CN117871202A - Extraction method and electrolysis device for inclusions in iron-based superalloy for turbine blades - Google Patents
Extraction method and electrolysis device for inclusions in iron-based superalloy for turbine blades Download PDFInfo
- Publication number
- CN117871202A CN117871202A CN202410043688.5A CN202410043688A CN117871202A CN 117871202 A CN117871202 A CN 117871202A CN 202410043688 A CN202410043688 A CN 202410043688A CN 117871202 A CN117871202 A CN 117871202A
- Authority
- CN
- China
- Prior art keywords
- electrolysis
- workpiece
- electrolyte
- inclusions
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 80
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 16
- 238000000605 extraction Methods 0.000 title claims abstract description 14
- 229910000601 superalloy Inorganic materials 0.000 title claims description 19
- 239000003792 electrolyte Substances 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000000956 alloy Substances 0.000 claims abstract description 44
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 43
- 238000004140 cleaning Methods 0.000 claims abstract description 30
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 20
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical class OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 10
- 239000011780 sodium chloride Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000003754 machining Methods 0.000 claims abstract description 9
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 43
- 238000000926 separation method Methods 0.000 claims description 27
- 239000000126 substance Substances 0.000 claims description 20
- 239000012535 impurity Substances 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 11
- 238000004090 dissolution Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- 230000010355 oscillation Effects 0.000 claims 1
- 238000000746 purification Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 239000000463 material Substances 0.000 description 19
- 238000009826 distribution Methods 0.000 description 8
- 238000011161 development Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910018575 Al—Ti Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of inclusions in high-temperature alloys, and discloses an extraction method and an electrolysis device for inclusions in iron-based high-temperature alloys for turbine blades, wherein a machining mode is adopted to cut a block-shaped workpiece; putting the cut workpiece into an ultrasonic cleaner for vibration cleaning; the electrolyte is electrolyzed by adopting aqueous solution after drying, and the electrolyte comprises the following components in parts by mass: 1% of ferric chloride, 1% of sodium chloride and the balance of distilled water; the electrolysis temperature is controlled to be 20-25 ℃ in a water bath, the voltage is constant to be 10V, and electrolyte is replaced once every 180min of electrolysis until the workpiece is completely electrolyzed. Separating the electrolytic product and the liquid by a centrifugal machine, wherein the rotating speed is 5000r/s, and the time is 5min; repeatedly cleaning with deionized water; putting the obtained electrolysis product into saturated oxalic acid and 10% concentrated nitric acid solution, and soaking for 12h; and (3) repeatedly washing and drying the acidolysis product separated by the centrifugal machine by deionized water to finally obtain the high-temperature alloy inclusion.
Description
Technical Field
The invention designs a research method of inclusions in a superalloy, and particularly relates to a method for extracting inclusions in an iron-based superalloy for a turbine blade and an electrolysis device.
Background
K213 is Fe-Ni-Cr base casting superalloy, which is mainly added with Al-Ti to form gamma' phase for precipitation strengthening, and added with a certain amount of W for solid solution strengthening and trace boron for strengthening grain boundary. The alloy has good casting technological property, and good comprehensive performance and tissue stability below 750 ℃. The iron-based superalloy has the defects of poor structural stability and oxidation resistance of the alloy and insufficient high-temperature performance. But has low cost and good medium temperature performance. Iron-based superalloys are widely used on different engine turbine disks below 750 ℃.
The high-temperature alloy has low return material availability, a large amount of return materials are not fully utilized, and the core technology of pretreatment and recycling of the return materials is mainly lacked. Therefore, the system researches the characteristics and the formation mechanism of the types, the sizes, the contents, the distribution and the like of the inclusions in the alloy, and has very important significance for purifying and smelting the high-temperature alloy return material and safely and effectively playing the alloy performance.
Disclosure of Invention
The invention aims to provide a method for extracting inclusions in an iron-based superalloy for a turbine blade.
The invention relates to a method for extracting inclusions in an iron-based superalloy for a turbine blade, which comprises the following steps:
(1) Preparing a workpiece: cutting a blocky workpiece at the position of an inclusion enrichment area in a turbine blade in a machining mode; placing the cut workpiece into an ultrasonic cleaner to be subjected to vibration cleaning for about 10 minutes;
(2) Preparing an electrolyte: adopting aqueous solution for electrolysis, wherein the electrolyte comprises the following components in parts by mass: 1% of ferric chloride, 1% of sodium chloride and the balance of distilled water;
(3) Preparing an acid dissolution liquid: the chemical separation is adopted, and the acid solution is as follows: saturated oxalic acid and 10% concentrated nitric acid solution;
(4) Electrolyzing an aqueous solution: connecting the workpiece obtained in the first step with an electrolysis device to ionize; the electrolysis adopts a constant voltage method, the electrolysis temperature is controlled to be about 20 ℃ in a water bath, the voltage is constant to be 10V, and electrolyte is replaced once every 180min of electrolysis until the workpiece is completely electrolyzed;
(5) Physical separation and cleaning: separating the electrolytic product and the liquid by a centrifugal machine, wherein the rotating speed is 5000r/s, and the time is 5min; repeatedly cleaning with deionized water, and drying to obtain an electrolytic product;
(6) Chemical separation: putting the electrolysis product obtained in the fifth step into saturated oxalic acid and 10% concentrated nitric acid solution, and soaking for 12h;
(7) Cleaning and collecting: and repeatedly washing the acidolysis product obtained in the sixth step with deionized water, and drying to finally obtain the inclusion in the high-temperature alloy.
Further, in the step, the experiment was performed at room temperature under normal atmospheric pressure.
In the present invention, the connection relationship of the respective devices of the conventional electrolysis apparatus of the extraction method of inclusions in iron-based superalloy for turbine blades is as follows:
water bath (1): a container for holding electrolyte provides a stable temperature environment for electrolysis.
Filter paper (2): is typically located inside the electrolytic cell for filtering solid impurities in the electrolyte.
Alloy workpiece (anode) (3): the workpiece to be electrolyzed is connected to the anode of the electrolysis apparatus.
Cathode (4): the cathode of the electrolysis apparatus is immersed in the electrolyte together with the anode (alloy workpiece).
Anode clamp (5): means for securing and connecting the anode (alloy workpiece) to a power source.
Thermometer (6): for monitoring the temperature of the electrolyte, ensuring that the electrolysis process is carried out at a constant temperature.
Beaker (7): for loading electrolyte, placed in a water bath.
Power supply (8): the electrolyzer is powered and connected to an anode clamp (attached to the alloy workpiece) and to a cathode.
The connection mode is as follows: the alloy workpiece is connected to the anode end of the power supply through an anode clamp, and the cathode is directly connected to the cathode end of the power supply. Thus, when the power supply is turned on, an electric current passes through the alloy workpiece (anode) and the electrolyte to the cathode, thereby achieving electrolysis. Meanwhile, the thermometer is used for monitoring the temperature in the water bath in real time so as to ensure the temperature control of the electrolysis process.
In combination with the technical scheme and the technical problems to be solved, the technical scheme to be protected has the following advantages and positive effects:
firstly, the electrolysis device is simple, and has no strict requirements on the size, weight and surface smoothness of a sample; the electrolyte has simple preparation components, no volatilization, no pollution and little energy consumption in the electrolysis process; the electrolytic product is soaked by saturated oxalic acid and 10% concentrated nitric acid solution to separate out impurities, the operation process is simple, efficient and pollution is small, and the impurities in the iron-based high-temperature alloy can be extracted comprehensively without damage.
The whole experimental device is simple and convenient to assemble, convenient to operate, free of strict requirements on raw material samples, low in energy consumption and pollution in the whole process, convenient to collect the obtained product, and capable of completely and comprehensively obtaining the inclusions in the material.
The expected benefits and commercial values after the technical scheme of the invention is converted are as follows: saving the cost of the collecting and processing device, the cost of raw material treatment, the cost of experimental consumables and the pollution treatment cost. The product obtained by the technology is beneficial to researching the performance of the material and has important significance for improving the application range and the service life of the material.
Second, the process flow of the present invention describes a method for extracting inclusions from superalloy that combines machining, chemical treatment and physical separation techniques. The significant technological advances that this brings can be analyzed from several aspects:
1. improves the extraction purity and efficiency of the inclusion
Accurate positioning and extraction: the inclusion enrichment area in the turbine blade is precisely cut through machining, so that the accuracy and purity of inclusion extraction can be effectively improved.
Efficient chemical and physical treatment: the inclusion can be effectively separated by combining electrolysis and chemical dissolution, and meanwhile, the structural integrity and the component integrity of the inclusion are maintained, so that the extraction efficiency is improved.
2. Reducing environmental impact
Electrolyte and acid solution selection: the relatively environment-friendly chemicals such as ferric chloride, sodium chloride, oxalic acid and the like are adopted as the electrolyte and the dissolution liquid, so that the use of harmful chemicals is reduced, and the environmental pollution is reduced.
Energy saving and emission reduction: the voltage and the temperature in the electrolysis process are controlled, so that the whole process is more energy-efficient, and the energy consumption and the waste emission are reduced.
3. Improving the safety and controllability of operation
Strict temperature and voltage control: the temperature and the voltage are strictly controlled in the electrolysis process, so that the safety and the controllability of the operation are improved, and the risk in the operation process is reduced.
Automated physical separation: and the centrifugal machine is used for physical separation and cleaning, so that the automation degree of operation is improved.
4. Improves the economic benefit of the process
The material utilization rate is improved: through effectively extracting the inclusions, the high-temperature alloy material can be better utilized, and the economic value of the material is improved.
Energy and material cost are reduced: by optimizing the electrolysis and chemical treatment steps, the energy consumption and the use of chemical materials are reduced, and the cost of the whole process is reduced.
5. Promote the development of material science
Study of material properties: the inclusion extracted by the method can be used for further material property research, and promotes the development of the field of material science.
Development potential of new technology: this procedure also inspires innovation and development of other material extraction and processing techniques.
The process flow provided by the invention combines mechanical, chemical and physical methods, so that not only is the efficiency and purity of extracting the inclusion from the high-temperature alloy improved, but also the obvious technical progress is achieved in the aspects of environmental protection, operation safety, economic benefit, material science development and the like.
Drawings
FIG. 1 is a schematic view of a conventional electrolytic apparatus employed in the present invention, with reference numerals and corresponding names: 1-a water bath, 2-a filter paper, 3-an alloy workpiece (anode), 4-a cathode, 5-an anode clamp, 6-a thermometer, 7-a beaker and 8-a power supply;
FIG. 2 is a flow chart of a method for extracting alloy inclusions provided by an embodiment of the invention;
FIGS. 3 and 4 are morphology diagrams of an alloy inclusion scanning electron microscope according to a first embodiment of the present invention;
FIG. 5A is a graph showing the composition of the alloy inclusion scanning electron microscope shown in FIG. 4;
FIG. 5B is a view showing the Al distribution in the inclusions shown in FIG. 4;
FIG. 5C shows the Fe distribution in the inclusions shown in FIG. 4;
FIG. 5D is a graph showing the distribution of O in the inclusions shown in FIG. 4;
FIG. 5E shows the distribution of B in the inclusions shown in FIG. 4;
FIG. 5F shows the Cr distribution in the inclusions shown in FIG. 4;
FIG. 5G is a view showing the distribution of N in the inclusions shown in FIG. 4;
the inclusion composition shown in FIG. 5 was obtained from an oxynitride of iron, and a small amount of aluminum and chromium compounds.
Detailed Description
The following are two specific examples illustrating specific implementations of inclusion extraction from superalloy:
application example 1
Inclusions in high temperature alloys used in aircraft engines are extracted for material analysis and performance testing.
1) Preparing a workpiece:
a block-shaped workpiece containing an inclusion enrichment area is precisely cut from a turbine blade made of high-temperature alloy of an aero-engine by a precise machining method.
2) Cleaning a workpiece:
placing the cut workpiece into an ultrasonic cleaner, and cleaning the workpiece for 10 minutes by using distilled water to remove surface impurities.
3) Preparing an electrolyte:
preparing electrolyte according to the mass ratio: 1% of ferric chloride, 1% of sodium chloride and the balance of distilled water.
4) And (3) electrolytic treatment:
the cleaned workpiece is connected to an electrolysis device. The electrolysis was carried out in a water bath at 20℃with a voltage set at 10V, and the electrolyte was replaced every 180 minutes until the work piece was completely electrolyzed.
5) Physical separation:
the electrolysis product and the liquid were separated using a centrifuge at 5000 rpm for 5 minutes.
Repeatedly cleaning the electrolytic product with deionized water, and then drying.
6) Chemical separation:
the dried electrolytic product was put into a mixed solution of saturated oxalic acid and 10% concentrated nitric acid and immersed for 12 hours.
7) Final cleaning and collection:
repeatedly washing acidolysis products with deionized water, drying and collecting to obtain pure impurities.
The extracted inclusions were subjected to composition and structural analysis to evaluate their effect on superalloy properties.
Application example 2
Inclusions are extracted from superalloy for industrial gas turbines for material reuse studies.
1) Preparing a workpiece:
from the high-temperature alloy blade used in the industrial gas turbine, small workpieces containing the inclusion area are precisely cut by using a CNC machine tool.
2) Cleaning a workpiece:
the workpiece was cleaned in distilled water for 15 minutes using an ultrasonic cleaner with temperature control.
3) Preparing an electrolyte:
preparing electrolyte according to the weight ratio: 2% of ferric chloride, 2% of sodium chloride and the balance of distilled water.
4) And (3) electrolytic treatment:
the work piece was subjected to electrolysis in a constant temperature environment (about 25 ℃), the voltage being set at 12V, the electrolyte being replaced every 150 minutes, and continued until the work piece was completely electrolyzed.
5) Physical separation and washing:
separation was performed using a 6000 rpm centrifuge for 10 minutes.
Multiple washes with deionized water followed by drying.
6) Chemical separation:
the electrolytic product was immersed in a mixed solution of saturated oxalic acid and 15% concentrated nitric acid for 24 hours.
The invention relates to a method for extracting inclusions in an iron-based superalloy for a turbine blade, which comprises the following steps:
(1) Preparing a workpiece: cutting a blocky workpiece at the position of an inclusion enrichment area in a turbine blade in a machining mode; placing the cut workpiece into an ultrasonic cleaner to be subjected to vibration cleaning for about 10 minutes;
(2) Preparing an electrolyte: adopting aqueous solution for electrolysis, wherein the electrolyte comprises the following components in parts by weight: 1% of ferric chloride, 1% of sodium chloride and the balance of distilled water;
(3) Preparing an acid dissolution liquid: the chemical separation is adopted, and the acid solution is as follows: saturated oxalic acid and 10% concentrated nitric acid solution;
(4) Electrolyzing an aqueous solution: connecting the workpiece obtained in the first step with an electrolysis device to ionize; the electrolysis adopts a constant voltage method, the electrolysis temperature is controlled to be about 20 ℃ in a water bath, the voltage is constant to be 10V, and electrolyte is replaced once every 180min of electrolysis until the workpiece is completely electrolyzed;
(5) Physical separation and cleaning: separating the electrolytic product and the liquid by a centrifugal machine, wherein the rotating speed is 5000r/s, and the time is 5min; repeatedly cleaning with deionized water, and drying to obtain an electrolytic product;
(6) Chemical separation: putting the electrolysis product obtained in the fifth step into saturated oxalic acid and 10% concentrated nitric acid solution, and soaking for 12h;
(7) Cleaning and collecting: and repeatedly washing the acidolysis product obtained in the sixth step with deionized water, and drying to finally obtain the inclusion in the high-temperature alloy.
Further, the method comprises the steps of:
preparing a workpiece: cutting a blocky workpiece at the position of an inclusion enrichment area in a turbine blade in a machining mode; placing the cut workpiece into an ultrasonic cleaner to be subjected to vibration cleaning for about 10 minutes;
preparing an electrolyte: adopting aqueous solution for electrolysis, wherein the electrolyte comprises the following components in parts by weight: 1% of ferric chloride, 1% of sodium chloride and the balance of distilled water;
preparing an acid dissolution liquid: the chemical separation is adopted, and the acid solution is as follows: saturated oxalic acid and 10% concentrated nitric acid solution;
electrolyzing an aqueous solution: connecting the workpiece obtained in the first step with an electrolysis device to ionize; the electrolysis adopts a constant voltage method, the electrolysis temperature is controlled to be about 20 ℃ in a water bath, the voltage is constant to be 10V, and electrolyte is replaced once every 180min of electrolysis until the workpiece is completely electrolyzed;
physical separation and cleaning: separating the electrolytic product and the liquid by a centrifugal machine, wherein the rotating speed is 5000r/s, and the time is 5min; repeatedly cleaning with deionized water, and drying to obtain an electrolytic product;
chemical separation: putting the electrolysis product obtained in the fifth step into saturated oxalic acid and 10% concentrated nitric acid solution, and soaking for 12h;
cleaning and collecting: and repeatedly washing the acidolysis product obtained in the sixth step with deionized water, and drying to finally obtain the inclusion in the high-temperature alloy.
Application examples
In this embodiment, a turbine blade is taken as an example, and the turbine blade is K213 alloy. The method for extracting the inclusion in the iron-based superalloy for the turbine blade provided by the embodiment of the invention is used for separating and extracting the inclusion in the K213 alloy, and comprises the following specific steps:
the first step: preparing a workpiece:
cutting a block-shaped workpiece at the position of an inclusion enrichment area in a turbine blade, wherein the workpiece size is 20mm multiplied by 20mm; placing the cut workpiece into an ultrasonic cleaner for vibration cleaning for 10min;
and a second step of: preparing an electrolyte:
the electrolyte comprises the following components in parts by weight: 1% of ferric chloride, 1% of sodium chloride and the balance of distilled water;
and a third step of: preparing an acid dissolution liquid:
the acid dissolution liquid is as follows: saturated oxalic acid and 10% concentrated nitric acid solution;
fourth step: electrolyzing an aqueous solution:
the electrolytic device is connected as shown in FIG. 1; the electrolysis is carried out by adopting a constant voltage method, the electrolysis temperature is controlled at 25 ℃ in a water bath, the voltage is constant at 10V, electrolyte is replaced once every 180min of electrolysis until the workpiece is completely electrolyzed, and filter paper is used for collecting metal slag and impurities after electrolysis;
fifth step: physical separation and cleaning:
after the electrolysis is completed, taking out filter paper, separating the product by using a centrifugal machine, wherein the rotating speed is 5000r/s, the time is 5min, taking out the solid obtained by separation, repeatedly cleaning with deionized water, and drying to obtain an electrolysis product; taking a small amount of electrolysis products by using a medicine spoon for observation by a scanning electron microscope;
sixth step: chemical separation:
putting the electrolysis product obtained in the fifth step into saturated oxalic acid and 10% concentrated nitric acid solution, soaking for 12 hours, and exposing impurities in the electrolysis product;
seventh step: cleaning and collecting:
repeatedly washing the impurities obtained in the sixth step with deionized water, collecting the impurities on a centrifugal machine, and drying the impurities to finally obtain the impurities in the high-temperature alloy.
Eighth step: scanning electron microscope analysis:
and placing the impurities collected after the electrolytic extraction of the alloy sample on a single-sided conductive adhesive, and placing the single-sided conductive adhesive into a scanning electron microscope for analysis of the morphology and the size of the impurities, as shown in fig. 3 and 4. And analyzed for its composition using energy spectra, as shown in fig. 4 for the elemental distribution in fig. 4. Thereby determining the basic size of the inclusions between 20 and 40 mu m, the shapes of the inclusions are mainly blocky and spherical, and the inclusions are mainly composed of Al 2 O 3 、CrO 2 、CrO 2 、Cr 2 N、AlN、Cr 3 B 4 Oxides, nitrides, and borides of Fe 2B. In the present invention, the connection relationship of the respective devices of the conventional electrolysis apparatus of the extraction method of inclusions in iron-based superalloy for turbine blades is as follows:
water bath (1): a container for holding electrolyte provides a stable temperature environment for electrolysis.
Filter paper (2): is typically located inside the electrolytic cell for filtering solid impurities in the electrolyte.
Alloy workpiece (anode) (3): the workpiece to be electrolyzed is connected to the anode of the electrolysis apparatus.
Cathode (4): the cathode of the electrolysis apparatus is immersed in the electrolyte together with the anode (alloy workpiece).
Anode clamp (5): means for securing and connecting the anode (alloy workpiece) to a power source.
Thermometer (6): for monitoring the temperature of the electrolyte, ensuring that the electrolysis process is carried out at a constant temperature.
Beaker (7): for loading electrolyte, placed in a water bath.
Power supply (8): the electrolyzer is powered and connected to an anode clamp (attached to the alloy workpiece) and to a cathode.
The connection mode is as follows: the alloy workpiece is connected to the anode end of the power supply through an anode clamp, and the cathode is directly connected to the cathode end of the power supply. Thus, when the power supply is turned on, an electric current passes through the alloy workpiece (anode) and the electrolyte to the cathode, thereby achieving electrolysis. Meanwhile, the thermometer is used for monitoring the temperature in the water bath in real time so as to ensure the temperature control of the electrolysis process.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.
Claims (9)
1. The method for extracting the inclusions in the iron-based superalloy for the turbine blade is characterized by comprising the following steps of:
preparing a workpiece: cutting a blocky workpiece at the position of an inclusion enrichment area in a turbine blade in a machining mode; putting the cut workpiece into an ultrasonic cleaner for vibration cleaning;
preparing an electrolyte: adopting aqueous solution for electrolysis, wherein the electrolyte comprises the following components in parts by mass: 1% of ferric chloride, 1% of sodium chloride and the balance of distilled water;
preparing an acid dissolution liquid: the chemical separation is adopted, and the acid solution is as follows: saturated oxalic acid and 10% concentrated nitric acid solution;
electrolyzing an aqueous solution: connecting the workpiece obtained in the first step with an electrolysis device to ionize; the electrolysis adopts a constant voltage method, the electrolysis temperature is controlled to be about 20 ℃ in a water bath, the voltage is constant to be 10V, and electrolyte is replaced once every 180min of electrolysis until the workpiece is completely electrolyzed;
physical separation and cleaning: separating the electrolytic product and the liquid by a centrifugal machine, wherein the rotating speed is 5000r/s, and the time is 5min; repeatedly cleaning with deionized water, and drying to obtain an electrolytic product;
chemical separation: putting the electrolysis product obtained in the fifth step into saturated oxalic acid and 10% concentrated nitric acid solution, and soaking for 12h;
cleaning and collecting: and repeatedly washing the acidolysis product obtained in the sixth step with deionized water, and drying to finally obtain the inclusion in the high-temperature alloy.
2. The method according to claim 1, wherein in the workpiece preparation step, a block-shaped workpiece is cut at the position of the inclusion enrichment area in the turbine blade by means of machining to ensure maximum collection of inclusions;
the method comprises the steps of placing a cut workpiece into an ultrasonic cleaner, and cleaning by utilizing the oscillation action of ultrasonic waves for about 10 minutes to remove greasy dirt and impurities on the surface of the workpiece.
3. The method according to claim 1, wherein in the step of preparing the electrolyte, water is used as a solvent, and 1% of ferric chloride and 1% of sodium chloride are added according to the mass ratio, and the balance is distilled water, so that the electrolyte has good conductivity and stability, and is suitable for high-efficiency electrolysis.
4. The method according to claim 1, wherein in the step of electrolyzing the aqueous solution, the work piece and the electrolysis apparatus are connected to perform electrolysis, and a constant voltage method is adopted during electrolysis, and the electrolysis temperature is controlled to be about 20 ℃ in a water bath, the voltage is kept constant at 10V, and the electrolyte is replaced every 180 minutes until the work piece is completely electrolyzed, so that the complete and effective extraction of the impurities is ensured.
5. The method according to claim 1, wherein in the physical separation and washing step, the electrolyzed liquid is separated by using a centrifuge, the centrifugal speed is set to 5000r/s, and the centrifugal time is set to 5 minutes, so as to realize rapid separation of the electrolysis product and the liquid; and then repeatedly cleaning with deionized water, and drying to obtain an electrolysis product, thereby further reducing impurities in the impurities.
6. The method according to claim 1, wherein in the chemical separation step, the electrolytic product is put into a saturated oxalic acid and 10% concentrated nitric acid solution, and immersed for 12 hours to ensure sufficient reaction and separation of inclusions; and then repeatedly washing with deionized water, and finally obtaining the inclusions in the high-temperature alloy through drying, thereby realizing efficient collection and purification of the inclusions.
7. An electrolysis device for extracting inclusions in an iron-based superalloy for a turbine blade according to claim 1, wherein the electrolysis device comprises a water bath, filter paper, an alloy workpiece, a cathode, an anode clamp, a thermometer, a beaker, a power supply and the like, wherein the water bath is used for loading electrolyte and providing a stable temperature environment, the filter paper is positioned in the electrolysis bath and is used for filtering solid impurities in the electrolyte, the alloy workpiece is used as an anode, the cathode and the anode are immersed in the electrolyte together, the anode clamp is used for fixing and connecting the anode and the power supply, the thermometer is used for monitoring the temperature of the electrolyte, the beaker is used for loading the electrolyte, and the power supply is used for providing electric energy for the electrolysis device.
8. The electrolysis apparatus of claim 7, wherein the alloy workpiece is connected to the anode end of the power supply by an anode clamp and the cathode is directly connected to the cathode end of the power supply, such that when the power supply is turned on, an electric current is passed through the alloy workpiece and the electrolyte to the cathode to effect electrolysis.
9. The electrolysis apparatus according to any one of claims 7 or 8, wherein a thermometer is used to monitor the temperature in the water bath in real time to ensure temperature control of the electrolysis process, ensuring that the electrolysis process is performed at a constant temperature, thereby improving the efficiency and purity of the extraction of inclusions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410043688.5A CN117871202A (en) | 2024-01-11 | 2024-01-11 | Extraction method and electrolysis device for inclusions in iron-based superalloy for turbine blades |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410043688.5A CN117871202A (en) | 2024-01-11 | 2024-01-11 | Extraction method and electrolysis device for inclusions in iron-based superalloy for turbine blades |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117871202A true CN117871202A (en) | 2024-04-12 |
Family
ID=90587947
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410043688.5A Pending CN117871202A (en) | 2024-01-11 | 2024-01-11 | Extraction method and electrolysis device for inclusions in iron-based superalloy for turbine blades |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117871202A (en) |
-
2024
- 2024-01-11 CN CN202410043688.5A patent/CN117871202A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ge et al. | Electrochemical dissolution behavior of the nickel-based cast superalloy K423A in NaNO3 solution | |
| CN106757299B (en) | A kind of the electrobrightening corrosive agent and its application method of nickel-base alloy metallographic structure | |
| CN101806684B (en) | Specimen preparation and organization exposure method of metallic phase of zinc and alloy thereof | |
| CN105738188B (en) | The separation method of non-metallic inclusion in Inconel625 series of high temperature alloys | |
| CN103323310B (en) | Large gauge titanium or titanium alloy metallographic specimen preparation method | |
| CN105098280B (en) | A kind of method that collector is reclaimed from waste and old lithium ion battery | |
| CN101481824A (en) | Method for cleaning polycrystal carbon head material | |
| CN102443841B (en) | Metallographic structure electrolytic solution, corrosion method of molybdenum and metallographic structure display method thereof | |
| CN102286768A (en) | Process method for preparing superhydrophobic magnesium alloy surfaces | |
| CN110157916A (en) | A kind of method using neodymium iron boron oil base slice greasy filth preparation high-performance anisotropy NdFeB magnetic powder of low cost | |
| CN107746953A (en) | The method that high purity copper and nickel nitrate are prepared with electroplating sludge | |
| CN111238916B (en) | Classified extraction and quantitative analysis method for nonmetallic inclusions in high-temperature alloy | |
| CN201038237Y (en) | Selective volatilization recovery system for waste zinc-manganese battery | |
| CN104047022A (en) | Electrolyzing and recovering method for copper in waste diamond cutter | |
| CN106053175B (en) | The simple and easy method of carbide in a kind of extractor tool steel | |
| CN106025421B (en) | A kind of plating stripping recovery method of electrode of lithium cell | |
| CN117871202A (en) | Extraction method and electrolysis device for inclusions in iron-based superalloy for turbine blades | |
| CN108871924A (en) | A method of extracting carbide from rich chromium cast iron | |
| CN113640090B (en) | GH4141 high-temperature alloy metallographic structure corrosive and corrosion method | |
| CN107541728A (en) | A kind of preparation method for being used to prepare corrosive agent of carbide and preparation method thereof, carbide in steel alloy | |
| CN111238915A (en) | Method for extracting non-metallic inclusions in high-temperature alloy | |
| CN113337875B (en) | Iron-based deformation high-temperature alloy forging low-power flow line corrosion liquid and corrosion method thereof | |
| CA2384465C (en) | Selective removal of brazing compound from joined assemblies | |
| CN110528010B (en) | Method for cleaning fracture of nickel-based high-temperature alloy | |
| CN108193213A (en) | It is a kind of using anodic oxidation waste sulfate suitable for the electrochemical deoiling liquid of aluminium alloy and its application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |