CN112553679A - Monomer separation method for harmful phase of isothermal forging die material for turbine disc - Google Patents
Monomer separation method for harmful phase of isothermal forging die material for turbine disc Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000010275 isothermal forging Methods 0.000 title claims abstract description 39
- 239000000178 monomer Substances 0.000 title claims abstract description 31
- 238000000926 separation method Methods 0.000 title claims abstract description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 238000000605 extraction Methods 0.000 claims abstract description 28
- 238000005728 strengthening Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 12
- 238000004062 sedimentation Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 39
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 239000003792 electrolyte Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 10
- 238000005242 forging Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000004816 latex Substances 0.000 claims description 6
- 229920000126 latex Polymers 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims 1
- 229910052721 tungsten Inorganic materials 0.000 claims 1
- 239000010937 tungsten Substances 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 9
- 238000005191 phase separation Methods 0.000 abstract 1
- 238000004445 quantitative analysis Methods 0.000 abstract 1
- 235000011187 glycerol Nutrition 0.000 description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 229910052759 nickel Inorganic materials 0.000 description 5
- 229910000601 superalloy Inorganic materials 0.000 description 5
- 238000009991 scouring Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000002939 deleterious effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000001473 noxious effect Effects 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005363 electrowinning Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0419—Solvent extraction of solutions which are liquid in combination with an electric or magnetic field or with vibrations
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a monomer separation method of a harmful phase of an isothermal forging die material for a turbine disc, which comprises the steps of firstly, carrying out electrolysis extraction on a mixed solution containing the harmful phase and a plurality of strengthening phases from a sample of the isothermal forging die material for the turbine disc, adding a proper amount of glycerol into the mixed solution to adjust the viscosity after the electrolysis is finished, and further independently separating a solid harmful phase single-phase entity by utilizing the density difference of the harmful phase and the strengthening phases and the sedimentation rate difference of the harmful phase and the strengthening phases in a liquid with specific viscosity. The method solves the problem that the traditional technology can only separate the harmful phase and the strengthening precipitated phase from the matrix in a mixed state but can not separate the single-phase harmful phase, realizes the single-phase separation of the harmful phase of the isothermal forging die material for the turbine disc, and can be used for accurate quantitative analysis of the harmful phase.
Description
Technical Field
The invention discloses a monomer separation method of a harmful phase of an isothermal forging die material for a turbine disc, and belongs to the technical field of high-temperature structural materials.
Background
High temperature alloys are used in large quantities for the manufacture of hot end components of aircraft engines, known as "the heart of gas turbines". The nickel-based superalloy is also a key material for manufacturing gas turbines for ship power and power generation, carrier rocket engines, hot end parts of ultra-supercritical power station units, chemical engineering fields, ocean engineering equipment and isothermal forging dies. The turbine disk is an important core hot end part of an aeroengine, the working condition of the turbine disk is extremely severe, the turbine disk bears complex thermal and mechanical loads during flight, and all parts bear stress and temperatureLikewise, the material of the turbine disk is required to have sufficient mechanical properties, in particular as high a fatigue resistance as possible, a durability and a good creep resistance in the temperature range in which it is used. At present, most of advanced gas turbines adopt powder high-temperature alloy to prepare turbine disks, and isothermal forging is not required to form the turbine disks, so that the performance and the service life of isothermal forging die materials become key factors for preparing the turbine disks. The existing isothermal forging die material for the turbine disc sometimes generates harmful phases in the preparation process, such as thick, hard and brittle M6The C carbide phase, directly affects the performance and life of the mold. Isothermal forging dies containing a large amount of deleterious phases have been found to have a reduction in tensile strength of about 50MPa at 1100 c, a 50% reduction in endurance life at 1100 c, and are highly susceptible to cracking after use. In the manufacturing process of the large-size isothermal forging die, because the section is thick and the cooling speed is low, severe macrosegregation sometimes occurs to cause harmful phases and uneven distribution characteristics, and the weight percentage of the harmful phases needs to be accurately measured when evaluating the macrosegregation degree, so that the acquisition and quantitative characterization of the monomer of the harmful phases of the isothermal forging die material for the turbine disc have important significance.
Disclosure of Invention
The invention provides a monomer separation method of a harmful phase of a nickel-based superalloy material for a turbine disc isothermal forging die aiming at overcoming the defects in the prior art, and aims to solve the problems that the traditional electrolytic extraction method can only separate the harmful phase and a strengthening precipitation phase in the material for the turbine disc isothermal forging die from a matrix in a mixed state and can not separate the harmful phase from the matrix in a monomer manner. The method is successfully applied to the monomer separation and accurate quantitative characterization of the harmful phase of the isothermal forging die material for the turbine disc, and can also be used for selective monomer separation of precipitated phases of other metal materials.
The purpose of the invention is realized by the following technical scheme:
the method for separating the monomer of the harmful phase of the isothermal forging die material for the turbine disc comprises the steps of firstly, electrolytically extracting an electrolytic extraction mixed solution containing the harmful phase and a strengthening phase from a sample of the isothermal forging die material for the turbine disc, adding glycerol into the mixed solution for adjusting viscosity after electrolysis is finished, wherein the volume ratio of the added volume of the glycerol to the volume of the electrolytic extraction mixed solution is (0.8-1.2): 4, stirring, then, filling the mixture into a measuring cylinder, standing for more than 2 hours, then sucking away 90% of liquid above the bottom of the measuring cylinder, obtaining the solution only containing the harmful phase by utilizing the selectivity of the settling rate of suspended particles according to the density difference of the harmful phase and other phases in different liquid viscosities, and finally, diluting the solution by pure alcohol and finally separating the monomer harmful phase from the residual liquid at the bottom of the measuring cylinder.
In practice, the step of electrolytically extracting a mixed solution of a harmful phase and a strengthening phase from the isothermal die forging material for turbine disks is as follows:
step one, preparing an electrolytic extraction solution with a formula of 100ml hydrochloric acid and 900ml methanol, and fully and uniformly stirring;
injecting an electrolytic extraction solution into an electrolytic tank of a glass container, taking stainless steel as a cathode, electrolyzing the isothermal forging die material sample for the turbine disc, taking out the isothermal forging die material sample for the turbine disc from the electrolytic tank every 0.5h, wiping the surface of the sample by using the end part of a latex tube sleeved on a glass rod, spraying alcohol to flush the end part of the latex tube attached to the glass rod and the residue on the surface of the test rod, collecting the residue in a beaker, wherein about 50ml of liquid in the beaker after each operation is used, and then continuously electrolyzing; repeating the operation for 4 times, wiping the turbine disc for the last time, immersing the test bar in the used electrolyte, and oscillating and cleaning by using an ultrasonic oscillator;
step three, washing the cathode by using methanol after the electrolysis is finished, and converging the washing liquid and the ultrasonically vibrated electrolyte into the electrolyte in the electrolytic cell;
and step four, standing the electrolyte in the electrolytic cell for more than 2 hours, sucking 80% of the liquid on the upper layer by using a suction pipe, transferring the residual liquid on the bottom of the electrolytic cell and the precipitate to the beaker containing the 4 times of flushing liquid and collecting the residue, and obtaining the electrolytic extraction mixed solution of the harmful phase and the strengthening phase.
Further, the total time of repeating the operation of the second step for 4 times of electrolytic extraction is not less than 2 h.
Further, the current density at which the sample of the isothermal forging die material for turbine disks was electrolyzed in the second step was 50mA/cm2。
Further, the time for the ultrasonic oscillator to oscillate and clean in the step two is 10 min.
The electrowinning operation of the above-described process is capable of separating all precipitated phases, including deleterious phases and other strengthening phases, from the alloy matrix.
In practice, the isothermal forging die material samples for turbine disks are cut from the isothermal forging die to be analyzed and processed into round bars of phi 5-10mm X50-100 mm, polished and weighed on an analytical balance.
In the implementation, when the monomer harmful phase in the residual liquid precipitated at the bottom of the discharge cylinder is separated by using the pure alcohol, the pure alcohol with the volume more than 5 times that of the residual liquid is added, the solution is absorbed after stirring, and the pure alcohol is used for washing twice, so that the monomer harmful phase without the residual solution is separated. The operation is to dilute the viscous solution with harmful phase residue with a large amount of alcohol, then suck most of the upper solution, and naturally dry to obtain the harmful phase monomer without residual solution. The obtained monomer can be used for quantitative (weight percentage) analysis, three-dimensional morphology analysis, chemical composition analysis, structural analysis and the like.
The technical scheme of the invention separates the harmful phase from the mixed phase extracted by electrolysis by utilizing the density difference between the harmful phase and other phases and the settling rate selectivity of the harmful phase and other phases in proper liquid viscosity, and after the electrolysis extraction is finished, proper amount of glycerin is selected and added into the mixed solution containing the electrolysis extraction phase, the harmful phase with higher density sinks in the process of standing, other strengthening phases with lower density are suspended in the solution, and most other strengthening phases in the suspension are sucked away by a suction pipe, so that the harmful phase is independently preserved. The method overcomes the defect that the traditional method can only separate the harmful phase and the strengthening precipitation phase in the isothermal forging die nickel-based superalloy material for the turbine disc from the matrix in a mixed state and cannot separate the harmful phase by monomer, and further separates solid harmful phase entities by utilizing the selectivity of the settling rate of suspended matters according to the performance of density difference of the harmful phase and other phases in different settling rates of proper liquid viscosity on the basis of electrolytically extracting the mixture of the harmful phase and the strengthening phase from the matrix, thereby realizing the monomer separation of the harmful phase of the isothermal forging die material for the turbine disc. The method can also be used for separating and characterizing precipitated phase monomers of other metal materials.
The technical scheme of the invention has the following advantages:
firstly, the problem that the existing electrolytic extraction technology can only extract all precipitated phases from a matrix but cannot distinguish various precipitated phases is solved, and harmful phases in the isothermal forging die material for the turbine disc can be separated in a single body;
secondly, the characteristics of density difference between the harmful phase and the strengthened precipitated phase are fully utilized, the single-phase entity of the harmful phase is separated independently through the sedimentation rate difference of the precipitated phase obtained by electrolysis in the liquid with specific viscosity, the purity of the harmful phase in the extracted phase can reach more than 99 percent, and the yield can reach 99.14 percent (the loss and dispersion rate of the harmful phase is less than 0.86 percent);
thirdly, compared with the two-dimensional image method which can only obtain the area percentage of the harmful phase, the method can accurately obtain the three-dimensional shape of the monomer harmful phase and the weight ratio of the harmful phase in the matrix;
fourthly, the size of the harmful phase can be measured and counted after the harmful phase of the monomer is separated;
fifthly, interference factors of the matrix can be eliminated, and the structure and the component of the harmful phase can be analyzed more conveniently and accurately;
sixthly, the glycerol is adopted as an additive and is easily dissolved into the existing electrolytic extraction mixed solution and pure alcohol, the solution viscosity can be conveniently adjusted and the subsequent dilution and removal are convenient, and the harmful phase is stable in the glycerol and can not be converted;
seventhly, pure alcohol is used as a diluting solvent, so that the efficiency of extracting residues of the harmful phase monomer from the glycerol can be greatly improved, a viscous glycerol solution can be quickly removed, and meanwhile, the harmful phase monomer can be quickly and naturally dried in the later period.
Detailed Description
The technical solution of the present invention will be further described with reference to the following examples:
example 1
The method for separating the harmful phases of the isothermal forging die nickel-based superalloy material for the turbine disc by using the method comprises the following steps:
(1) machining a round bar with the diameter of 10mm X80 mm from an isothermal forging die to be analyzed, polishing the surface of the round bar, and weighing the round bar on an analytical balance;
(2) preparing an electrolytic extraction solution with a formula of 100 hydrochloric acid and 900ml of methanol, and fully and uniformly stirring;
(3) pouring the solution into an electrolytic tank of a glass container, electrolyzing with stainless steel as cathode at a current density of 50mA/cm2Taking out samples every 0.5h, wiping the surface of the samples by using the end part of a latex tube sleeved on a glass rod, spraying alcohol by using a wash bottle filled with the alcohol, washing off residues attached to the surface of the test rod, collecting the residues in a beaker, wherein the volume of the liquid is about 50ml, and then continuously electrolyzing until the steps are repeated for 4 times, wherein the time is 2 hours; after wiping the sample for the last time, immersing the test bar in the used electrolyte, and oscillating for 10min on an ultrasonic oscillator;
(4) after the electrolytic extraction, the cathode is washed by methanol, and the washing liquid and the electrolyte after ultrasonic oscillation are converged into the electrolyte in the electrolytic cell;
(5) standing the electrolyte in the electrolytic cell for 2h, sucking off 800ml of the upper layer of electrolyte by using a straw to obtain 200ml of the remaining electrolyte, transferring the remaining electrolyte and the precipitate to a sample containing 200ml of the surface scouring solution for 4 times of scouring (50 ml each time), wherein the total volume of the sample is 400ml, and the harmful phase (M) is mainly contained in the mixed solution6C) And small amounts of carbides, borides (MC, M)3B2) A mixture of (a).
(6) Adding 80ml of glycerol into 400ml of the mixed liquid containing the mixed extraction phase in the step 5, filling the mixture into a cylindrical measuring cylinder through vigorous stirring, standing for 2 hours, and then sucking 90% of liquid away. At the moment, according to the performances of the density difference of the harmful phase and other phases in different liquid viscosities, the solution only containing the harmful phase is obtained by utilizing the selectivity of the sedimentation rate of suspended particles;
(7) adding 5 times of pure alcohol to the residual solution containing extraction residue (only harmful phase), stirring, standing for 10min, sucking off the solution, washing with pure alcohol twice, naturally drying, and separating out harmful monomer phase without residual solution.
(8) The separated harmful phase is M detected by X-ray6Type C carbide noxious phase, free of MC carbide and M3B2Boride diffraction peak.
Example 2
The method for separating the harmful phases of the isothermal forging die nickel-based superalloy material for the turbine disc by using the method comprises the following steps:
(1) machining a round bar with the diameter of 10mm X80 mm from an isothermal forging die to be analyzed, polishing the surface of the round bar, and weighing the round bar on an analytical balance;
(2) preparing an electrolytic extraction solution with a formula of 100ml hydrochloric acid and 900ml methanol, and fully and uniformly stirring;
(3) pouring the solution into an electrolytic tank of a glass container, electrolyzing with stainless steel as cathode at a current density of 50mA/cm2Taking out samples every 0.5h, wiping the surface of the samples by using the end part of a latex tube sleeved on a glass rod, spraying alcohol by using a wash bottle filled with the alcohol, washing off residues attached to the surface of the test rod, collecting the residues in a beaker, wherein the volume of the liquid is about 50ml, and then continuously electrolyzing until the steps are repeated for 4 times, wherein the time is 2 hours; after wiping the sample for the last time, immersing the test bar in the used electrolyte, and oscillating for 10min on an ultrasonic oscillator;
(4) after the electrolytic extraction, the cathode is washed by methanol, and the washing liquid and the electrolyte after ultrasonic oscillation are converged into the electrolyte in the electrolytic cell;
(5) standing the electrolyte in the electrolytic cell for 2h, sucking off 800ml of the upper layer of electrolyte by using a suction pipe, leaving 200ml, transferring the electrolyte and the precipitate to a sample containing 200ml of surface scouring solution for 4 times of scouring (about 50ml each time), counting 400ml of liquid, wherein the harmful phase (M) is mainly in the mixed solution6C) And a small amount of carbonizationCompound and boride (MC, M)3B2) A mixture of (a).
(6) Adding 120ml of glycerol into 400ml of the mixed liquid containing the mixed extraction phase in the step 5, filling the mixture into a cylindrical measuring cylinder through vigorous stirring, standing for 2 hours, and then sucking 90% of liquid away. At the moment, according to the performances of the density difference of the harmful phase and other phases in different liquid viscosities, the solution only containing the harmful phase is obtained by utilizing the selectivity of the sedimentation rate of suspended particles;
(7) adding 5 times of pure alcohol to the residual solution containing extraction residue (only harmful phase), stirring, standing for 10min, sucking off the solution, washing with pure alcohol twice, naturally drying, and separating out harmful monomer phase without residual solution.
(8) The separated harmful phase is M detected by X-ray6Type C carbide noxious phase, free of MC carbide and M3B2Boride diffraction peak.
The density difference of the harmful phase and other strengthening phases and the sedimentation rate difference of the harmful phase and the other strengthening phases in the liquid with specific viscosity are utilized, and the liquid viscosity is improved by adding proper content of glycerin into the mixed solution of the electrolytic extraction, so that the harmful phase with higher density is settled and the other strengthening phases are suspended. If the proportion of glycerin is too low, the solution viscosity is insufficient, other strengthening phases with lower density can not effectively suspend, and part of strengthening phases sink to the bottom and are mixed with harmful phases; if the proportion of the glycerol is too high, the solution viscosity is excessive, so that part of harmful phases cannot effectively sink and are mixed and suspended with other strengthening phases, and the separation effect of the harmful phases from the monomers in the mixed solution is influenced. Experiments show that the ratio of glycerol to the mixed solution is (0.8-1.2): 4, proper viscosity and proper separation and sedimentation rate can be obtained, and good harmful phase monomer separation effect is obtained.
Claims (9)
1. A monomer separation method of harmful phases of isothermal forging die materials for turbine discs is characterized by comprising the following steps: the method comprises the steps of firstly, carrying out electrolytic extraction on a mixed solution containing a harmful phase and a plurality of strengthening phases from an isothermal forging die material for a turbine disc, adding a proper amount of glycerol into the electrolytic extraction mixed solution to adjust the viscosity of the solution after the electrolysis is finished, and further independently separating a solid harmful phase single-phase entity by utilizing the density difference of the harmful phase and the strengthening phase and the sedimentation rate difference of the harmful phase and the strengthening phase in a liquid with a specific viscosity.
2. The method for separating a harmful phase of an isothermal die forging material for a turbine disk according to claim 1, wherein: and after the electrolysis is finished, the volume ratio of the added volume of the glycerol to the volume of the mixed solution of the electrolytic extraction is (0.8-1.2): 4, the glycerol is stirred and then is filled into a measuring cylinder to be stood for more than 2 hours, so that the harmful phase with high density is settled at the bottom of the solution, the other strengthening phases with low density are suspended in the solution, and then a suction pipe is adopted to suck 90% of the liquid above the bottom of the measuring cylinder. Finally, pure alcohol is used for further diluting the residual viscous solution with the deposited harmful phase monomer, the upper solution is sucked, and finally the harmful phase monomer in the residual liquid at the bottom of the discharge cylinder is separated.
3. The method for separating a harmful phase of an isothermal die forging material for a turbine disk according to claim 1, wherein: the phase contained in the mixed solution extracted by electrolysis in the isothermal forging die material for the turbine disc is mainly coarse hard brittle tungsten-rich M with higher density6A mixture of harmful phases of C-type carbide and strengthening phases of MC-type carbide and boride with lower density.
4. The method for separating a harmful phase of an isothermal die forging material for a turbine disk according to claim 1, wherein: the step of electrolytically extracting the mixed solution of the harmful phase and the strengthening phase from the isothermal forging die material for the turbine disc comprises the following steps:
step one, preparing an electrolytic extraction solution with a formula of 100ml hydrochloric acid and 900ml methanol, and fully and uniformly stirring;
injecting an electrolytic extraction solution into an electrolytic bath of a glass container, taking stainless steel as a cathode, electrolyzing the isothermal forging die material sample for the turbine disc, taking out the isothermal forging die material sample for the turbine disc from the electrolytic bath every 0.5h, wiping the surface of the sample by using the end part of a latex tube sleeved on a glass rod, spraying alcohol to flush the latex tube attached to the glass rod and residues on the surface of the test rod, collecting the residues in a beaker, wherein about 50ml of liquid in the beaker after each operation is carried out, and then continuously electrolyzing; repeating the operation for 4 times, wiping the turbine disc for the last time, immersing the test bar in the used electrolyte, and oscillating and cleaning by using an ultrasonic oscillator;
step three, washing the cathode by using methanol after the electrolysis is finished, and converging the washing liquid and the ultrasonically vibrated electrolyte into the electrolyte in the electrolytic cell;
and step four, standing the electrolyte in the electrolytic cell for not less than 2 hours, sucking 80% of the liquid on the upper layer by using a suction pipe, transferring the residual liquid on the bottom of the electrolytic cell and the precipitate to the beaker containing the 4 times of flushing liquid and collecting the residue, and obtaining the electrolytic extraction mixed solution of the harmful phase and the strengthening phase.
5. The method for separating a harmful phase of an isothermal die forging material for a turbine disk according to claim 4, wherein: and repeating the operation of the second step for 4 times, wherein the total time of electrolytic extraction is not less than 2 h.
6. The method for separating a harmful phase of an isothermal die forging material for a turbine disk according to claim 4, wherein: in the second step, the current density for electrolyzing the isothermal forging die material sample for the turbine disc is 50mA/cm2。
7. The method for separating a harmful phase of an isothermal die forging material for a turbine disk according to claim 4, wherein: and the time for the ultrasonic oscillator to oscillate and clean in the step two is 10 min.
8. The method for separating a harmful phase of an isothermal die forging material for a turbine disk according to claim 1, wherein: the isothermal forging die material sample for the turbine disk is cut from the isothermal forging die to be analyzed and processed into a round bar of phi 5-10mm X50-100 mm, polished, and weighed on an analytical balance.
9. The method for separating a harmful phase of an isothermal die forging material for a turbine disk according to claim 2, wherein: when the monomer harmful phase in the residual liquid at the bottom of the measuring cylinder is diluted by pure alcohol, the pure alcohol with the volume more than 5 times that of the residual liquid is added, the solution is absorbed after the stirring and the standing for 10min, the solution is washed twice by the alcohol, and the monomer harmful phase without the residual solution can be separated after the natural drying.
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Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101418381A (en) * | 2008-11-28 | 2009-04-29 | 东北大学 | Method for purifying non-metal inclusion in magnesium alloy by ultrasonic agglomeration |
CN101545887A (en) * | 2008-03-28 | 2009-09-30 | 中国科学院金属研究所 | Quantitative analysis method for boride |
CN108896378A (en) * | 2018-06-13 | 2018-11-27 | 中国航发北京航空材料研究院 | A kind of the electrobrightening corrosive agent and its application method of high temperature alloy |
CN109342254A (en) * | 2018-09-19 | 2019-02-15 | 中国航发北京航空材料研究院 | A kind of method of fast quantitative analysis high temperature alloy inclusion content |
CN109763165A (en) * | 2019-02-22 | 2019-05-17 | 江苏科技大学 | The electrolytic etching method of precipitation phase in a kind of cobalt-base alloys |
CN110003391A (en) * | 2019-04-03 | 2019-07-12 | 黎明职业大学 | Collect polymerization, pore-forming, the method for being granulated synchronous preparation high water absorption rate aggregation object |
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 |
CN111579323A (en) * | 2020-05-09 | 2020-08-25 | 中国航发北京航空材料研究院 | High-throughput preparation and test method of powder superalloy inclusion sample |
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 |
CN116818483A (en) * | 2023-05-31 | 2023-09-29 | 钢铁研究总院有限公司 | Quantitative analysis sample dissolving method for high-stability precipitated phase in high-carbon steel |
-
2020
- 2020-11-03 CN CN202011213696.8A patent/CN112553679B/en active Active
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101545887A (en) * | 2008-03-28 | 2009-09-30 | 中国科学院金属研究所 | Quantitative analysis method for boride |
CN101418381A (en) * | 2008-11-28 | 2009-04-29 | 东北大学 | Method for purifying non-metal inclusion in magnesium alloy by ultrasonic agglomeration |
CN108896378A (en) * | 2018-06-13 | 2018-11-27 | 中国航发北京航空材料研究院 | A kind of the electrobrightening corrosive agent and its application method of high temperature alloy |
CN109342254A (en) * | 2018-09-19 | 2019-02-15 | 中国航发北京航空材料研究院 | A kind of method of fast quantitative analysis high temperature alloy inclusion content |
CN109763165A (en) * | 2019-02-22 | 2019-05-17 | 江苏科技大学 | The electrolytic etching method of precipitation phase in a kind of cobalt-base alloys |
CN110003391A (en) * | 2019-04-03 | 2019-07-12 | 黎明职业大学 | Collect polymerization, pore-forming, the method for being granulated synchronous preparation high water absorption rate aggregation object |
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 |
CN111579323A (en) * | 2020-05-09 | 2020-08-25 | 中国航发北京航空材料研究院 | High-throughput preparation and test method of powder superalloy inclusion sample |
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 |
CN116818483A (en) * | 2023-05-31 | 2023-09-29 | 钢铁研究总院有限公司 | Quantitative analysis sample dissolving method for high-stability precipitated phase in high-carbon steel |
Non-Patent Citations (1)
Title |
---|
李玲霞 等: "高温轴承钢中析出相的表征", 冶金分析, vol. 37, no. 8, pages 9 - 141 * |
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