CN112986522A - High-efficiency determination method for oxygen existence form of high-temperature alloy powder - Google Patents
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- 239000000843 powder Substances 0.000 title claims abstract description 102
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 82
- 239000001301 oxygen Substances 0.000 title claims abstract description 82
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 73
- 239000000956 alloy Substances 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 claims abstract description 14
- 238000005520 cutting process Methods 0.000 claims abstract description 7
- 230000005540 biological transmission Effects 0.000 claims abstract description 5
- 238000011065 in-situ storage Methods 0.000 claims abstract description 5
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 40
- 238000001556 precipitation Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000012360 testing method Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 13
- 238000003795 desorption Methods 0.000 claims description 10
- 238000012216 screening Methods 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 7
- 238000010926 purge Methods 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- 238000004098 selected area electron diffraction Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052759 nickel Inorganic materials 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 239000000654 additive Substances 0.000 abstract 1
- 230000000996 additive effect Effects 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 229910000601 superalloy Inorganic materials 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 238000007872 degassing Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000001627 detrimental effect Effects 0.000 description 2
- 238000004868 gas analysis Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229920011250 Polypropylene Block Copolymer Polymers 0.000 description 1
- 229910002065 alloy metal Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
- G01N33/2022—Non-metallic constituents
- G01N33/2025—Gaseous constituents
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- General Health & Medical Sciences (AREA)
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Abstract
The invention belongs to the field of powder high-temperature alloy, and relates to a high-efficiency determination method for an oxygen existence form of high-temperature alloy powder. The thickness and the composition of the oxide film on the surface of the powder are analyzed through X-ray photoelectron spectroscopy (XPS) or focused ion beam in-situ cutting combined with a transmission electron microscope (FIB-TEM), the existence form of oxygen is verified, and technical support is provided for the preparation and the application of the nickel-based high-temperature alloy powder for high-quality powder metallurgy and additive manufacturing.
Description
Technical Field
The invention belongs to the field of powder high-temperature alloy, and discloses a high-efficiency determination method for an oxygen existence form of high-temperature alloy powder.
Background
The high-temperature alloy powder is mainly applied to manufacturing of aeroengine powder metallurgy turbine disc parts and 3D printing complex structural parts at present. The alloy powder particles formed by rapidly solidifying the liquid drops with the micron-sized diameter have uniform and fine structures, and the component segregation is limited in the range of the fine dendrite size in the spherical powder particles, so that the purpose of homogenization is achieved. However, the powder has a larger specific surface area compared with the bulk alloy, so that the probability of gas adsorption and surface oxidation is increased, a certain amount of gas is left in gaps and surfaces of powder particles or a surface oxide film is formed, and defects such as original powder particle boundaries may be formed in the subsequent forming process. Oxygen in superalloy powders is generally considered to be a detrimental impurity element, and in fact exists in forms that are divided into free oxygen and combined oxygen, with the detrimental effect of combined oxygen generally being much greater than free oxygen. Currently, the common method for determining the oxygen content of superalloy powders is gas analysis, which determines what is actually the total amount of oxygen. In some cases it has been found that the total metal content is not high, but the performance is poor, possibly due to the high oxygen content in the alloy in the combined state, and currently only the total oxygen content is of concern. Alloy powders typically need to be degassed prior to use, and if the original powder has a high proportion of combined oxygen and a low content of free oxygen, the effectiveness of the degassing process is greatly compromised or even lost. Therefore, distinguishing and determining the presence of oxygen in a superalloy powder, rather than simply regarding the total oxygen content, is critical to the powder forming process and the mechanical properties of the alloy.
Disclosure of Invention
The purpose of the invention is: the method is used for solving the technical problem that the existing form of oxygen is limited when the existing form of oxygen is not distinguished in the prior art for measuring the content of high-temperature alloy metal, and the purpose of distinguishing the existing forms of free-state oxygen and combined-state oxygen is achieved.
In order to solve the technical problem, the technical scheme of the invention is as follows:
a high-efficiency determination method for the oxygen existence form of high-temperature alloy powder comprises the steps of firstly, rapidly determining the free-state oxygen content in the alloy powder by combining a protective atmosphere temperature programming desorption device and a mass spectrometer; determining whether the existence form of oxygen in the alloy powder is mainly harmful combined oxygen; and finally, analyzing the thickness and the composition of the oxide film on the surface of the powder by X-ray photoelectron spectroscopy (XPS) or focused ion beam in-situ cutting in combination with a transmission electron microscope (FIB-TEM), and analyzing and verifying the content and the structure of harmful compound oxygen.
The method for determining whether the presence of oxygen in the alloy powder is dominated by harmful combined oxygen is determined by the measured temperature and the presence of a significant oxygen-containing gas evolution peak in the gas evolution curve:
if the curve is smooth and no obvious gas precipitation peak exists, the existence of free oxygen can be judged, and the powder oxygen is mainly in a compound state.
The method comprises the following steps:
firstly, selecting high-temperature alloy powder with target components as sections with different particle sizes for later use;
secondly, selecting high-temperature alloy powder of a target granularity section, putting the high-temperature alloy powder into temperature programmed desorption equipment with a mass spectrometer, and purging a cavity by adopting high-purity inert gas to enable the alloy powder to be in a protective atmosphere;
step three, carrying out temperature programming on the high-temperature alloy powder, and heating the high-temperature alloy powder from room temperature to 1000 ℃; the room temperature is generally 20 ℃;
synchronously recording the ionic strength of ionized precipitated gas in the temperature rising process by adopting a mass spectrometer to form a gas precipitation curve at the temperature of 20-1000 ℃;
step five, reading gas precipitation amount curves at different temperatures, and judging that no free state oxygen exists if the curves are smooth and no obvious gas precipitation peak exists, wherein the powder oxygen is mainly in a chemical combination state;
and step six, measuring the thickness of the oxide film on the surface of the powder.
And step one, screening by a mechanical vibration screening machine.
The particle size range of the first step comprises 0-48 mu m, 48-106 mu m, 106-150 mu m and 150-355 mu m.
And in the second step, the inert gas is He gas.
The heating rate in the third step is 5-30 ℃/min.
And step six, specifically, measuring the thickness of the oxide film on the surface of the powder by one of the following operations:
XPS test is carried out on the high-temperature alloy powder with the same grain size section in the test, the thickness of an oxide film on the surface of the powder is measured, and the content of the combined oxygen is characterized.
And (3) carrying out in-situ cutting on the high-temperature alloy powder with the same granularity section in the test by adopting a focused ion beam, cutting a TEM film sample containing a surface oxide film, carrying out transmission electron microscope observation and selected area electron diffraction test, and measuring the thickness of the surface oxide film and the structural composition of the oxide film.
The invention has the beneficial effects that:
firstly, the method can rapidly distinguish the existence form of oxygen through the temperature and gas precipitation curve, determine whether the high-temperature alloy powder with different components and particle size ranges is mainly free-state oxygen or combined-state oxygen, and solve the defect that the prior art can only determine the total oxygen content of the high-temperature alloy powder and cannot distinguish the existence form of oxygen;
secondly, the efficiency is high, the cost is low, a gas precipitation characteristic curve of the high-temperature alloy powder in the full temperature range is obtained through one test in a mode of combining temperature programmed desorption and mass spectrum, and the existence form of oxygen is quickly judged at low cost according to the curve form;
thirdly, according to the result of the judged oxygen existence form, the effectiveness of the high-temperature alloy powder degassing process can be quickly judged in advance, and a theoretical basis is provided for whether degassing treatment is necessary or not, if the powder is mainly composed of compound oxygen, the degassing treatment is not needed;
fourthly, the defect that the total oxygen amount measured by gas analysis can not be directly hooked with the mechanical property of the alloy is made up, and theoretical basis is provided for the influence of the oxygen content on the mechanical property of the alloy, particularly the influence of the plastic index through the determination of harmful compound oxygen;
fifth, the presence of oxygen in the powder in the form of a film is common, and if the powder is determined to be mainly composed of oxygen, the thickness and structure of the oxide film on the surface of the powder can be easily verified by XPS or TEM analysis. If it is determined that free oxygen is dominant, it is also known what type of gas oxygen is present, such as oxygen, water vapor, carbon dioxide, carbon monoxide;
sixth, it can be used as a rapid determination method of the defect forming tendency of the original grain boundaries (PPBs) of the powder superalloy.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Features of various aspects of embodiments of the invention will be described in detail below. In the following detailed description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced without these specific details. The following description of the embodiments is merely intended to better understand the present invention by illustrating examples thereof. The present invention is not limited to any particular arrangement or method provided below, but rather covers all product structures, any modifications, alterations, etc. of the method covered without departing from the spirit of the invention.
In the following description, well-known structures and techniques are not shown to avoid unnecessarily obscuring the present invention.
Example 1
The technical scheme adopted by the invention comprises the following specific steps:
firstly, screening prepared nickel-based superalloy (alloy 1) powder with the components of 21Cr-9Mo-5Nb-5Fe-0.5Ti-0.5Al-0.02C (mass fraction percent) into a particle size section of 0-48 mu m by a mechanical vibration screening machine;
placing the powder into temperature programmed desorption equipment with a mass spectrometer, and purging a cavity by using high-purity inert gas He gas to enable the alloy powder to be in a protective atmosphere;
thirdly, heating the high-temperature alloy powder at a heating speed of 20 ℃/min, heating the high-temperature alloy powder from room temperature to a set programmed temperature of 1000 ℃, and carrying out stepless temperature change in the heating process;
synchronously recording the ionic strength of ionized precipitated gas in the temperature rising process by adopting a mass spectrometer to form a gas precipitation curve at the temperature of 20-1000 ℃;
step five, reading different gas precipitation curves at 20-1000 ℃, wherein the curves of oxygen and water vapor are smooth and have no obvious gas precipitation peak, and the alloy powder can be judged to be mainly based on combined oxygen;
and sixthly, carrying out XPS test on the high-temperature alloy powder with the same grain size section in the test, and measuring the thickness of an oxide film on the surface of the powder to be 8.4 nm.
Example 2
The technical scheme adopted by the invention comprises the following specific steps:
firstly, screening prepared nickel-based high-temperature alloy (alloy 2) powder with the components of 16Cr-13Co-4W-4Ti-4Mo-0.8Nb-2Al-0.03C (mass fraction percent) into a particle size section of 0-48 mu m by a mechanical vibration screening machine;
placing the powder into temperature programmed desorption equipment with a mass spectrometer, and purging a cavity by using high-purity inert gas He gas to enable the alloy powder to be in a protective atmosphere;
thirdly, heating the high-temperature alloy powder at a heating speed of 20 ℃/min, heating the high-temperature alloy powder from room temperature to a set programmed temperature of 1000 ℃, and carrying out stepless temperature change in the heating process;
synchronously recording the ionic strength of ionized precipitated gas in the temperature rising process by adopting a mass spectrometer to form a gas precipitation curve at the temperature of 20-1000 ℃;
step five, reading different gas precipitation curves at 20-1000 ℃, wherein the oxygen and steam curves have obvious gas precipitation peaks at 400 ℃, and the alloy powder can be judged to be mainly based on free oxygen;
and sixthly, carrying out XPS test on the high-temperature alloy powder with the same grain size section in the test, and measuring the thickness of an oxide film on the surface of the powder to be 5.7 nm.
Example 3
The technical scheme adopted by the invention comprises the following specific steps:
firstly, screening prepared nickel-based high-temperature alloy (alloy 2) powder with the components of 16Cr-13Co-4W-4Ti-4Mo-0.8Nb-2Al-0.03C (mass fraction percent) into a particle size section of 106-150 mu m by a mechanical vibration screening machine;
placing the powder into temperature programmed desorption equipment with a mass spectrometer, and purging a cavity by using high-purity inert gas He gas to enable the alloy powder to be in a protective atmosphere;
thirdly, heating the high-temperature alloy powder at a heating speed of 20 ℃/min, heating the high-temperature alloy powder from room temperature to a set programmed temperature of 1000 ℃, and carrying out stepless temperature change in the heating process;
synchronously recording the ionic strength of ionized precipitated gas in the temperature rising process by adopting a mass spectrometer to form a gas precipitation curve at the temperature of 20-1000 ℃;
step five, reading different gas precipitation curves at 20-1000 ℃, wherein the curves of oxygen and water vapor are smooth and have no obvious gas precipitation peak, and the alloy powder can be judged to be mainly based on combined oxygen;
and sixthly, carrying out XPS test on the high-temperature alloy powder with the same grain size section in the test, and measuring the thickness of an oxide film on the surface of the powder to be 7.8 nm.
Combining the results of the above examples, a comparison can be made to find that:
(1) under the condition of different grain sizes of the alloy 1 with the same component, the existence form of oxygen is obviously changed. In example 2, the temperature and gas evolution characteristic curve of the fine powder (0-48 microns) obtained by combining temperature programmed desorption and a mass spectrometer has obvious oxygen and water vapor evolution peaks, so that the alloy powder is mainly based on free-state oxygen. The temperature and gas precipitation characteristic curve of the coarse powder (106-150 mu m) in the embodiment 3 is smooth and has no obvious oxygen and water vapor precipitation peaks, and the main oxygen in a compound state is used. In order to further verify the accuracy of the results, the thickness of the oxide film on the surface of the fine powder (0 to 48 μm) and the coarse powder (106 to 150 μm) of alloy 1 measured by XPS was 5.7nm and 7.8nm, respectively, and the oxide film on the surface of the powder in the grain size range of the coarse powder (106 to 150 μm) mainly containing compound oxygen was thicker and was consistent with the results of the measurements.
(2) The existence forms of oxygen of two alloy powders with different components in the same granularity section (0-48 mu m) are also obviously different. In example 2, the alloy powder 2 has obvious oxygen and water vapor precipitation peaks in a temperature and gas precipitation characteristic curve obtained by combining temperature programmed desorption and a mass spectrometer, so that the alloy powder is mainly based on free-state oxygen; the temperature and gas evolution characteristic curve of the alloy 1 powder of example 1 was smooth and free of significant oxygen and water vapor evolution peaks, mainly composed of combined oxygen. In order to further verify the accuracy of the result, the thickness of the oxide film on the surface of the alloy 1 and the alloy 2 with the same particle size range (0-48 μm) and different components is respectively 8.4nm and 5.7nm by XPS measurement, and the oxide film on the surface of the alloy 1 powder mainly containing the compound oxygen is thicker and is consistent with the measurement result.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive various equivalent modifications or substitutions within the technical scope of the present invention, and these modifications or substitutions should be covered within the scope of the present invention.
Claims (9)
1. A high-efficiency determination method for the oxygen existence form of high-temperature alloy powder is characterized by comprising the following steps: firstly, measuring the free state oxygen content in alloy powder by combining a protective atmosphere temperature programming desorption device and a mass spectrometer; determining whether the existence form of oxygen in the alloy powder is mainly harmful combined oxygen; and finally, analyzing the thickness and the composition of the oxide film on the surface of the powder by X-ray photoelectron spectroscopy (XPS) or focused ion beam in-situ cutting in combination with a transmission electron microscope (FIB-TEM), and analyzing and verifying the content and the structure of harmful compound oxygen.
2. The method of claim 1, wherein: the method for determining whether the presence of oxygen in the alloy powder is dominated by harmful combined oxygen is determined by the measured temperature and the presence of a significant oxygen-containing gas evolution peak in the gas evolution curve:
if the curve is smooth and no obvious gas precipitation peak exists, the existence of free oxygen can be judged, and the powder oxygen is mainly in a compound state.
3. The method of claim 2, wherein: the method comprises the following steps:
firstly, selecting high-temperature alloy powder with target components as sections with different particle sizes for later use;
secondly, selecting high-temperature alloy powder of a target granularity section, putting the high-temperature alloy powder into temperature programmed desorption equipment with a mass spectrometer, and purging a cavity by adopting high-purity inert gas to enable the alloy powder to be in a protective atmosphere;
step three, carrying out temperature programming on the high-temperature alloy powder, and heating the high-temperature alloy powder from room temperature to 1000 ℃;
step four, synchronously recording the ionic strength of ionized precipitated gas in the temperature rising process by adopting a mass spectrometer, and forming a gas precipitation quantity curve in the temperature range of the step three;
step five, reading gas precipitation amount curves at different temperatures, and judging that no free state oxygen exists if the curves are smooth and no obvious gas precipitation peak exists, wherein the powder oxygen is mainly in a chemical combination state;
and step six, measuring the thickness of the oxide film on the surface of the powder.
4. The method of claim 3, wherein: and step one, screening by a mechanical vibration screening machine.
5. The method of claim 3, wherein: the particle size range of the first step comprises 0-48 μm, 48-106 μm, 106-150 μm and 150-355 μm.
6. The method of claim 3, wherein: and the high-purity inert gas in the second step is He gas.
7. The method of claim 3, wherein: the heating rate in the third step is 5-30 ℃/min.
8. The method of claim 3, wherein: the operation of measuring the thickness of the oxide film on the surface of the powder in the sixth step is as follows:
XPS test is carried out on the high-temperature alloy powder with the same grain size section in the test, the thickness of an oxide film on the surface of the powder is measured, and the content of the combined oxygen is characterized.
9. The method of claim 3, wherein: the operation of measuring the thickness of the oxide film on the surface of the powder in the sixth step is as follows:
and (3) carrying out in-situ cutting on the high-temperature alloy powder with the same granularity section in the test by adopting a focused ion beam, cutting a TEM film sample containing a surface oxide film, carrying out transmission electron microscope observation and selected area electron diffraction test, and measuring the thickness of the surface oxide film and the structural composition of the oxide film.
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Cited By (1)
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| CN113985000A (en) * | 2021-10-15 | 2022-01-28 | 中国航发北京航空材料研究院 | Method for measuring content of oxygen and nitrogen elements in high-temperature alloy powder for additive manufacturing |
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