CN107607567B - Quantitative characterization method for nonmetallic inclusions in nickel-based superalloy powder - Google Patents
Quantitative characterization method for nonmetallic inclusions in nickel-based superalloy powder Download PDFInfo
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Abstract
The invention belongs to the technical field of metal physical chemistry, and discloses a quantitative characterization method for nonmetallic inclusions in nickel-based superalloy powder. Taking nickel-based superalloy powder, and adopting an electron beam remelting method to prepare a metal ingot with nonmetallic inclusions gathered on the upper surface. Then cutting off the part containing the non-metallic inclusions, and carrying out acid dissolution treatment. Different elements and compounds are dissolved by acid step by step, the leaching separation is carried out, finally, the non-metallic inclusions in the powder are leached and filtered on the mixed cellulose microporous filter membrane, and the scanning electron microscope is adopted to carry out morphology observation, ingredient confirmation and inclusion quantity statistics on the non-metallic inclusions on the mixed cellulose microporous filter membrane, so that the quantitative extraction of the non-metallic inclusions in the high-temperature alloy powder is realized. The method has the advantages of easy acquisition of used equipment, simple operation, short time consumption, high extraction rate and unconstrained separation size.
Description
Technical Field
The invention belongs to the technical field of metal physical chemistry, and particularly relates to a quantitative characterization method for nonmetallic inclusions in nickel-based superalloy powder.
Background
The nickel-based high-temperature alloy powder refers to a series of high-temperature alloy powder prepared by adopting an argon or nitrogen atomization method, and is mainly applied to key parts of aerospace engines. The material has extremely high performance requirements, even trace non-metallic inclusions can seriously affect various physical and chemical properties of the finally prepared alloy part, and the strict control of the content of the non-metallic inclusions in the alloy powder is an important condition for obtaining high-performance aviation parts. Therefore, in order to accurately analyze the nonmetallic inclusions in the nickel-base superalloy powder, the inclusions need to be extracted, and then the morphology, size distribution and quantity of the inclusions are observed through a scanning electron microscope, and the energy spectrum analysis is carried out on the components of the inclusions.
Nonmetallic inclusions in the argon or nitrogen atomized high-temperature alloy powder mainly come from falling off of refractory materials of a crucible, a leakage ladle and a nozzle of a master alloy smelting and powder making device, and the main inclusions are SiO 2 、Al 2 O 3 And the like. However, the existing equipment conditions and powder-making technology can not completely eliminate the impurities.
At present, the method for separating or extracting nonmetallic inclusion in the high-temperature alloy mainly comprises a water elutriation method, an electrolysis method, an electrostatic separation method and the like. The water elutriation method is used for separating the nonmetallic inclusions in the high-temperature alloy powder, the theoretical particle size and the critical water flow speed of the graded elutriation need to be calculated, and because the shapes of the nonmetallic inclusions are irregular, the water flow speed is non-uniform, and the particles are subjected to interference settling, the separation efficiency is reduced, the nonmetallic inclusions are easy to be incompletely separated, and the requirements on the technology and experience of operators are high; the electrolytic method is used for separating nonmetallic inclusions in the high-temperature alloy, a powder sample is required to be processed into an anode electrode, a proper electrolyte formula is selected, the potential is controlled to be stable, the temperature rise is controlled, the pH value of the electrolyte is kept to be stable, the operation is relatively complicated, the electrolytic time is long and reaches dozens of hours or even dozens of hours, only limited small electrodes can be electrolyzed, the powder taking amount for preparing the electrodes is limited, the amount of the inclusions in the powder is difficult to represent objectively, and the electrolytic method has certain limitation in both the difficulty degree and the extraction accuracy degree of experiments; the electrostatic separation method for extracting the nonmetallic inclusions in the high-temperature alloy usually needs to control proper corona electrode voltage and metal roller rotating speed, the optimal separation size of the inclusions exists, and the separation rate cannot reach 100%. Due to the limitations of the above prior art methods, and the very low content of non-metallic inclusions in the powder itself (perhaps only 20 non-metallic inclusions below 100 μm in 1kg of powder), the current methods are difficult to use as an accurate quantitative extraction of non-metallic inclusions in high purity nickel-base superalloy powders.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a quantitative characterization method for nonmetallic inclusions in nickel-based superalloy powder.
The purpose of the invention is realized by the following technical scheme:
a quantitative characterization method for nonmetallic inclusions in nickel-based superalloy powder comprises the following steps:
(1) taking nickel-based high-temperature alloy powder for ingot pressing, then adopting electron beam remelting to prepare an alloy ingot, and floating up and enriching non-molten non-metallic inclusion to the upper surface of an ingot head in the downward ingot casting process;
(2) cutting off the part containing the nonmetallic inclusion on the upper surface of the ingot head by adopting a linear cutting mode, polishing the cutting surface of the ingot head by using abrasive paper, then washing and drying the cut off part, adding the part into acid liquor for dissolving, and separating the nonmetallic inclusion enriched to the upper surface of the ingot head into the acid liquor in the process of dissolving the alloy surface to obtain colloidal suspension acid liquor;
(3) adding deionized water into the colloidal suspended acid solution obtained in the step (2) for dilution, and then performing suction filtration by adopting a mixed cellulose microporous filter membrane to attach the colloidal suspended substance to the mixed cellulose microporous filter membrane; then immersing the mixed cellulose microporous filter membrane attached with the colloidal suspended matters into deionized water, and desorbing the colloidal suspended matters into the deionized water by ultrasonic oscillation to obtain colloidal suspension;
(4) adding H into the colloidal suspension of the step (3) 2 O 2 Fully reacting with oxalic acid, diluting the reaction solution with deionized water, and performing suction filtration by using a mixed cellulose microfiltration membrane to attach undissolved residues to the mixed cellulose microfiltration membrane; then immersing the mixed cellulose microporous filter membrane attached with the residues into deionized water, and desorbing the residues into the deionized water by ultrasonic oscillation to obtain a residue mixed solution;
(5) adding HCl solution and HNO into the residue mixed solution in the step (4) 3 The solution is fully reacted, and the reaction solution is diluted by deionized water and then adopts a mixed cellulose microporous filter membraneCarrying out suction filtration to make undissolved residues attached to the mixed cellulose microporous filter membrane; then immersing the mixed cellulose microporous filter membrane attached with the residues into deionized water, and performing ultrasonic oscillation to desorb the residues into the deionized water;
(6) adding sufficient deionized water into the solution obtained in the step (5), performing suction filtration on the solution by adopting a mixed cellulose microporous filter membrane, and placing the collected filter membrane in a drying box for drying;
(7) and (5) performing gold spraying treatment on the front surface (the surface attached with the residues) of the filter membrane obtained in the step (6), fixing the edge in the orthogonal direction by using conductive adhesive, representing the morphology and components of the nonmetallic inclusion on the filter membrane by using a scanning electron microscope and an energy spectrometer, and counting the number of particles of the nonmetallic inclusion.
The amount of the nickel-based superalloy powder in the step (1) can be freely and properly selected according to the amount of the powder to be analyzed, and the non-metallic inclusions possibly existing in the powder can be quantitatively analyzed more accurately.
The abrasive paper polishing in the step (2) is to polish with No. 1200 abrasive paper; the cleaning is ultrasonic cleaning in acetone solution and ethanol in sequence, and then washing with deionized water.
Preferably, the acid solution in step (2) refers to concentrated HCl and concentrated HNO 3 Wherein the mass fraction of the concentrated HCl is 36-38%, and the concentrated HNO is 3 The mass fraction of (A) is 65-68%; concentrated HCl and concentrated HNO 3 Is preferably 6: 1.
Preferably, the pore size of the mixed cellulose microfiltration membrane described in steps (3) to (6) is 0.22 μm, 0.45 μm or 0.8. mu.m.
Preferably, the ultrasonic oscillation in steps (3) to (5) has a frequency of 40kHz and a power of 100W.
Preferably, the HCl solution in the step (5) is 20% by mass of HCl solution, and the HNO 3 The solution is HNO with the mass fraction of 65-68% 3 And (3) solution.
The principle of the invention is as follows: in the production process of the nickel-based high-temperature alloy powder, the crucible and the leakage of the master alloy smelting and powder making deviceThe refractory material of the ladle and the nozzle falls off, even deoxidation products in the smelting process, solid particles in the atomizing medium argon gas and process environment pollution are likely to introduce non-metallic inclusions, such as SiO 2 、Al 2 O 3 And the like. The chemical components of the nickel-based superalloy mainly comprise nickel, chromium, cobalt, tungsten, molybdenum, niobium, titanium, aluminum and other elements, the chemical properties of the alloy elements are utilized, and proper reagents are selected to promote the alloy elements to enter a solution in the form of ions, and SiO which is relatively stable to the chemical properties 2 、Al 2 O 3 And separating the non-metallic inclusions to finally achieve the purpose of extracting the non-metallic inclusions. By controlling the acid solution ratio (concentrated HCl and concentrated HNO) 3 The volume ratio of the solution is about 6:1), H is added in sequence 2 O 2 And oxalic acid, HCl solution and HNO 3 The solution is used for dissolving insoluble matters (such as W, Mo, Nb, Ti and corresponding oxides) and is filtered by using a mixed cellulose microporous filter membrane, so that the number, components and morphological characteristics of the nonmetallic inclusions in the nickel-based superalloy powder are quantitatively characterized.
The method of the invention has the following advantages and beneficial effects:
(1) the invention can analyze alloy powder with any amount, and overcomes the defect of limited sample size by an electrolysis method.
(2) Compared with microporous filter membranes made of other materials, the mixed cellulose microporous filter membrane adopted by the invention has better hydrophilicity, is mainly used for filtering water system solution, and has the advantages of easily obtained materials and low cost. The microporous membrane has the characteristics of uniform microporous structure, high porosity, no medium falling, high filtering speed, small adsorption, dilute acid resistance and the like. In the ultrasonic oscillation process, attachments on the surface of the filter membrane are easy to separate, the filter membrane is not damaged, and the extraction rate of the nonmetallic inclusion is greatly improved.
(3) The invention adopts the combination of the electron beam remelting and the acid dissolution method to extract the non-metallic inclusions in the nickel-based superalloy powder, and compared with the water elutriation method, the extraction rate is higher, and the non-metallic inclusions in the powder can be more accurately quantified.
(4) Compared with an electrolytic method, the method has the characteristics of simple operation, shorter time consumption and higher extraction rate, and can solve the limitation of extraction by the electrolytic method when the inclusion content is very low.
(5) Compared with the electrostatic separation method, the method has higher extraction rate and is not restricted by the optimal size of the nonmetallic inclusion.
(6) Compared with the observation of nonmetallic inclusions in the workpiece, the invention overcomes the defect of incomplete observation of the workpiece.
(7) The powder is used as a research object, the powder is simply pressed into blocks to be subjected to electron beam remelting, special processing and heat treatment are not needed, and the operation process is simple in equipment and easy to obtain.
Drawings
FIG. 1 is an alloy ingot with a top surface enriched with nonmetallic inclusions according to an embodiment of the present invention;
FIG. 2 is an alloy ingot of an embodiment of the present invention, which is cut and cleaned and has inclusions on the upper surface;
FIG. 3 shows the dissolution separation of the non-metallic inclusion containing fraction and the alloy fraction during the acid dissolution in the example of the present invention;
FIG. 4 is a schematic diagram of a suction filtration process in an embodiment of the present invention;
FIG. 5 shows a mixed cellulose microporous membrane after suction filtration according to an embodiment of the present invention;
FIG. 6 shows the non-metallic inclusions on the filter membrane observed by SEM in the example of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Examples
In this embodiment, the FGH96 nickel-based superalloy powder with a particle size of 105 μm or less is taken as an example, and the main elements of the alloy are: the method comprises the following steps of carrying out quantitative extraction and characterization on the nonmetallic inclusion in Cr, Co, W, Mo, Ti, Al, Nb and Ni, and specifically comprising the following steps:
(1) taking 270g of FGH96 nickel-based high-temperature alloy powder, pressing the powder into ingots, then adopting electron beam remelting to prepare alloy powder ingots, and floating up and enriching non-metallic inclusions to the upper surface of ingot heads, as shown in figure 1;
(2) cutting off the inclusion-containing part on the upper surface of the ingot by adopting a linear cutting mode, polishing the cut surface to 1200 # abrasive paper by using abrasive paper, then carrying out ultrasonic cleaning on the cut part in an acetone solution for 10min, carrying out ultrasonic cleaning by using alcohol for 10min, washing with deionized water for three times, and drying for later use, wherein the figure is 2;
(3) 70mL of acid solution is prepared, and the acid solution is concentrated HCl and concentrated HNO 3 The volume ratio of the mixed solution is 6:1, wherein the mass fraction of the concentrated HCl solution is 36-38%, and the concentrated HNO solution is concentrated 3 The mass fraction of the solution is about 65-68%;
(4) placing the sample treated in the step (2) into the acid solution in the step (3) at room temperature for chemical reaction, dissolving and separating the inclusion-containing part and the alloy part after about 20min, taking out the undissolved alloy block after separation, and washing the taken-out alloy block for 3 times in the direction of a beaker by using deionized water, wherein the undissolved alloy block is shown in figure 3;
(5) adding 2L of deionized water into the colloidal suspension obtained in the step (4) for dilution; then, carrying out suction filtration on the obtained diluent by adopting a mixed cellulose microporous filter membrane to ensure that colloidal suspended matters are attached to the mixed cellulose microporous filter membrane, wherein the aperture of the mixed cellulose microporous filter membrane is 0.8 mu m;
(6) placing the mixed cellulose microporous filter membrane attached with the colloidal suspended matters in the step (5) in a beaker filled with 20mL of deionized water, carrying out ultrasonic oscillation for 10min to obtain colloidal suspension, gently taking out the filter membrane from the beaker by using a pair of tweezers, and washing the filter membrane for 3 times in the direction of the beaker by using the deionized water, wherein the ultrasonic frequency is 40kHz and the power is 100W;
(7) to the colloidal suspension obtained in step (6), 300mL of 30 wt.% H was added 2 O 2 Adding 20g of oxalic acid crystals into the solution, fully stirring until the oxalic acid crystals are completely dissolved, turning the solution to yellow, clarifying the suspension, keeping the process for about 30min, and finally adding 500Ml of deionized water for dilution;
(8) performing suction filtration on the solution obtained in the step (7) by adopting a mixed cellulose microporous filter membrane, placing the collected filter membrane in a beaker filled with 20mL of deionized water, performing ultrasonic oscillation for 10min to obtain a residue mixed solution, gently taking the filter membrane out of the beaker by using tweezers, and flushing the filter membrane for 3 times in the direction of the beaker by using the deionized water;
(9) adding 100mL of 20 wt.% HCl solution to the residue mixture of step (8), stirring well, and adding 30mL of 65 wt.% HNO 3 Fully stirring the solution until residues are dissolved, and adding 500mL of deionized water for dilution, wherein the clarity of the solution is higher; then, carrying out suction filtration on the obtained clarified liquid by adopting a mixed cellulose microporous filter membrane, placing the collected filter membrane in a beaker filled with 20mL of deionized water, carrying out ultrasonic oscillation for 10min, gently taking out the filter membrane from the beaker by using tweezers, and washing the filter membrane for 3 times in the direction of the beaker by using the deionized water;
(10) adding 500mL of deionized water into the solution obtained in the step (9), performing suction filtration on the solution by adopting a mixed cellulose microporous filter membrane, wherein the suction filtration process is shown in figure 4, the filter membrane is shown in figure 5, and drying the collected filter membrane in a drying oven;
(11) and (3) carrying out gold spraying treatment on the front surface of the filter membrane obtained in the step (10), fixing the edges in the orthogonal direction by using conductive adhesive, representing the appearance and components of the nonmetallic inclusion on the filter membrane by using a scanning electron microscope and an energy spectrometer, and counting the number of particles of the nonmetallic inclusion, wherein the results are shown in a figure 6 and a table 1.
TABLE 1
| Element(s) | Mass fraction/% | Atomic percent/%) |
| O | 59.26 | 71.86 |
| Si | 40.74 | 28.14 |
| Total of | 100.00 | 100.00 |
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (5)
1. A quantitative characterization method for nonmetallic inclusions in nickel-based superalloy powder is characterized by comprising the following steps:
(1) taking nickel-based high-temperature alloy powder for ingot pressing, then adopting electron beam remelting to prepare an alloy ingot, and floating up and enriching non-molten non-metallic inclusion to the upper surface of an ingot head in the downward ingot casting process;
(2) cutting off the part containing the nonmetallic inclusion on the upper surface of the ingot head by adopting a linear cutting mode, polishing the cutting surface of the ingot head by using abrasive paper, then washing and drying the cut off part, adding the part into acid liquor for dissolving, and separating the nonmetallic inclusion enriched to the upper surface of the ingot head into the acid liquor in the process of dissolving the alloy surface to obtain colloidal suspension acid liquor;
(3) adding deionized water into the colloidal suspended acid solution obtained in the step (2) for dilution, and then performing suction filtration by adopting a mixed cellulose microporous filter membrane to attach the colloidal suspended substance to the mixed cellulose microporous filter membrane; then immersing the mixed cellulose microporous filter membrane attached with the colloidal suspended matters into deionized water, and desorbing the colloidal suspended matters into the deionized water by ultrasonic oscillation to obtain colloidal suspension;
(4) adding into the colloidal suspension of the step (3)Addition of H 2 O 2 Fully reacting with oxalic acid, diluting the reaction solution with deionized water, and performing suction filtration by using a mixed cellulose microfiltration membrane to attach undissolved residues to the mixed cellulose microfiltration membrane; then immersing the mixed cellulose microporous filter membrane attached with the residues into deionized water, and desorbing the residues into the deionized water by ultrasonic oscillation to obtain a residue mixed solution;
(5) adding HCl solution and HNO into the residue mixed solution in the step (4) 3 Fully reacting the solution, diluting the reaction solution by deionized water, and performing suction filtration by using a mixed cellulose microporous filter membrane to attach undissolved residues to the mixed cellulose microporous filter membrane; then immersing the mixed cellulose microporous filter membrane attached with the residues into deionized water, and performing ultrasonic oscillation to desorb the residues into the deionized water;
(6) adding enough deionized water into the solution obtained in the step (5), performing suction filtration on the solution by adopting a mixed cellulose microporous filter membrane, and placing the collected filter membrane in a drying box for drying;
(7) performing gold spraying treatment on the front surface of the filter membrane obtained in the step (6), fixing the edges in the orthogonal direction by using conductive adhesive, representing the appearance and components of the nonmetallic inclusion on the filter membrane by using a scanning electron microscope and an energy spectrometer, and counting the number of particles of the nonmetallic inclusion;
the acid liquor in the step (2) refers to concentrated HCl and concentrated HNO 3 The mixed solution of (2), wherein the mass fraction of the concentrated HCl is 36-38%, and the concentrated HNO is 3 The mass fraction of (A) is 65-68%;
the concentrated HCl and the concentrated HNO in the step (2) 3 The volume ratio of (A) to (B) is 6: 1; the HCl solution in the step (5) is a 20% HCl solution in mass fraction.
2. The method of claim 1, wherein the method comprises the steps of: the abrasive paper polishing in the step (2) is to polish with No. 1200 abrasive paper; the cleaning is ultrasonic cleaning in acetone solution and ethanol in sequence, and then washing with deionized water.
3. The method of claim 1, wherein the method comprises the steps of: the aperture of the mixed cellulose microporous filter membrane in the steps (3) to (6) is 0.22 μm, 0.45 μm or 0.8 μm.
4. The method of claim 1 for quantitative characterization of non-metallic inclusions in a nickel-base superalloy powder, wherein the method comprises: in the steps (3) to (5), the frequency of the ultrasonic oscillation is 40kHz, and the power is 100W.
5. The method of claim 1 for quantitative characterization of non-metallic inclusions in a nickel-base superalloy powder, wherein the method comprises: the HNO in the step (5) 3 The solution is HNO with the mass fraction of 65-68% 3 And (3) solution.
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| 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 |
| CN109374666A (en) * | 2018-10-16 | 2019-02-22 | 中国科学院金属研究所 | It detects selective laser and melts the method for being mingled with content in ultra-fine titanium alloy powder |
| 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 |
| CN111238916B (en) * | 2020-02-12 | 2021-05-07 | 北京科技大学 | Classified extraction and quantitative analysis method for nonmetallic inclusions in high-temperature alloy |
| CN111551576B (en) * | 2020-05-09 | 2023-07-21 | 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 high-temperature alloy performance |
| CN112945824A (en) * | 2021-02-24 | 2021-06-11 | 西安欧中材料科技有限公司 | Method for detecting inclusions in fine-particle-size nickel-based superalloy powder |
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