CN105738188A - Separation method for nonmetallic inclusions in Inconel625-series high-temperature alloy - Google Patents
Separation method for nonmetallic inclusions in Inconel625-series high-temperature alloy Download PDFInfo
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- CN105738188A CN105738188A CN201610108541.5A CN201610108541A CN105738188A CN 105738188 A CN105738188 A CN 105738188A CN 201610108541 A CN201610108541 A CN 201610108541A CN 105738188 A CN105738188 A CN 105738188A
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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
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
Abstract
The invention discloses a separation method for nonmetallic inclusions in an Inconel625-series high-temperature alloy, and belongs to the technical field of methods for researches on nonmetallic inclusions in metallic materials. A proper electrolyte is selected to electrolyze a high-temperature alloy test sample; a collected extract mixture is separated by virtue of a chemical method after electrolysis, and carbides are dissolved to completely and nondestructively extract fine oxide inclusions in the Inconel625-series high-temperature alloy; the obtained oxide inclusions are observed to have obvious particle shapes under a scanning electron microscope, and are proven to be Al and Mg containing composite oxide inclusions by energy spectrum analysis.
Description
Technical field
The present invention relates to the research method of non-metallic inclusion in a kind of metal material, particularly relate to the dose of non-metallic inclusion in Inconel625 series of high temperature alloy.
Background technology
Inconel625 series of high temperature alloy refers to 625 alloys and derived material thereof (718,706 etc.).It occupies extremely important status in high temperature alloy field, is widely used in the critical component in the heavy industry fields such as Aero-Space, industry gas turbine, petrochemical industry, boats and ships naval vessels, nuclear-plant.It is therefore desirable to this type of material must have high physics, chemical property, and trace non-metallic inclusion has a strong impact on its property indices.
At present, the research of non-metallic inclusion is concentrated mainly in ferrous materials, the research of nonmetallic inclusionsin steel is quite ripe, and to it, study electrolyte and the electrolysis system mainly by electroextraction nonmetallic inclusionsin steel of non-metallic inclusion in nickel base superalloy are carried out electrolysis.Serious matrix is there is and comes off problem in the method in the electrolysis of nickel base superalloy；Extract after usual electrolysis is often the mixture of carbide and nonmetal inclusion, and carbide accounts for the overwhelming majority, separates non-metallic inclusion and be not affected by enough attention always from the mixed extracts of carbide and nonmetal inclusion；And the degree of purity of nickel base superalloy is significantly larger than the degree of purity of common steel grade, cause the content of non-metallic inclusion and smaller, non-metallic inclusion tiny in process of setting is often as the nucleating center of carbide, partially carbonized thing forming core on non-metallic inclusion particle is grown up, form clad structure, have a strong impact on after electrolysis is collected the observation of non-metallic inclusion and analysis.Therefore, for nickel base superalloy, how life size, original shape looks extract non-metallic inclusion, and effectively remove the impact of carbide, have become as non-metallic inclusion in nickel base superalloy and observe and the emphasis analyzed and difficult point.
Summary of the invention
It is an object of the invention to provide the separation method of non-metallic inclusion in a kind of Inconel625 series of high temperature alloy.
The present invention is the separation method of non-metallic inclusion in Inconel625 series of high temperature alloy, the steps include:
(1) prepared by workpiece: adopt mach method to cut rod-shaped workpiece at alloy pig field trash enrichment positions；The workpiece cut is placed in acetone soln and utilizes ultrasonic wave concussion to clean about 10min；
(2) heat treatment: adopting chamber type electric resistance furnace that the workpiece after cleaning is carried out two-period form solution treatment, concrete Technology for Heating Processing is: 1130～1170 DEG C of insulation 1h, is warming up to 1200～1210 DEG C of insulation 1h, water-cooled；
(3) semipermeable membrane poly-bag is made: according to workpiece size, a small amount of liquid collodion is poured into the reaction vessel of suitable capacity, rotary container so that it is inwall uniformly adheres to one layer of collodion, pours out surplus liquid, solid Deng collodion, carefully tear take off immersion distilled water in standby；
(4) preparation electrolyte: adopt aqueous solution electrolysis, electrolyte concrete proportioning by weight is: ammonium sulfate 1%～2%, citric acid 2.5%～3.5%, citric acid ammonia 1%～2%, surplus is distilled water；
(5) surface treatment: by workpiece after heat treatment, in unfiltered electrolyte, large-current electric solution corrosion about 30～50min, removes the oxide skin of surface of the work, and cleans out surface of the work with hairbrush；
(6) aqueous solution electrolysis: the workpiece to be electrolysed of the 5th step gained and electrolysis unit are connected and carries out electrolysis；Adopting potentiostatic method during electrolysis, control electrolysis temperature at 25～35 DEG C in ice-water bath, electric current density is 90～120mA/cm2, change electrolyte after electrolysis 10～12h, until workpiece immerses the complete electrolysis of part of electrolyte, 7～15 workpiece of continuous electrolysis according to the actual requirements；
(7) clean: after electrolysis completes, take out semipermeable membrane poly-bag, extract therein is flushed in the beaker of 1L, topping-up, stands 6～12h, by the mixed extracts upper clear supernate of siphon sucking-off carbide Yu non-metallic inclusion, repeatedly fill standing sucking-off, until solution water white transparency；
(8) Chemical Decomposition: utilize water-bath that the 7th step gained mixed extracts aqueous solution is heated to 80～100 DEG C, add isopyknic saturated oxalic acid solution, after insulation 10～20min, concentrated nitric acid is dripped in beaker, until containing the nitric acid of 10% in solution, insulation 0.5～2h, dissolves carbide, retains and expose non-metallic inclusion；
(9) centrifugal collection: repeatedly cleaned by gained non-metallic inclusion in the 8th step, on centrifuge, centrifugal collection, dries, finally gives non-metallic inclusion.
The invention have the benefit that makes Laves phase fully dissolve by two-period form solution treatment, and a large amount of solid solution of MC, alloy substrate is uniform；Surface of the work smooth in this aqueous electrolyte (ammonium sulfate 1%～2%, citric acid 2.5%～3.5%, citric acid ammonia 1%～2%, surplus is distilled water) electrolysis alloy workpiece process, it is to avoid the problem of matrix severe detachment；The carbide collected after electrolysis and non-metallic inclusion mixed extracts adopt oxalic acid-nitrate method and non-metallic inclusion to be easily separated, and dissolve carbide, retain and expose non-metallic inclusion, thus the non-metallic inclusion in this series of high temperature alloy of lossless extraction.
Accompanying drawing explanation
Fig. 1 is the conventional electrolysers schematic diagram adopted in the present invention, and accompanying drawing labelling and corresponding name are called: 1 ice bath groove, and 2 support the glass frame of poly-bag, 3 negative electrodes; 4 cathode legs, 5 anode electrode folders, 6 thermometeies, 7 seal protection lid; 8 alloy workpieces (anode), 9 Pyroxylin poly-bags, 10 power supplys；Fig. 2 is the mixed extracts figure collected after electrolysis, the essentially carbide of skeletal like, and Fig. 3 is the scanning electron microscope shape appearance figure of Chemical Decomposition rear oxidation thing, for the composite oxides inclusion particle of Al-Mg-O composition.
Detailed description of the invention
The present invention is the separation method of non-metallic inclusion in Inconel625 series of high temperature alloy, the steps include:
(1) prepared by workpiece: adopt mach method to cut rod-shaped workpiece at alloy pig field trash enrichment positions；The workpiece cut is placed in acetone soln and utilizes ultrasonic wave concussion to clean about 10min；
(2) heat treatment: adopting chamber type electric resistance furnace that the workpiece after cleaning is carried out two-period form solution treatment, concrete Technology for Heating Processing is: 1130～1170 DEG C of insulation 1h, is warming up to 1200～1210 DEG C of insulation 1h, water-cooled；
(3) semipermeable membrane poly-bag is made: according to workpiece size, a small amount of liquid collodion is poured into the reaction vessel of suitable capacity, rotary container so that it is inwall uniformly adheres to one layer of collodion, pours out surplus liquid, solid Deng collodion, carefully tear take off immersion distilled water in standby；
(4) preparation electrolyte: adopt aqueous solution electrolysis, electrolyte concrete proportioning by weight is: ammonium sulfate 1%～2%, citric acid 2.5%～3.5%, citric acid ammonia 1%～2%, surplus is distilled water；
(5) surface treatment: by workpiece after heat treatment, in unfiltered electrolyte, large-current electric solution corrosion about 30～50min, removes the oxide skin of surface of the work, and cleans out surface of the work with hairbrush；
(6) aqueous solution electrolysis: the workpiece to be electrolysed of the 5th step gained and electrolysis unit are connected and carries out electrolysis；Adopting potentiostatic method during electrolysis, control electrolysis temperature at 25～35 DEG C in ice-water bath, electric current density is 90～120mA/cm2, change electrolyte after electrolysis 10～12h, until workpiece immerses the complete electrolysis of part of electrolyte, 7～15 workpiece of continuous electrolysis according to the actual requirements；
(7) clean: after electrolysis completes, take out semipermeable membrane poly-bag, extract therein is flushed in the beaker of 1L, topping-up, stands 6～12h, by the mixed extracts upper clear supernate of siphon sucking-off carbide Yu non-metallic inclusion, repeatedly fill standing sucking-off, until solution water white transparency；
(8) Chemical Decomposition: utilize water-bath that the 7th step gained mixed extracts aqueous solution is heated to 80～100 DEG C, add isopyknic saturated oxalic acid solution, after insulation 10～20min, concentrated nitric acid is dripped in beaker, until containing the nitric acid of 10% in solution, insulation 0.5～2h, dissolves carbide, retains and expose non-metallic inclusion；
(9) centrifugal collection: repeatedly cleaned by gained non-metallic inclusion in the 8th step, on centrifuge, centrifugal collection, dries, finally gives non-metallic inclusion.
Step (8) the described carbide of above-described separation method is NbC.
Step (8) the described non-metallic inclusion of above-described separation method is that fine oxide is mingled with, and the non-metallic inclusion in Inconel625 high temperature alloy is mainly the composite oxides of Al-Mg-O.
The present embodiment is for Inconel625 alloy, and Inconel625 alloy adds electroslag remelting (ESR) explained hereafter by vacuum induction melting (VIM).Hereinafter adopt the separation method of non-metallic inclusion in the Inconel625 series of high temperature alloy of embodiment of the present invention offer that non-metallic inclusion in Inconel625 alloy is easily separated extraction, specifically comprise the following steps that
The first step: prepared by workpiece:
Cutting rod-shaped workpiece in position, Inconel625 alloy cast ingot heart portion, workpiece size is 8 × 70mm(diameter × height).The workpiece cut is placed in acetone soln and utilizes ultrasonic wave concussion to clean 10min；
Second step: heat treatment:
Adopt chamber type electric resistance furnace that the rod-shaped workpiece after cleaning is carried out two-period form solution treatment.Concrete Technology for Heating Processing is: 1150 DEG C of insulation 1h, is warming up to 1200 DEG C of insulation 1h, water-cooled.Reach to eliminate microscopic segregation, the purpose of the certain MC of solid solution by heat treatment；
3rd step: make semipermeable membrane poly-bag:
Pour a small amount of liquid collodion into 150ml reaction vessel, rotary container so that it is inwall uniformly adheres to one layer of collodion, pours out surplus liquid, waits collodion solid, carefully tear take off immersion distilled water in standby；
4th step: preparation electrolyte:
Electrolyte concrete proportioning by weight is: ammonium sulfate 1%～2%, citric acid 2.5%～3.5%, citric acid ammonia 1%～2%, surplus is distilled water, pours the electrolyte in Pyroxylin poly-bag into and must filter through quantitative filter paper；
5th step: surface treatment:
Electrolysis unit is connected, when not putting into semipermeable membrane, by the large-current electric solution corrosion 30min in above-mentioned electrolyte of workpiece after heat treatment shown in Fig. 1, remove the black oxidation skin of surface of the work, surface is cleaned out to light with hairbrush, and workpiece of weighing, record numerical value；
6th step: aqueous solution electrolysis:
The workpiece to be electrolysed of the 5th step gained is assembled by shown in Fig. 1, adopts potentiostatic method to carry out electrolysis.Controlling electrolysis temperature 30 DEG C in ice-water bath, electric current density is 100mA/cm2, change electrolyte after electrolysis 12h, until workpiece immerses the complete electrolysis of part of electrolyte, 10 workpiece of continuous electrolysis.Electrolysis weighs residual metal workpiece weight record after completing；
7th step: clean:
After electrolysis completes, take out semipermeable membrane poly-bag, extract therein is flushed in the beaker of 1L, topping-up, stands 12h, with the clear liquid of siphon sucking-off carbide Yu non-metallic inclusion mixed extracts top, repeatedly fill standing sucking-off, until solution water white transparency.A small amount of mixed extracts is taken, for scanning electron microscopic observation with spoon；
8th step: Chemical Decomposition:
Utilize water-bath that the 7th step gained mixed extracts aqueous solution is heated to 90 DEG C, add isopyknic saturated oxalic acid solution, after insulation 15min, concentrated nitric acid is dripped in beaker, until containing the nitric acid of 10% in solution, after insulation 30min, dissolve carbide, retain and expose non-metallic inclusion；
9th step: centrifugal collection:
After in the 8th step, gained non-metallic inclusion cleans repeatedly, on centrifuge, centrifugal collection, dries, finally gives non-metallic inclusion, and weigh.
Tenth step: scanning electron microscope analysis:
Mixed extracts and non-metallic inclusion are disperseed with ultrasonic cleaner by dehydrated alcohol respectively, to its pattern and dimension analysis under scanning electron microscope after dispersion, as shown in Figure 2 and Figure 3, and utilizes power spectrum to its component analysis.So that it is determined that mixed extracts essentially size is at the NbC of about 10 μm skeletal likes after electrolysis, non-metallic inclusion size at about 1 μm, the graininess composite oxides being made up of Al-Mg-O.
Claims (3)
- The separation method of non-metallic inclusion in 1.Inconel625 series of high temperature alloy, it is characterised in that the steps include:(1) prepared by workpiece: adopt mach method to cut rod-shaped workpiece at alloy pig field trash enrichment positions；The workpiece cut is placed in acetone soln and utilizes ultrasonic wave concussion to clean about 10min；(2) heat treatment: adopting chamber type electric resistance furnace that the workpiece after cleaning is carried out two-period form solution treatment, concrete Technology for Heating Processing is: 1130～1170 DEG C of insulation 1h, is warming up to 1200～1210 DEG C of insulation 1h, water-cooled；(3) semipermeable membrane poly-bag is made: according to workpiece size, a small amount of liquid collodion is poured into the reaction vessel of suitable capacity, rotary container so that it is inwall uniformly adheres to one layer of collodion, pours out surplus liquid, solid Deng collodion, carefully tear take off immersion distilled water in standby；(4) preparation electrolyte: adopt aqueous solution electrolysis, electrolyte concrete proportioning by weight is: ammonium sulfate 1%～2%, citric acid 2.5%～3.5%, citric acid ammonia 1%～2%, surplus is distilled water；(5) surface treatment: by workpiece after heat treatment, in unfiltered electrolyte, large-current electric solution corrosion about 30～50min, removes the oxide skin of surface of the work, and cleans out surface of the work with hairbrush；(6) aqueous solution electrolysis: the workpiece to be electrolysed of the 5th step gained and electrolysis unit are connected and carries out electrolysis；Adopting potentiostatic method during electrolysis, control electrolysis temperature at 25～35 DEG C in ice-water bath, electric current density is 90～120mA/cm2, change electrolyte after electrolysis 10～12h, until workpiece immerses the complete electrolysis of part of electrolyte, 7～15 workpiece of continuous electrolysis according to the actual requirements；(7) clean: after electrolysis completes, take out semipermeable membrane poly-bag, extract therein is flushed in the beaker of 1L, topping-up, stands 6～12h, by the mixed extracts upper clear supernate of siphon sucking-off carbide Yu non-metallic inclusion, repeatedly fill standing sucking-off, until solution water white transparency；(8) Chemical Decomposition: utilize water-bath that the 7th step gained mixed extracts aqueous solution is heated to 80～100 DEG C, add isopyknic saturated oxalic acid solution, after insulation 10～20min, concentrated nitric acid is dripped in beaker, until containing the nitric acid of 10% in solution, insulation 0.5～2h, dissolves carbide, retains and expose non-metallic inclusion；(9) centrifugal collection: repeatedly cleaned by gained non-metallic inclusion in the 8th step, on centrifuge, centrifugal collection, dries, finally gives non-metallic inclusion.
- 2. the separation method of non-metallic inclusion in Inconel625 series of high temperature alloy according to claim 1, it is characterised in that carbide described in step 8 is NbC.
- 3. the separation method of non-metallic inclusion in Inconel625 series of high temperature alloy according to claim 1, it is characterized in that, non-metallic inclusion described in step 8 is that fine oxide is mingled with, and the non-metallic inclusion in Inconel625 high temperature alloy is mainly the composite oxides of Al-Mg-O.
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| CN107607567A (en) * | 2017-09-28 | 2018-01-19 | 华南理工大学 | The quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder |
| CN108362256A (en) * | 2018-03-07 | 2018-08-03 | 辽宁科技大学 | A kind of electroslag remelting metal bath bottom pattern aided observing device and observation procedure |
| CN108918221A (en) * | 2018-07-12 | 2018-11-30 | 中国航发哈尔滨轴承有限公司 | Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel |
| CN108918220A (en) * | 2018-07-12 | 2018-11-30 | 中国航发哈尔滨轴承有限公司 | Carbide Phases low-temperature extraction method in ZGCr15 bearing steel |
| 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 |
| 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 |
| CN111238915A (en) * | 2020-02-12 | 2020-06-05 | 北京科技大学 | Method for extracting non-metallic inclusions in high-temperature alloy |
| CN113466271A (en) * | 2021-07-30 | 2021-10-01 | 钢铁研究总院 | Method for accurately determining type, morphology and elemental composition of intermetallic compounds in steel |
| CN114113181A (en) * | 2022-01-27 | 2022-03-01 | 北京科技大学 | Original appearance analysis method for separating inclusions in non-aluminum weakly-deoxidized bearing steel through electrolysis |
| CN115144323A (en) * | 2022-08-29 | 2022-10-04 | 中国航发北京航空材料研究院 | Method for detecting content of non-metallic inclusions in metal powder for additive manufacturing |
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| CN107328619B (en) * | 2017-06-07 | 2020-11-06 | 北京科技大学 | Method for separating non-metallic inclusions and carbides in steel inclusions |
| CN107328619A (en) * | 2017-06-07 | 2017-11-07 | 北京科技大学 | A kind of method of non-metallic inclusion and carbide in separation of steel field trash |
| CN107607567A (en) * | 2017-09-28 | 2018-01-19 | 华南理工大学 | The quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder |
| CN107607567B (en) * | 2017-09-28 | 2022-08-12 | 华南理工大学 | Quantitative characterization method for nonmetallic inclusions in nickel-based superalloy powder |
| CN108362256A (en) * | 2018-03-07 | 2018-08-03 | 辽宁科技大学 | A kind of electroslag remelting metal bath bottom pattern aided observing device and observation procedure |
| CN108362256B (en) * | 2018-03-07 | 2023-09-08 | 辽宁科技大学 | Auxiliary observation device and method for bottom morphology of electroslag remelting metal molten pool |
| CN108918220A (en) * | 2018-07-12 | 2018-11-30 | 中国航发哈尔滨轴承有限公司 | Carbide Phases low-temperature extraction method in ZGCr15 bearing steel |
| CN108918221A (en) * | 2018-07-12 | 2018-11-30 | 中国航发哈尔滨轴承有限公司 | Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel |
| 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 |
| CN111238915A (en) * | 2020-02-12 | 2020-06-05 | 北京科技大学 | Method for extracting non-metallic inclusions in high-temperature alloy |
| 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 |
| CN111238915B (en) * | 2020-02-12 | 2021-05-07 | 北京科技大学 | Method for extracting non-metallic inclusions in high-temperature alloy |
| CN113466271A (en) * | 2021-07-30 | 2021-10-01 | 钢铁研究总院 | Method for accurately determining type, morphology and elemental composition of intermetallic compounds in steel |
| CN114113181A (en) * | 2022-01-27 | 2022-03-01 | 北京科技大学 | Original appearance analysis method for separating inclusions in non-aluminum weakly-deoxidized bearing steel through electrolysis |
| CN114113181B (en) * | 2022-01-27 | 2022-04-08 | 北京科技大学 | Original appearance analysis method for separating inclusions in non-aluminum weakly-deoxidized bearing steel through electrolysis |
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