Secondary pollution control method for high-temperature alloy powder

Abstract

The invention discloses a method for controlling secondary pollution of high-temperature alloy powder, which relates to the field of powder metallurgy and comprises the following steps: cleaning a container / transfer vessel of the high-temperature alloy powder; adhering the inner surface of the high-temperature alloy powder containing / transferring vessel for at least one time through the conductive adhesive to obtain a conductive adhesive sample; observing the conductive adhesive sample through a microscope, and judging whether the conductive adhesive sample adheres to inclusions or not; if yes, turning to the step S1; if not, it is judged that the containing / transferring vessel of the high-temperature alloy powder meets the cleanliness requirement; the high-temperature alloy powder is contained and / or transferred through the containing / transferring vessel meeting the cleanliness requirement, so that it can be ensured that all vessels for containing and / or transferring the high-temperature alloy powder do not contain inclusions, and it is effectively avoided that new pollutants are introduced into the contained and / or transferred high-temperature alloy powder; and secondary pollution to the high-temperature alloy powder is caused, so that the performance of the alloy can be ensured.

Description

Technical Field

[0001] The present invention relates to the field of powder metallurgy, and in particular to a method for controlling secondary pollution of high-temperature alloy powder. Background Art

[0002] In the field of powder metallurgy, after high-purity powder is prepared by argon atomization and plasma electrode rotation, the powder needs to be pre-treated and then hot-pressed to prepare high-temperature alloy parts.

[0003] The inventors of the present application have found through research that there is a risk of secondary contamination during powder pretreatment and powder transportation, which causes the performance of the alloy to deteriorate. Summary of the invention

[0004] The technical problem to be solved by the present invention is that in the prior art, there is a risk of secondary contamination of powder during pretreatment and powder transportation, resulting in a decrease in the performance of the alloy.

[0005] In order to solve the above problems, an embodiment of the present invention provides a method for controlling secondary pollution of high-temperature alloy powder, comprising:

[0006] S1, cleaning the container / transfer vessel for high temperature alloy powder;

[0007] S2, using a conductive adhesive to adhere the inner surface of the container / transfer container of the high-temperature alloy powder at least once to obtain a conductive adhesive sample;

[0008] S3, observing the conductive adhesive sample through a microscope to determine whether the conductive adhesive sample has adhered to inclusions;

[0009] S4, if the conductive adhesive sample is adhered to inclusions, go to step S1;

[0010] S5, if the conductive adhesive sample does not pick up inclusions, it is determined that the container / transfer vessel for the high-temperature alloy powder meets the cleanliness requirement;

[0011] S6, containing and / or transferring the high temperature alloy powder by using a containing / transfer vessel that meets the cleanliness requirement.

[0012] A further technical solution is that the cleaning process of the container / transfer vessel for the high temperature alloy powder comprises:

[0013] S11, ultrasonically cleaning the container / transfer vessel for the high temperature alloy powder;

[0014] S12, cleaning the container / transfer container of the high temperature alloy powder with a dust-free cloth and drying it;

[0015] S13, rinsing the container / transfer container of the high temperature alloy powder with alcohol and drying it.

[0016] A further technical solution is that in step S11, the cleaning time of ultrasonic cleaning is 10-30 minutes.

[0017] A further technical solution is that in step S13, the container for holding / transferring the high temperature alloy powder is dried in an oven, wherein the oven is wiped in advance before the container for holding / transferring the high temperature alloy powder is placed in the oven.

[0018] A further technical solution is that the conductive adhesive is adhered to the inner surface of the container / transfer vessel at least once to obtain a conductive adhesive sample, comprising:

[0019] In a clean area, the conductive glue is fixed on a sample table in advance, and then the conductive glue is randomly adhered to the inner surface of the cleaned container / transfer vessel from bottom to top for multiple times, while keeping the conductive glue without wrinkles, to obtain the conductive glue sample.

[0020] A further technical solution is that in step S2, the number of dipping is greater than 10 times.

[0021] A further technical solution is that observing the conductive adhesive sample through a microscope includes:

[0022] Through a microscope, various positions of the conductive adhesive sample are observed in sequence according to a preset observation direction.

[0023] A further technical solution is that the method for controlling secondary pollution of high-temperature alloy powder further includes:

[0024] If inclusions are adhered to the conductive adhesive sample, the morphology and element composition of the inclusions are analyzed by scanning electron microscopy.

[0025] A further technical solution is that the method for controlling secondary pollution of high-temperature alloy powder further includes:

[0026] If inclusions are adhered to the conductive adhesive sample, the inclusions are subjected to morphological analysis and elemental composition analysis by an energy dispersive spectrometer.

[0027] A further technical solution is that the container / transfer vessel for the high-temperature alloy powder includes a screening machine component, a screen, a bellows, a powder tank, a tray, a powder tank, a tray, a cover plate and a bag.

[0028] Compared with the prior art, the technical effects achieved by the present invention include:

[0029] The embodiment of the present invention provides a method for controlling secondary pollution of high-temperature alloy powder, comprising: S1, cleaning a container for containing / transferring the high-temperature alloy powder; S2, adhering the inner surface of the container for containing / transferring the high-temperature alloy powder at least once with conductive glue to obtain a conductive glue sample; S3, observing the conductive glue sample with a microscope to determine whether the conductive glue sample has adhered to inclusions; S4, if the conductive glue sample has adhered to inclusions, going to step S1; S5, if the conductive glue sample has not adhered to inclusions, determining that the container for containing / transferring the high-temperature alloy powder meets the cleanliness requirement; S6, containing and / or transferring the high-temperature alloy powder with a container for containing / transferring that meets the cleanliness requirement, thereby ensuring that the container for containing and / or transferring the high-temperature alloy powder does not contain inclusions, effectively avoiding the introduction of new pollutants in the containing and / or transferring of the high-temperature alloy powder, causing secondary pollution to the high-temperature alloy powder, thereby ensuring the performance of the alloy. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the technical solution of the present invention, the accompanying drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings in the following description are some embodiments of the present invention. For ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without paying any creative work.

[0031] Figure 1 A schematic diagram of a process for controlling secondary pollution of high-temperature alloy powder provided by an embodiment of the present invention;

[0032] Figure 2 A schematic diagram of fixing the conductive adhesive provided by an embodiment of the present invention on a sample stage;

[0033] Figure 3 A physical picture of a conductive adhesive sample provided by an embodiment of the present invention under a microscope;

[0034] Figure 4 This is a scanning electron microscope image of inclusions in the conductive adhesive sample in Example 1 of the present invention;

[0035] Figure 5 This is an energy spectrum diagram of inclusions in the conductive adhesive sample in Example 1 of the present invention;

[0036] Figure 6 This is a scanning electron microscope image of inclusions in the conductive adhesive sample in Example 2 of the present invention;

[0037] Figure 7 This is an energy spectrum diagram of inclusions in the conductive adhesive sample in Example 2 of the present invention;

[0038] Figure 8This is a scanning electron microscope image of inclusions in the conductive adhesive sample in Example 3 of the present invention;

[0039] Fig. 9 This is an energy spectrum diagram of inclusions in the conductive adhesive sample in Example 3 of the present invention;

[0040] Fig.10 This is a scanning electron microscope image of inclusions in the conductive adhesive sample in Example 4 of the present invention;

[0041] Fig.11 This is an energy spectrum diagram of inclusions in the conductive adhesive sample in Example 4 of the present invention. DETAILED DESCRIPTION

[0042] The technical solutions in the embodiments are described clearly and completely below. Obviously, the embodiments described below are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0043] It should be understood that when used in this specification and the appended claims, the terms "include" and "comprises" indicate the presence of described features, integers, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, integers, steps, operations, elements, components and / or combinations thereof.

[0044] It should also be understood that the terms used in this specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. As used in the specification of the present invention and the appended claims, unless the context clearly indicates otherwise, the singular forms "a", "an" and "the" are intended to include plural forms.

[0045] See also Figure 1 The embodiment of the present invention provides a method for controlling secondary pollution of high temperature alloy powder, which can reduce the risk of secondary pollution of high temperature alloy powder during pretreatment and powder transportation. Specifically, Figure 1 As shown, the method includes:

[0046] S1, cleaning the container / transfer vessel for the high temperature alloy powder.

[0047] In the embodiment of the present invention, firstly, in order to avoid secondary contamination of the high temperature alloy powder during the pretreatment process, the powder pretreatment atmosphere requirements are as follows:

[0048] After the high-temperature alloy powder is prepared, it should be stored in a clean powder making tank and must not be opened in non-clean room areas.

[0049] The transfer of powder from the powder making tank to the screening tank should be carried out in a clean area. Personnel need to wear clean clothes and gloves, and then perform powder pretreatment operations. The clean powder tank is connected to the screening machine through a bellows to avoid manual operation, which is easy to introduce rubber inclusions.

[0050] Qualified powder is stored in a clean room.

[0051] In a specific implementation, in order to provide a container / transfer vessel that meets the above-mentioned pretreatment requirements, the container / transfer vessel for the high-temperature alloy powder is first cleaned.

[0052] The container / transfer vessel for the high temperature alloy powder includes a screening machine component, a screen, a bellows, a powder tank, a tray, a powder tank, a tray, a cover plate and a package, which is not specifically limited in the present invention.

[0053] For example, in one embodiment, the above step of “cleaning the container / transfer vessel for the high temperature alloy powder” specifically includes the following steps:

[0054] S11, ultrasonically cleaning the container / transfer vessel for the high temperature alloy powder.

[0055] In a specific implementation, the container / transfer vessel of the high temperature alloy powder is ultrasonically cleaned by ultrasonic cleaning equipment to remove excess powder and residual inclusions. The ultrasonic cleaning time is 10-30 minutes, for example, in this embodiment, the ultrasonic cleaning time is 10 minutes.

[0056] It can be understood that the time for ultrasonic cleaning can be determined according to the size and degree of dirtiness of the container / transfer vessel.

[0057] S12, cleaning the container / transfer container of the high temperature alloy powder with a dust-free cloth and blowing it dry.

[0058] In a specific implementation, the container / transfer vessel of the high temperature alloy powder is cleaned with a dust-free cloth and blown dry with an air gun. Using a dust-free cloth can avoid introducing new pollutants and reduce the risk of secondary contamination. The container / transfer vessel can be reliably blown dry with an air gun.

[0059] S13, rinsing the container / transfer container of the high temperature alloy powder with alcohol and drying it.

[0060] In a specific implementation, in order to remove some organic pollutants, the container / transfer vessel for the high temperature alloy powder is further rinsed with alcohol, and after the rinsing, the container / transfer vessel is dried.

[0061] Specifically, the container / transfer vessel for holding / transferring the high-temperature alloy powder is dried in an oven, wherein the oven is wiped in advance before the container / transfer vessel for holding / transferring the high-temperature alloy powder is placed in the oven, thereby effectively avoiding the introduction of other new pollutants into the oven to cause secondary pollution.

[0062] S2, using conductive adhesive to adhere the inner surface of the container / transfer container of the high-temperature alloy powder at least once to obtain a conductive adhesive sample.

[0063] In a specific implementation, the conductive adhesive can effectively pick up inclusions in the container / transfer vessel without leaving any stains. In an embodiment of the present invention, the conductive adhesive is used to pick up the inner surface of the container / transfer vessel for the high-temperature alloy powder at least once, usually multiple times and multiple positions. After the pick-up is completed, a conductive adhesive sample is obtained, and by observing whether there are inclusions on the conductive adhesive sample, it is determined whether the inner surface of the container / transfer vessel meets the cleanliness requirements.

[0064] For example, in one embodiment, the above step of "cleaning the container / transfer vessel for high-temperature alloy powder" specifically includes the following steps: in a clean area, the conductive glue is fixed on a sample table in advance, and then the conductive glue is randomly adhered to the inner surface of the cleaned container / transfer vessel from bottom to top for multiple times, while keeping the conductive glue without wrinkles, to obtain the conductive glue sample.

[0065] In the specific implementation, the first step of dipping is performed in a clean area to avoid secondary contamination from the environment. The conductive glue is fixed on the sample stage in advance. Figure 2 As shown, for example, it is fixed by pasting. Then, the conductive adhesive is randomly adhered to the inner surface of the cleaned container / transfer vessel from bottom to top for multiple times to ensure that each area of ​​the inner surface of the container / transfer vessel is adhered. The number of times of adhesion is greater than 10 times, which can be determined according to the size of the container / transfer vessel. At the same time, during the adhesion, the conductive adhesive needs to be kept from wrinkling to avoid inclusions being hidden by wrinkles. After the adhesion is completed, the conductive adhesive sample is obtained. If the conductive adhesive is wrinkled during the adhesion, the conductive adhesive is taken again and step S2 is repeated.

[0066] S3, observing the conductive adhesive sample through a microscope to determine whether the conductive adhesive sample has adhered to inclusions.

[0067] In a specific implementation, various parts of the conductive adhesive sample are observed through a microscope to determine whether the conductive adhesive sample has adhered to inclusions.

[0068] For example, in one embodiment, each position of the conductive adhesive sample is observed in sequence according to a preset observation direction (for example, the observation direction is from left to right, from top to bottom) through a microscope.

[0069] For example, in one embodiment of the present invention, the conductive adhesive sample under a microscope is shown in the following figure: Figure 3 shown.

[0070] S4, if the conductive adhesive sample is adhered to inclusions, go to step S1.

[0071] In a specific implementation, if the conductive adhesive sample picks up inclusions, go to step S1, i.e., re-clean the container / transfer vessel for the high-temperature alloy powder, and perform subsequent steps in sequence until the conductive adhesive sample does not pick up inclusions and the container / transfer vessel for the high-temperature alloy powder meets the cleanliness requirements.

[0072] Furthermore, in some embodiments, if the conductive adhesive sample picks up inclusions, the inclusions are subjected to morphological analysis and elemental composition analysis by scanning electron microscopy, so as to determine the morphology and composition of the inclusions, and further determine their sources, providing a reference for subsequent reduction of secondary pollution.

[0073] Furthermore, if the conductive adhesive sample is adhered to inclusions, the inclusions are subjected to morphological analysis and elemental composition analysis by an energy spectrometer, so that the morphology and composition of the inclusions can be determined, and their sources can be further determined, providing a reference for subsequent reduction of secondary pollution.

[0074] For example, in Example 1 of the present invention, the SEM image of the inclusions in the conductive adhesive sample is as follows: Figure 4 As shown, the energy spectrum is Figure 5 As shown in the figure, the inclusions on the powder container are stainless steel materials of Fe / Cr / C.

[0075] In Example 2 of the present invention, the SEM image of inclusions in the conductive adhesive sample is as follows: Figure 6 As shown, the energy spectrum is Figure 7 shown.

[0076] In Example 3 of the present invention, the SEM image of the inclusions in the conductive adhesive sample is as follows: Figure 8 As shown, the energy spectrum is Fig. 9 shown.

[0077] In Example 4 of the present invention, the SEM image of the inclusions in the conductive adhesive sample is as follows: Fig.10 As shown, the energy spectrum is Fig.11 shown.

[0078] The morphology and composition of inclusions can be determined through the above-mentioned scanning electron microscope analysis and energy spectrum analysis.

[0079] S5, if the conductive adhesive sample does not pick up inclusions, it is determined that the container / transfer vessel for the high-temperature alloy powder meets the cleanliness requirement.

[0080] In a specific implementation, if the conductive adhesive sample does not pick up inclusions, it is determined that the container for holding / transferring the high-temperature alloy powder meets the cleanliness requirement. The cleaned container / transferring container can be used to hold and / or transfer the high-temperature alloy powder.

[0081] S6, containing and / or transferring the high temperature alloy powder by using a containing / transfer vessel that meets the cleanliness requirement.

[0082] In a specific implementation, the high temperature alloy powder is contained and / or transferred by using a containing / transferring vessel that meets the cleanliness requirements, thereby effectively preventing the high temperature alloy powder from being secondary contaminated during the containing and / or transferring process.

[0083] The embodiment of the present invention provides a method for controlling secondary pollution of high-temperature alloy powder, comprising: S1, cleaning a container for containing / transferring the high-temperature alloy powder; S2, adhering the inner surface of the container for containing / transferring the high-temperature alloy powder at least once with conductive glue to obtain a conductive glue sample; S3, observing the conductive glue sample with a microscope to determine whether the conductive glue sample has adhered to inclusions; S4, if the conductive glue sample has adhered to inclusions, going to step S1; S5, if the conductive glue sample has not adhered to inclusions, determining that the container for containing / transferring the high-temperature alloy powder meets the cleanliness requirement; S6, containing and / or transferring the high-temperature alloy powder with a container for containing / transferring that meets the cleanliness requirement, thereby ensuring that the container for containing and / or transferring the high-temperature alloy powder does not contain inclusions, effectively avoiding the introduction of new pollutants in the containing and / or transferring of the high-temperature alloy powder, causing secondary pollution to the high-temperature alloy powder, thereby ensuring the performance of the alloy.

[0084] It can be understood that the vessel cleanliness detection method proposed in the present invention can also be applied to the cleanliness detection of vessels in other fields.

[0085] In the above embodiments, the description of each embodiment has its own emphasis. For parts that are not described in detail in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.

[0086] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms should not be understood as necessarily referring to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification.

[0087] Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.

[0088] The above is a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can easily think of various equivalent modifications or replacements within the technical scope disclosed by the present invention, and these modifications or replacements should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention shall be based on the protection scope of the claims.

Claims

1. A method for controlling secondary pollution of high-temperature alloy powder, characterized in that: include: S1, cleaning the container / transfer vessel for high temperature alloy powder; S2, using a conductive adhesive to adhere the inner surface of the container / transfer container of the high-temperature alloy powder at least once to obtain a conductive adhesive sample; S3, observing the conductive adhesive sample through a microscope to determine whether the conductive adhesive sample has adhered to inclusions; S4, if the conductive adhesive sample is adhered to inclusions, go to step S1; S5, if the conductive adhesive sample does not pick up inclusions, it is determined that the container / transfer vessel for the high-temperature alloy powder meets the cleanliness requirement; S6, containing and / or transferring the high temperature alloy powder by using a containing / transfer vessel that meets the cleanliness requirement.

2. The method for controlling secondary pollution of high-temperature alloy powder according to claim 1, characterized in that: The cleaning process of the container / transfer vessel for the high temperature alloy powder comprises: S11, ultrasonically cleaning the container / transfer vessel for the high temperature alloy powder; S12, cleaning the container / transfer container of the high temperature alloy powder with a dust-free cloth and drying it; S13, rinsing the container / transfer container of the high temperature alloy powder with alcohol and drying it.

3. The method for controlling secondary pollution of high temperature alloy powder according to claim 2, characterized in that: In step S11, the cleaning time of ultrasonic cleaning is 10-30 minutes.

4. The method for controlling secondary pollution of high-temperature alloy powder according to claim 2, characterized in that: In step S13, the container for holding / transferring the high temperature alloy powder is dried in an oven, wherein the oven is wiped in advance before the container for holding / transferring the high temperature alloy powder is placed in the oven.

5. The method for controlling secondary pollution of high temperature alloy powder according to claim 1, characterized in that: The step of sticking the conductive adhesive to the inner surface of the container / transfer vessel at least once to obtain a conductive adhesive sample comprises: In a clean area, the conductive glue is fixed on a sample table in advance, and then the conductive glue is randomly adhered to the inner surface of the cleaned container / transfer vessel from bottom to top for multiple times, while keeping the conductive glue without wrinkles, to obtain the conductive glue sample.

6. The method for controlling secondary pollution of high temperature alloy powder according to claim 5, characterized in that: In step S2, the number of dipping is greater than 10 times.

7. The method for controlling secondary pollution of high temperature alloy powder according to claim 1, characterized in that: The step of observing the conductive adhesive sample through a microscope includes: Through a microscope, various positions of the conductive adhesive sample are observed in sequence according to a preset observation direction.

8. The method for controlling secondary pollution of high temperature alloy powder according to claim 1, characterized in that: Also includes: If inclusions are adhered to the conductive adhesive sample, the morphology and element composition of the inclusions are analyzed by scanning electron microscopy.

9. The method for controlling secondary pollution of high temperature alloy powder according to claim 1, characterized in that: Also includes: If inclusions are adhered to the conductive adhesive sample, the inclusions are subjected to morphological analysis and elemental composition analysis by an energy dispersive spectrometer.

10. The method for controlling secondary pollution of high temperature alloy powder according to claim 1, characterized in that: The container / transfer vessel for containing / transferring the high-temperature alloy powder comprises a screening machine component, a screen, a bellows, a powder tank, a tray, a powder tank, a tray, a cover plate and a bag cover.

Images