CN112945824A - Method for detecting inclusions in fine-particle-size nickel-based superalloy powder - Google Patents
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- 239000000843 powder Substances 0.000 title claims abstract description 123
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 52
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 45
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 40
- 238000001514 detection method Methods 0.000 claims abstract description 27
- 239000012046 mixed solvent Substances 0.000 claims description 59
- 239000012535 impurity Substances 0.000 claims description 40
- 239000002904 solvent Substances 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 11
- YMWUJEATGCHHMB-UHFFFAOYSA-N methylene chloride Substances ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000002344 surface layer Substances 0.000 claims description 9
- 239000010419 fine particle Substances 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 239000010410 layer Substances 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 6
- 238000003723 Smelting Methods 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000002184 metal Substances 0.000 abstract description 29
- 229910052751 metal Inorganic materials 0.000 abstract description 29
- 238000012216 screening Methods 0.000 description 15
- 229910000816 inconels 718 Inorganic materials 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000007769 metal material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N2015/0019—Means for transferring or separating particles prior to analysis, e.g. hoppers or particle conveyors
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
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Abstract
The invention belongs to the technical field of metal powder performance detection, and discloses a method for detecting inclusions in fine-grained nickel-based superalloy powder.
Description
Technical Field
The invention belongs to the technical field of metal powder performance detection, and particularly relates to a method for detecting inclusions in fine-particle-size nickel-based superalloy powder.
Background
With the continuous development of manufacturing industry and the improvement of the performance requirements of various industries on metal materials, the traditional metal manufacturing and processing mode cannot meet the requirement of obtaining metal materials with higher performance, so in order to obtain metal materials with better performance, an advanced powder metallurgy method is widely developed and used, has the advantages of higher material utilization rate, isotropy, capability of processing special materials, lower cost and the like, and becomes a preferred processing mode for producing metal materials in high-end fields at present. However, this method requires production of a large amount of high-quality powder before use, and during the production process of the powder, it is very easy to remove clean inclusions, mainly including ceramics, polymer materials, and dissimilar metals. Inclusions of different types and sizes can form a combined weak area or a different interface with a matrix, so that the structure and the mechanical property of the material are influenced, and particularly the fatigue is easy to occur and the durability is obviously reduced. Therefore, controlling and efficiently assessing the inclusion content during powder production is critical to obtaining high quality metal powder.
At present, the method for evaluating the inclusion content of the metal powder is mainly an artificial screening method, namely a visual method. The method can find out and count most of inclusions in the sample, but the method consumes large manpower and material resources and has insufficient comprehensiveness.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a method for detecting inclusions in fine-particle-size nickel-based superalloy powder, which overcomes the defects in the prior art.
In order to solve the technical problem, the technical scheme of the invention is as follows: a method for detecting inclusions in fine-particle-size nickel-based superalloy powder specifically comprises the following steps:
step 1: a mixed solvent configured for detection, in volume percent, theThe mixed solvent comprises the following components: 50-65% of H3PO430 to 40% of CH2Cl25-10% of liquid Br2；
Step 2: measuring each solvent in the step 1 according to volume percentage, and adding CH into a beaker2Cl2Followed by slow addition of H3PO4Standing for 2-3 min, and dripping liquid Br2Obtaining a mixed solvent;
and step 3: uniformly stirring the mixed solvent obtained in the step 2 by using a stirring rod, standing for 10-15 min, wherein the density of the mixed solvent is 1.4-1.8 g/cm3；
And 4, step 4: preparing 3-5 groups of 240-1500 g of fine-particle-size nickel-based superalloy powder to be detected in the same batch, wherein each group is divided into 30-60 g samples by a balance, and the total number of the samples is 8-25;
and 5: uniformly pouring 1 part of the sample obtained in the step (4) into the mixed solvent prepared in the step (3) at a constant speed, and standing for 3-5 min after all the fine-grain-size nickel-based superalloy powder is precipitated at the bottom of the mixed solvent;
step 6: counting the non-settled particles floating on the surface layer of the mixed solvent to obtain the number of the impurities in the sample;
and 7: respectively filtering impurities on the upper layer and the nickel-based superalloy powder with the bottom fine particle size by using filter paper, and simultaneously recovering a mixed solvent for subsequent detection;
and 8, repeating the steps 5-7 until the counting of the number of the inclusions of all samples in all the groups is completed, obtaining the content of the inclusions in the batch of the fine-grain-size nickel-based superalloy powder to be detected, and performing reverse thrust and improvement on the technological process by identifying the types and sizes of the inclusions.
Preferably, in said step 1, H3PO4The concentration of (A) is 80-95%.
Preferably, in the step 4, the granularity of the nickel-based superalloy powder with the fine particle size to be detected is 0-60 mu m, and the density is 7.5-9.0 g/cm3。
Preferably, in the step 8, the sum of the number of all the part inclusions in each group is used as the content of the group of the fine-particle-size nickel-based superalloy powder inclusions to be detected, and the obtained content of all the group of the fine-particle-size nickel-based superalloy powder inclusions to be detected is averaged to obtain the content of the inclusions in the batch of the fine-particle-size nickel-based superalloy powder to be detected.
Preferably, in the step 8, the inclusions obtained by separation are subjected to category identification through component analysis, size statistics is performed through microscopic measurement, and if the ceramic inclusions are too many, the mother alloy smelting process needs to be checked reversely; if the high molecular impurities are more, the powder preparation process needs to be checked reversely, and whether the equipment is polluted by high molecular materials or not is judged; the size of the inclusions is used to determine whether or not inclusions larger than a predetermined size are present in the powder.
Compared with the prior art, the invention has the advantages that:
(1) according to the method, the solvent with a certain density is prepared, the metal powder and the impurities are separated by utilizing the density difference of the metal powder and the impurities, the metal powder can be deposited at the bottom of the solution due to the high density of the metal powder, and the impurities can float on the surface layer of the solution due to the low density of the impurities;
(2) the solvent adopted by the invention can not react with the metal powder to be detected and impurities, so that the true performance of the metal powder can be better reduced, the detection process time is shorter, the introduction of new impurities caused by overlong detection time is avoided, and the mixed solvent can be repeatedly used by matching with filter paper, so that the detection efficiency is improved and the detection cost is reduced;
(3) the invention can identify the category of the inclusions obtained by separation through component analysis, carry out size statistics through microscopic measurement, and if the ceramic inclusions are too much, the smelting process of the master alloy needs to be checked; if the high molecular impurities are more, the powder preparation process should be checked reversely to see whether the equipment has high molecular material pollution, and the size of the impurities is used for judging whether the impurities with the size larger than the specified size exist in the powder.
Drawings
FIG. 1 is a schematic diagram showing the separation of inclusions in a fine-grained nickel-base superalloy powder according to the method of the present invention.
Description of reference numerals:
1. inclusions, 2, powder.
Detailed Description
The following describes embodiments of the present invention with reference to examples:
it should be noted that the structures, proportions, sizes, and other elements shown in the specification are included for the purpose of understanding and reading only, and are not intended to limit the scope of the invention, which is defined by the claims, and any modifications of the structures, changes in the proportions and adjustments of the sizes, without affecting the efficacy and attainment of the same.
The invention discloses a method for detecting inclusions in fine-particle-size nickel-based superalloy powder, which comprises the following steps of:
step 1: the mixed solvent for detection is prepared from the following components in percentage by volume: 50-65% of H3PO430 to 40% of CH2Cl25-10% of liquid Br2；
Step 2: measuring each solvent in the step 1 according to volume percentage, and adding CH into a beaker2Cl2Followed by slow addition of H3PO4Standing for 2-3 min, and dripping liquid Br2Obtaining a mixed solvent;
and step 3: uniformly stirring the mixed solvent obtained in the step 2 by using a stirring rod, standing for 10-15 min, wherein the density of the mixed solvent is 1.4-1.8 g/cm3；
And 4, step 4: preparing 3-5 groups of 240-1500 g of fine-particle-size nickel-based superalloy powder to be detected in the same batch, wherein each group is divided into 30-60 g samples by a balance, and the total number of the samples is 8-25;
and 5: uniformly pouring 1 part of the sample obtained in the step (4) into the mixed solvent prepared in the step (3) at a constant speed, and standing for 3-5 min after all the fine-grain-size nickel-based superalloy powder is precipitated at the bottom of the mixed solvent;
step 6: counting the non-settled particles floating on the surface layer of the mixed solvent to obtain the number of the impurities in the sample;
and 7: respectively filtering impurities on the upper layer and the nickel-based superalloy powder with the bottom fine particle size by using filter paper, and simultaneously recovering a mixed solvent for subsequent detection;
and 8, repeating the steps 5-7 until the counting of the number of the inclusions of all samples in all the groups is completed, obtaining the content of the inclusions in the batch of the fine-grain-size nickel-based superalloy powder to be detected, and performing reverse thrust and improvement on the technological process by identifying the types and sizes of the inclusions.
Preferably, in said step 1, H3PO4The concentration of (A) is 80-95%.
Preferably, in the step 4, the granularity of the nickel-based superalloy powder with the fine particle size to be detected is 0-60 mu m, and the density is 7.5-9.0 g/cm3。
Preferably, in the step 8, the sum of the number of all the part inclusions in each group is used as the content of the group of the fine-particle-size nickel-based superalloy powder inclusions to be detected, and the obtained content of all the group of the fine-particle-size nickel-based superalloy powder inclusions to be detected is averaged to obtain the content of the inclusions in the batch of the fine-particle-size nickel-based superalloy powder to be detected.
Preferably, in the step 8, the inclusions obtained by separation are subjected to category identification through component analysis, size statistics is performed through microscopic measurement, and if the ceramic inclusions are too many, the mother alloy smelting process needs to be checked reversely; if the high molecular impurities are more, the powder preparation process needs to be checked reversely, and whether the equipment is polluted by high molecular materials or not is judged; the size of the inclusions is used to determine whether or not inclusions larger than a predetermined size are present in the powder.
H according to the invention3PO4、CH2Cl2Liquid state, liquid stateBr2Are all commercial products.
Example 1
The invention discloses a method for detecting inclusions in fine-particle-size nickel-based superalloy powder, which comprises the following steps of:
step 1: the mixed solvent for detection was prepared by preparing 60mL of 85% H in volume percent3PO4Solution, 36mL of CH2Cl24mL of liquid Br2And is ready for use;
step 2: sequentially adding the solvents prepared in the step 1 into a beaker, and adding CH firstly2Cl2Then 85% strength H was added slowly3PO4Standing the solution for 2min, and dripping liquid Br2Obtaining a mixed solvent;
and step 3: uniformly stirring the mixed solvent obtained in the step 2 by using a stirring rod, standing for 10min to obtain the mixed solvent with the density of 1.63g/cm3A mixed solvent of (1);
and 4, step 4: selecting the same batch of FGH4096 powder with the particle size of 0-60 mu m as the metal powder to be detected, wherein the density is 8.34g/cm3Dividing the batch of powder into 3 groups of 500g each, and dividing each group into 50g portions by using a balance, wherein the total number of the portions is 10;
and 5: taking 1 part of the sample in the step 4, uniformly pouring the sample into the mixed solvent prepared in the step 3 at a constant speed, and standing for 5min after all the fine-grain metal powder is precipitated at the bottom of the solvent;
step 6: counting the non-settled particles floating on the surface layer of the mixed solvent to obtain the number of the impurities in the sample;
and 7: respectively filtering impurities on the upper layer and the nickel-based superalloy powder with the bottom fine particle size by using filter paper, and simultaneously recovering a mixed solvent for subsequent detection;
and 8, repeating the steps 5 to 7 until the counting of the number of the inclusions of all samples in the 3 groups is completed, taking the sum of the number of the inclusions of all samples as the content of the group of metal powder inclusions for each group of powder, taking the average value of the obtained content of the 3 groups of powder inclusions as the content of the inclusions in the batch of FGH4096 powder, and taking the implementation result as shown in Table 1:
table 1 statistical units of number of inclusions: an
In order to compare the implementation effect of the invention, the same batch of powder is selected to be subjected to manual screening of the same group as a comparison test, the manual screening result is that the impurity content in the batch of FGH4096 powder samples is 10, the total consumed working hour is 5h, the solvent detection method shown in Table 1 is used for detecting the impurity content in the batch of FGH4096 powder samples is 16, the total consumed working hour is 2.3h, and the comparison can be known by combining the properties of the separated impurities, the solvent method is used for detecting the impurities and the content in the powder, the result is more accurate and reliable than the manual screening method, and the total consumed working hour is less than half of the manual screening method.
Example 2
The invention discloses a method for detecting inclusions in fine-particle-size nickel-based superalloy powder, which comprises the following steps of:
step 1: the mixed solvent for detection was prepared by preparing 110mL of 90% H in percentage by volume3PO4Solution, 80mL of CH2Cl210mL of liquid Br2And is ready for use;
step 2: sequentially adding the solvents prepared in the step 1 into a beaker, and adding CH2Cl2Then slowly adding H with the concentration of 90%3PO4Standing the solution for 3min, and dripping liquid Br2Obtaining a mixed solvent;
and step 3: uniformly stirring the mixed solvent obtained in the step 2 by using a stirring rod, standing for 15min to obtain the mixed solvent with the density of 1.58g/cm3A mixed solvent of (1);
and 4, step 4: selecting Inconel 718 powder with the same batch of particle size of 0-60 mu m as metal powder to be detected, wherein the density of the Inconel 718 powder is 8.24g/cm3The batch was divided into 3 groups of 1000g each, each group being divided into 40g portions on a balance, the total number of portions being 25；
And 5: taking 1 part of the sample in the step 4, uniformly pouring the sample into the mixed solvent prepared in the step 3 at a constant speed, and standing for 3min after all the fine-grain metal powder is precipitated at the bottom of the mixed solvent;
step 6: counting the non-settled particles floating on the surface layer of the solvent to obtain the number of the impurities in the sample;
step 7, filtering the upper-layer inclusions and the bottom fine-particle-size nickel-based superalloy powder by using filter paper respectively, and recovering the mixed solvent for subsequent detection;
and 8, repeating the steps 5-7 until the counting of the number of the inclusions of all samples in the 3 groups is completed, taking the sum of the number of the inclusions of all samples as the content of the inclusions in the group of metal powder for each group of powder, taking the average value of the content of the obtained 3 groups of powder inclusions as the content of the inclusions in the batch of Inconel 718 powder, and taking the implementation result as shown in Table 2:
TABLE 2 statistics of the number of inclusions
Unit: an
In order to compare the implementation effect of the invention, the same batch of powder is selected to be subjected to manual screening of the same group as a comparison test, the manual screening result is that the content of inclusions in the Inconel 718 powder sample is 21, the total consumed labor hour is 13h, while the solvent detection method shown in Table 2 is used for detecting the content of inclusions in the Inconel 718 powder sample is 28, the total consumed labor hour is 4.6h, the properties of the separated inclusions are combined, the inclusions and the content in the powder are detected by adopting a solvent method, the separation of the inclusions is more accurate and comprehensive, and the total labor hour consumed by the solvent method is far lower than that consumed by the manual screening method for the case of more sample amount.
Example 3
The invention discloses a method for detecting inclusions in fine-particle-size nickel-based superalloy powder, which comprises the following steps of:
step 1: for disposition50mL of 85% H in percentage by volume in the mixed solvent to be tested was prepared3PO4Solution, 40mL of CH2Cl210mL of liquid Br2And is ready for use;
step 2: sequentially adding the solvents prepared in the step 1 into a beaker, and adding CH firstly2Cl2Then 85% strength H was added slowly3PO4Standing the solution for 2min, and dripping liquid Br2Obtaining a mixed solvent;
and step 3: uniformly stirring the mixed solvent obtained in the step 2 by using a stirring rod, standing for 10min to obtain the mixed solvent with the density of 1.75g/cm3A mixed solvent of (1);
and 4, step 4: selecting the same batch of FGH4096 powder with the particle size of 0-60 mu m as the metal powder to be detected, wherein the density is 8.34g/cm3Dividing the batch of powder into 3 groups of 500g each, and dividing each group into 50g portions by using a balance, wherein the total number of the portions is 10;
and 5: taking 1 part of the sample in the step 4, uniformly pouring the sample into the mixed solvent prepared in the step 3 at a constant speed, and standing for 5min after all the fine-grain metal powder is precipitated at the bottom of the solvent;
step 6: counting the non-settled particles floating on the surface layer of the mixed solvent to obtain the number of the impurities in the sample;
and 7: respectively filtering impurities on the upper layer and the nickel-based superalloy powder with the bottom fine particle size by using filter paper, and simultaneously recovering a mixed solvent for subsequent detection;
and 8, repeating the steps 5 to 7 until the counting of the number of the inclusions of all samples in the 3 groups is completed, taking the sum of the number of the inclusions of all samples as the content of the group of metal powder inclusions for each group of powder, taking the average value of the obtained content of the group of powder inclusions as the content of the inclusions in the batch of FGH4096 powder, and taking the implementation result as shown in Table 3:
TABLE 3 statistics of the number of inclusions
Unit: an
In order to compare the implementation effect of the invention, the same batch of powder is selected to be subjected to manual screening of the same group as a comparison test, the manual screening result is that the impurity content in the batch of FGH4096 powder samples is 10, the total consumed working hour is 5h, while the solvent detection method shown in Table 1 is used for detecting the impurity content in the batch of FGH4096 powder samples is 14, the total consumed working hour is 2.2h, the comparison can be known by combining the properties of the separated impurities, the solvent method is used for detecting the impurities and the content in the powder, the result is more accurate and reliable than the manual screening method, and the total working hour consumed by the solvent method is far lower than the manual screening method.
Example 4
The invention discloses a method for detecting inclusions in fine-particle-size nickel-based superalloy powder, which comprises the following steps of:
step 1: the mixed solvent for detection was prepared by preparing 130mL of 90% H in percentage by volume3PO4Solution, 60mL CH2Cl210mL of liquid Br2And is ready for use;
step 2: sequentially adding the solvents prepared in the step 1 into a beaker, and adding CH2Cl2Then slowly adding H with the concentration of 90%3PO4Standing the solution for 3min, and dripping liquid Br2Obtaining a mixed solvent;
and step 3: uniformly stirring the mixed solvent obtained in the step 2 by using a stirring rod, standing for 15min to obtain the mixed solvent with the density of 1.62g/cm3A mixed solvent of (1);
and 4, step 4: selecting Inconel 718 powder with the same batch of particle size of 0-60 mu m as metal powder to be detected, wherein the density of the Inconel 718 powder is 8.24g/cm3Dividing the batch of powder into 3 groups of 1000g each, and dividing each group into 40g samples with a balance, wherein the total number of the samples is 25;
and 5: taking 1 part of the sample in the step 4, uniformly pouring the sample into the mixed solvent prepared in the step 3 at a constant speed, and standing for 3min after all the fine-grain metal powder is precipitated at the bottom of the mixed solvent;
step 6: counting the non-settled particles floating on the surface layer of the solvent to obtain the number of the impurities in the sample;
step 7, filtering the upper-layer inclusions and the bottom fine-particle-size nickel-based superalloy powder by using filter paper respectively, and recovering the mixed solvent for subsequent detection;
and 8, repeating the steps 5-7 until the counting of the number of the inclusions of all samples in the 3 groups is completed, taking the sum of the number of the inclusions of all samples as the content of the inclusions in the group of metal powder for each group of powder, taking the average value of the content of the obtained 3 groups of powder inclusions as the content of the inclusions in the batch of Inconel 718 powder, and taking the implementation result as shown in Table 4:
TABLE 4 statistics of the number of inclusions
Unit: an
In order to compare the implementation effect of the invention, the same batch of powder is selected to be subjected to manual screening of the same group as a comparison test, the manual screening result is that the content of inclusions in the Inconel 718 powder sample is 21, the total consumed labor hour is 13h, while the solvent detection method shown in Table 2 is used for detecting the content of inclusions in the Inconel 718 powder sample is 25, the total consumed labor hour is 4.5h, the properties of the separated inclusions are combined, the inclusions and the content in the powder are detected by adopting a solvent method, the separation of the inclusions is more accurate and comprehensive, and the total labor hour consumed by the solvent method is far lower than that consumed by the manual screening method for the case of more sample amount.
The solvent with certain density is prepared, the metal powder and the impurities are separated by utilizing the density difference of the metal powder and the impurities, the metal powder can be deposited at the bottom of the solution due to high density, and the impurities can float on the surface layer of the solution due to low density.
The mixed solvent adopted by the invention can not react with the metal powder to be detected and impurities, the true performance of the metal powder can be better reduced, the detection process time is shorter, the introduction of new impurities caused by overlong detection time is avoided, the prepared solvent can be repeatedly used by matching with filter paper, the detection efficiency is improved, and the detection cost is reduced.
The invention can identify the category of the inclusions obtained by separation through component analysis, carry out size statistics through microscopic measurement, and if the ceramic inclusions are too much, the smelting process of the master alloy needs to be checked; if the high molecular impurities are more, the powder preparation process should be checked reversely to see whether the equipment has high molecular material pollution, and the size of the impurities is used for judging whether the impurities with the size larger than the specified size exist in the powder.
While the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (5)
1. The method for detecting the inclusions in the fine-particle-size nickel-based superalloy powder is characterized by comprising the following steps of:
step 1: the mixed solvent for detection is prepared from the following components in percentage by volume: 50-65% of H3PO430 to 40% of CH2Cl25-10% of liquid Br2；
Step 2: measuring each solvent in the step 1 according to volume percentage, and adding CH into a beaker2Cl2Followed by slow addition of H3PO4Standing for 2-3 min, and dripping liquid Br2Obtaining a mixed solvent;
and step 3: uniformly stirring the mixed solvent obtained in the step 2 by using a stirring rod, standing for 10-15 min, wherein the density of the mixed solvent is 1.4-1.8 g/cm3；
And 4, step 4: preparing 3-5 groups of 240-1500 g of fine-particle-size nickel-based superalloy powder to be detected in the same batch, wherein each group is divided into 30-60 g samples by a balance, and the total number of the samples is 8-25;
and 5: uniformly pouring 1 part of the sample obtained in the step (4) into the mixed solvent prepared in the step (3) at a constant speed, and standing for 3-5 min after all the fine-grain-size nickel-based superalloy powder is precipitated at the bottom of the mixed solvent;
step 6: counting the non-settled particles floating on the surface layer of the mixed solvent to obtain the number of the impurities in the sample;
and 7: respectively filtering impurities on the upper layer and the nickel-based superalloy powder with the bottom fine particle size by using filter paper, and simultaneously recovering a mixed solvent for subsequent detection;
and 8, repeating the steps 5-7 until the counting of the number of the inclusions of all samples in all the groups is completed, obtaining the content of the inclusions in the batch of the fine-grain-size nickel-based superalloy powder to be detected, and performing reverse thrust and improvement on the technological process by identifying the types and sizes of the inclusions.
2. The method for detecting inclusions in fine-grained nickel-base superalloy powder according to claim 1, wherein the method comprises: in said step 1, H3PO4The concentration of (A) is 80-95%.
3. The method for detecting inclusions in fine-grained nickel-base superalloy powder according to claim 1, wherein the method comprises: in the step 4, the granularity of the nickel-based superalloy powder with the fine particle size to be detected is 0-60 mu m, and the density is 7.5-9.0 g/cm3。
4. The method for detecting inclusions in fine-grained nickel-base superalloy powder according to claim 1, wherein the method comprises: in the step 8, the sum of the number of all the part inclusions in each group is used as the content of the group of the fine-grain-size nickel-based superalloy powder inclusions to be detected, and the obtained content of all the group of the fine-grain-size nickel-based superalloy powder inclusions to be detected is averaged to obtain the content of the inclusions in the batch of the fine-grain-size nickel-based superalloy powder to be detected.
5. The method for detecting inclusions in fine-grained nickel-base superalloy powder according to claim 1, wherein the method comprises: in the step 8, the inclusions obtained by separation are subjected to category identification through component analysis, size statistics is carried out through microscopic measurement, and if the ceramic inclusions are excessive, the smelting process of the master alloy needs to be checked reversely; if the high molecular impurities are more, the powder preparation process needs to be checked reversely, and whether the equipment is polluted by high molecular materials or not is judged; the size of the inclusions is used to determine whether or not inclusions larger than a predetermined size are present in the powder.
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