN201710896251 A CN 201710896251A CN 107607567 A CN107607567 A CN 107607567A
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Abstract
The invention belongs to physical chemistry of metal technical field, a kind of quantitatively characterizing method of non-metallic inclusion in Ni-base Superalloy Powder is disclosed.Ni-base Superalloy Powder is taken, using the method for electron beam remelting, the ingot that non-metallic inclusion is gathered in upper surface is made.Then part containing non-metallic inclusion is extracted, carries out the molten processing of acid.Pass through the molten different element of substep acid and compound, and carry out suction filtration separation, most the non-metallic inclusion in powder is filtered onto cellulose mixture miillpore filter at last, and morphology observation, identification and the amount of inclusions are carried out to the non-metallic inclusion on cellulose mixture miillpore filter using ESEM and counted, realize the quantitative extraction of non-metallic inclusion in superalloy powder.The method of the present invention has the advantages of easily being obtained using equipment, be simple to operate, short time consumption is short, recovery rate is high, size of separation is unfettered.
Description
Technical field
The invention belongs to physical chemistry of metal technical field, and in particular to nonmetallic folder in a kind of Ni-base Superalloy Powder
The quantitatively characterizing method of debris.
Background technology
Ni-base Superalloy Powder refers to a series of superalloy powders using argon gas or the preparation of nitrogen atomization method, mainly should
Critical component for Aero-Space engine.There is high performance requirement for such material, even micro is nonmetallic
Field trash, also can to finally preparing every physics of alloy components, chemical property produces serious influence, strictly control alloy powder
In non-metallic inclusion content be obtain high performance turbine part essential condition.Therefore, it is accurate analysis nickel base superalloy
Non-metallic inclusion in powder, these field trashes need to be extracted, then pass through scanning electron microscopic observation its form, size point
Cloth and quantity, and energy spectrum analysis is carried out to its composition.
Non-metallic inclusion is mainly derived from foundry alloy melting and powder processed dress in argon gas or nitrogen atomization superalloy powder
Crucible, bottom pour ladle, the refractory material of nozzle put come off, main inclusions SiO2、Al2O3Deng.However, existing appointed condition
And this type impurity can't be completely eliminated for powder-making technique.
At present, the method for separating or extracting non-metallic inclusion in high temperature alloy mainly has water elutriation method, electrolysis, electrostatic
Partition method etc..Non-metallic inclusion in water elutriation method separating high-temp alloy powder is, it is necessary to calculate the theoretical particles that classification is eluriated
Size and critical flow speed, due to non-metallic inclusion shape and irregular, doing between the inhomogeneities of water flow velocity, particle
Sedimentation is related to, then separative efficiency can be caused to reduce, and easily causes non-metallic inclusion separation not exclusively, to the technology of operating personnel
And skill requirement is high；Non-metallic inclusion in electrolysis separating high-temp alloy, generally require that powder sample first is processed into sun
Pole electrode, the suitable electrolyte prescription of selection, controlling potential are stable, control temperature rise and keep electrolyte ph stable, operate compared with
To be cumbersome, and electrolysis time is grown, and up to more than ten or even tens hours, limited small electrode can only be electrolysed, and prepares electricity
Pole takes powder amount limited, it is difficult to which the amount of contained field trash in objective characterisation powder, the complexity that electrolysis is either tested is also
It is the extraction degree of accuracy, all has some limitations；Non-metallic inclusion in electrostatic separation method extraction high temperature alloy, is often needed
Suitable corona electrode voltage, metal roller rotating speed are controlled, field trash optimal separation size be present, and separation rate can not reach
100%.Due to the limitation of above-mentioned existing method, and in powder non-metallic inclusion content very low (1kg powder in itself
The middle non-metallic inclusion that may only have 20 less than 100 μm), current method is difficult to be used as high-purity nickel base superalloy powder
The accurate quantitative analysis extraction of last non-metallic inclusion.
The content of the invention
In place of shortcoming and defect existing for above prior art, it is an object of the invention to provide a kind of nickel-base high-temperature
The quantitatively characterizing method of non-metallic inclusion in alloy powder.
The object of the invention is achieved through the following technical solutions：
The quantitatively characterizing method of non-metallic inclusion, comprises the following steps in a kind of Ni-base Superalloy Powder：
(1) take Ni-base Superalloy Powder briquetting, alloy pig then prepared using electron beam remelting, under draw ingot casting process
In, insoluble non-metallic inclusion, which floats, is enriched to head of ingot upper surface；
(2) by the way of wire cutting, part of the head of ingot upper surface containing non-metallic inclusion is cut down, it is cut
Face is polished with sand paper, then by the part cut down it is cleaned, dry after be added in acid solution and dissolve, be enriched to head of ingot upper table
The non-metallic inclusion in face is separated to acid solution in alloy surface course of dissolution, obtains colloidal suspension acid solution；
(3) toward addition deionized water dilution in colloidal suspension acid solution obtained by step (2), then using cellulose mixture micropore
Filter membrane is filtered, and colloidal suspensions is attached on cellulose mixture miillpore filter；Then colloidal suspensions will be attached with
Cellulose mixture miillpore filter is immersed in deionized water, and sonic oscillation makes colloidal suspensions be desorbed into deionized water, obtains glue
Shape suspension；
(4) toward adding H in the gluey suspension of step (3)2O2Fully reacted with oxalic acid, reaction solution is through deionized water
Filtered after dilution using cellulose mixture miillpore filter, undissolved residue is attached to cellulose mixture miillpore filter
On；Then the cellulose mixture miillpore filter for being attached with residue is immersed in deionized water, sonic oscillation is desorbed residue
Into deionized water, residue mixed liquor is obtained；
(5) toward addition HCl solution and HNO in the residue mixed liquor of step (4)3Solution is fully reacted, reaction solution
Filtered after deionized water dilutes using cellulose mixture miillpore filter, undissolved residue is attached to composite fibre
On plain miillpore filter；Then the cellulose mixture miillpore filter for being attached with residue is immersed in deionized water, sonic oscillation makes
Residue is desorbed into deionized water；
(6) toward adding Enough Dl water in resulting solution in step (5), and using cellulose mixture miillpore filter to molten
Liquid is filtered, and the filter membrane being collected into is placed in drying box and dried；
(7) metal spraying processing, orthogonal direction edge are carried out to filter membrane positive (one side for being attached with residue) obtained by step (6)
Place is fixed using conducting resinl, and the pattern and composition of non-metallic inclusion on filter membrane are entered using SEM and energy disperse spectroscopy
Row characterizes, and counts non-metallic inclusion particles quantity.
The selection of Ni-base Superalloy Powder amount in step (1), it can be carried out freely according to the size of amount of powder to be analyzed
It is appropriately selected, can more accurately non-metallic inclusion that may be present in quantitative analysis powder.
The polishing of sand paper described in step (2) refers to use is polished using No. 1200 sand paper；Described cleaning refers to successively third
It is cleaned by ultrasonic in ketone solution and ethanol, is then rinsed with deionization.
Preferably, the acid solution described in step (2) refers to dense HCl and dense HNO3Mixed solution, wherein dense HCl quality
Fraction is 36~38%, dense HNO3Mass fraction be 65~68%；Dense HCl and dense HNO3Volume ratio be preferably 6:1.
Preferably, the aperture of the cellulose mixture miillpore filter described in step (3)~(6) be 0.22 μm, 0.45 μm or
0.8μm。
Preferably, the frequency of sonic oscillation described in step (3)~(5) be 40kHz, power 100W.
Preferably, the mass fraction that HCl solution refers to described in step (5) be 20% HCl solution, the HNO3Solution
Refer to the HNO that mass fraction is 65~68%3Solution.
The present invention principle be：In the production process of Ni-base Superalloy Powder, because foundry alloy melting and powder processed fill
Crucible, bottom pour ladle, the refractory material of nozzle put come off, in the deoxidation products, atomizing medium argon gas even in fusion process
Solid particle and technical process environmental pollution are likely to introduce non-metallic inclusion, such as SiO2、Al2O3Deng.And nickel-base high-temperature closes
The chemical composition of gold mainly has the elements such as nickel, chromium, cobalt, tungsten, molybdenum, niobium, titanium, aluminium, using the chemical property of each alloying element, selects
Suitable reagent promotes alloying element to enter in the form of ion among solution, with the metastable SiO of chemical property2、Al2O3
Separation is produced Deng non-metallic inclusion, is finally reached the purpose of extraction non-metallic inclusion.It is (dense by controlling acid solution to match
HCl and dense HNO3The volume ratio of solution is about 6:1) H, is sequentially added2O2With oxalic acid, HCl solution and HNO3Solution is to dissolve indissoluble
Thing (such as W, Mo, Nb, Ti and its corresponding oxide), and filtered using cellulose mixture miillpore filter, so as to quantitative table
Levy number, composition and the shape characteristic of non-metallic inclusion in Ni-base Superalloy Powder.
The method of the present invention has the following advantages that and beneficial effect：
(1) present invention can be analyzed the alloy powder of any amount, and it is limited not to overcome electrolysis sample size
Foot.
(2) the cellulose mixture miillpore filter that the present invention uses has more preferable compared with the miillpore filter of other materials
Hydrophily, it is mainly used in the filtering of aqueous solution, material is easy to get and cost is low.It is also equipped with that microcellular structure is uniform, porosity is high, nothing
Medium comes off, filtering velocity is fast, and absorption is minimum, is resistant to the features such as diluted acid.During sonic oscillation, the attachment of filter membrane surface is easy
Depart from, and do not damage filter membrane, substantially increase the recovery rate of non-metallic inclusion.
(3) present invention is combined the nonmetallic folder in extraction Ni-base Superalloy Powder using electron beam remelting with acid extracting
Debris, compared with water elutriation method, recovery rate is higher, non-metallic inclusion that can more accurately in powder quantitatively.
(4) present invention has simple to operate, time-consuming feature shorter, recovery rate is higher, and can solve compared with electrolysis
The limitation extracted when inclusion content is few using electrolysis.
(5) for the present invention compared with electrostatic separation method, recovery rate is higher, and not by the pact of non-metallic inclusion optimum size
Beam.
(6) present invention overcomes product and observes incomplete deficiency compared with observing the non-metallic inclusion in product.
(7) present invention uses powder as research object, it is only necessary to the simple briquet of powder is subjected to electron beam remelting,
Special processing and heat treatment need not be carried out, and operating process simply, is easily obtained using equipment.
Brief description of the drawings
Fig. 1 is the alloy pig that upper surface is enriched with non-metallic inclusion in the embodiment of the present invention；
Fig. 2 is alloy block of the upper surface containing field trash after cutting cleaning in the embodiment of the present invention；
Fig. 3 is the separated and dissolved of part containing non-metallic inclusion and alloy component in acid dissolution in the embodiment of the present invention；
Fig. 4 is to filter process schematic in the embodiment of the present invention；
Fig. 5 is filtered cellulose mixture miillpore filter in the embodiment of the present invention；
Fig. 6 be the embodiment of the present invention in scanning electron microscopic observation to filter membrane on non-metallic inclusion.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment
The present embodiment is so that particle diameter is less than 105 μm of FGH96 Ni-base Superalloy Powders as an example, the essential element of alloy
For：Cr, Co, W, Mo, Ti, Al, Nb and Ni, quantitative extraction is carried out to non-metallic inclusion contained therein and is characterized, specific step
It is rapid as follows：
(1) about 270g FGH96 Ni-base Superalloy Powders are taken, by powder briquetting, is then prepared and closed using electron beam remelting
Bronze end ingot, non-metallic inclusion, which floats, is enriched to head of ingot upper surface, sees Fig. 1；
(2) by the way of wire cutting, ingot upper surface part containing field trash is cut down, and cut surface is beaten with sand paper
No. 1200 sand paper are milled to, then the part cut down are carried out to ultrasonic wave cleaning 10min in acetone soln, and surpassed with alcohol
Sound cleans 10min, is then flushed three times with deionized water, and dries up stand-by, sees Fig. 2；
(3) 70mL acid solutions are prepared, acid solution is dense HCl and dense HNO3Mixed liquor, volume ratio 6:1, wherein dense HCl
The mass fraction of solution is 36~38%, dense HNO3The mass fraction of solution is about 65~68%；
(4) sample after step (2) processing is put into the acid solution of step (3) at room temperature and chemically reacted,
After about 20min, Fig. 3 with alloy component separated and dissolved, is seen in part containing field trash, takes out not molten alloy block after separation,
And the alloy block 3 times taken out is rinsed toward beaker direction with deionized water；
(5) toward in the colloidal suspensions obtained by step (4), adding the dilution of 2L deionized waters；Then cellulose mixture is used
Miillpore filter is filtered to the dilution of gained so that colloidal suspensions are attached on cellulose mixture miillpore filter, described
Cellulose mixture miillpore filter aperture be 0.8 μm；
(6) the cellulose mixture miillpore filter that colloidal suspensions are attached with step (5) is placed in and fills 20mL deionizations
In the beaker of water, sonic oscillation 10min, gluey suspension is obtained, filter membrane is gently taken out from beaker with tweezers, and use deionization
Water rinses filter membrane 3 times toward beaker direction, and the supersonic frequency is 40kHz, power 100W；
(7) toward in the gluey suspension of gained in step (6), 300mL 30wt.%H are added2O2Solution, add 20g grass
Acid crystal, it is stirred well to oxalic acid crystal and is completely dissolved, solution turned yellow, suspension starts to become clarification, and beaker bottom has obvious residual
Thing is stayed, this process lasts about 30min, is eventually adding 500Ml deionized waters and is diluted；
(8) resulting solution in step (7) is filtered using cellulose mixture miillpore filter, the filter membrane being collected into is put
In the beaker for filling 20mL deionized waters, sonic oscillation 10min, residue mixed liquor is obtained, with tweezers gently from beaker
Filter membrane is taken out, and filter membrane is rinsed 3 times toward beaker direction with deionized water；
(9) 100mL 20wt.%HCl solution is added toward the residue mixed liquor in step (8), is sufficiently stirred, adds
30mL 65wt.%HNO3Solution, residue dissolving is stirred well to, clarity of solution is higher, adds 500mL deionized waters and enters
Row dilution；Then the clarified solution of gained is filtered using cellulose mixture miillpore filter, the filter membrane being collected into is placed in Sheng
In the beaker for there are 20mL deionized waters, sonic oscillation 10min, filter membrane is gently taken out from beaker with tweezers, and use deionized water
Filter membrane is rinsed toward beaker direction 3 times；
(10) toward addition 500mL deionized waters in the solution of gained in step (9), and cellulose mixture miillpore filter is used
Solution is filtered, suction filtration process is shown in Fig. 4, and filter membrane is shown in Fig. 5, and the filter membrane being collected into is placed in drying box and dried；
(11) metal spraying processing being carried out to filter membrane front obtained by step (10), orthogonal direction edge is fixed using conducting resinl,
The pattern and composition of the non-metallic inclusion on filter membrane are characterized using SEM and energy disperse spectroscopy, as a result see figure
6 with table 1, and count non-metallic inclusion particles quantity.
Table 1
| Element | Mass fraction/% | Atomic percent/% |
| O | 59.26 | 71.86 |
| Si | 40.74 | 28.14 |
| Amount to | 100.00 | 100.00 |
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. the quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder, it is characterised in that including following step
Suddenly：
(1) take Ni-base Superalloy Powder briquetting, alloy pig then prepared using electron beam remelting, under draw ingot casting during, no
Molten non-metallic inclusion, which floats, is enriched to head of ingot upper surface；
(2) by the way of wire cutting, part of the head of ingot upper surface containing non-metallic inclusion is cut down, its cut surface is used
Sand paper is polished, then by the part cut down it is cleaned, dry after be added in acid solution and dissolve, be enriched to head of ingot upper surface
Non-metallic inclusion is separated to acid solution in alloy surface course of dissolution, obtains colloidal suspension acid solution；
(3) toward addition deionized water dilution in colloidal suspension acid solution obtained by step (2), then using cellulose mixture miillpore filter
Filtered, colloidal suspensions is attached on cellulose mixture miillpore filter；Then the mixing of colloidal suspensions will be attached with
Cellulose microporosity filter membrane is immersed in deionized water, and sonic oscillation makes colloidal suspensions be desorbed into deionized water, is obtained gluey outstanding
Turbid；
(4) toward adding H in the gluey suspension of step (3)2O2Fully reacted with oxalic acid, reaction solution dilutes through deionized water
Filtered afterwards using cellulose mixture miillpore filter, undissolved residue is attached on cellulose mixture miillpore filter；
Then the cellulose mixture miillpore filter that residue will be attached with is immersed in deionized water, and sonic oscillation makes residue be desorbed to going
In ionized water, residue mixed liquor is obtained；
(5) toward addition HCl solution and HNO in the residue mixed liquor of step (4)3Solution is fully reacted, reaction solution through go from
Filtered after sub- water dilution using cellulose mixture miillpore filter, undissolved residue is attached to cellulose mixture micropore
On filter membrane；Then the cellulose mixture miillpore filter for being attached with residue is immersed in deionized water, sonic oscillation makes residue
Desorption is into deionized water；
(6) toward adding Enough Dl water in resulting solution in step (5), and solution is entered using cellulose mixture miillpore filter
Row is filtered, and the filter membrane being collected into is placed in drying box and dried；
(7) metal spraying processing is carried out to filter membrane front obtained by step (6), orthogonal direction edge is fixed using conducting resinl, using sweeping
Retouch electron microscope and energy disperse spectroscopy to characterize the pattern and composition of non-metallic inclusion on filter membrane, and count nonmetal inclusion
Composition granule quantity.
2. the quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder according to claim 1, its
It is characterised by：The polishing of sand paper described in step (2) refers to use is polished using No. 1200 sand paper；Described cleaning refers to successively third
It is cleaned by ultrasonic in ketone solution and ethanol, is then rinsed with deionization.
3. the quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder according to claim 1, its
It is characterised by：Acid solution described in step (2) refers to dense HCl and dense HNO3Mixed solution, wherein dense HCl mass fraction is
36~38%, dense HNO3Mass fraction be 65~68%.
4. the quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder according to claim 3, its
It is characterised by：The dense HCl and dense HNO3Volume ratio be 6:1.
5. the quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder according to claim 1, its
It is characterised by：The aperture of cellulose mixture miillpore filter described in step (3)~(6) is 0.22 μm, 0.45 μm or 0.8 μm.
6. the quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder according to claim 1, its
It is characterised by：The frequency of sonic oscillation described in step (3)~(5) is 40kHz, power 100W.
7. the quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder according to claim 1, its
It is characterised by：The mass fraction that HCl solution refers to described in step (5) be 20% HCl solution, the HNO3Solution refers to matter
Measure the HNO that fraction is 65~68%3Solution.
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| CN109269965A (en) * | 2018-11-08 | 2019-01-25 | 马鞍山沐及信息科技有限公司 | A kind of metallic inclusion integrates extraction element and extracting method |
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| CN109374666A (en) * | 2018-10-16 | 2019-02-22 | 中国科学院金属研究所 | It detects selective laser and melts the method for being mingled with content in ultra-fine titanium alloy powder |
| CN111238916A (en) * | 2020-02-12 | 2020-06-05 | 北京科技大学 | Classified extraction and quantitative analysis method for nonmetallic inclusions in high-temperature alloy |
| CN111551576A (en) * | 2020-05-09 | 2020-08-18 | 中国航发北京航空材料研究院 | Method for quantitatively evaluating influence of vacuum degree and oxidation products on performance of high-temperature alloy |
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| CN111551576A (en) * | 2020-05-09 | 2020-08-18 | 中国航发北京航空材料研究院 | Method for quantitatively evaluating influence of vacuum degree and oxidation products on performance of high-temperature alloy |
| CN112945824A (en) * | 2021-02-24 | 2021-06-11 | 西安欧中材料科技有限公司 | Method for detecting inclusions in fine-particle-size nickel-based superalloy powder |
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