CN111781043A - Sample preparation method for measuring oxygen content of nickel-based superalloy - Google Patents
Sample preparation method for measuring oxygen content of nickel-based superalloy Download PDFInfo
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- CN111781043A CN111781043A CN202010657380.1A CN202010657380A CN111781043A CN 111781043 A CN111781043 A CN 111781043A CN 202010657380 A CN202010657380 A CN 202010657380A CN 111781043 A CN111781043 A CN 111781043A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
Abstract
The invention provides a sample preparation method for measuring oxygen content of a nickel-based superalloy, which comprises the following steps: a) digging a primary sample by using a wire cutting machine; b) performing lathe machining on the primary sample through a lathe to obtain a first sample; c) performing lathe machining on the first sample through a lathe to obtain a second sample; d) performing lathe machining on the second sample through a lathe to obtain a third sample; e) grinding and polishing the third sample to obtain a fourth sample; f) cutting off the head and the tail of the fourth sample, cutting the rest part into a sheet sample, and then placing the sheet sample in a container filled with a solvent for ultrasonic cleaning; g) and putting the sheet sample into a container filled with acetone, ultrasonically cleaning and drying to obtain a sample to be detected. The sample preparation method for measuring the oxygen content of the nickel-based superalloy is convenient to operate, can be used for accurately measuring the oxygen content of the nickel-based superalloy, reduces instability in subsequent turning through turning of a shorter primary sample length, and is high in operability.
Description
Technical Field
The invention relates to the technical field of sample preparation, in particular to a sample preparation method for measuring oxygen content of a nickel-based superalloy.
Background
Nickel-base superalloys are widely used in the manufacture of power turbines and related parts for the aerospace industry, such as turbine blades, guide vanes, turbine disks, high pressure compressor disks and combustors and other high temperature components for aircraft, naval and industrial gas turbines. Residual oxygen in the high-temperature alloy usually exists in the form of inclusions, and creep rupture performance and instantaneous tensile and impact properties are influenced; meanwhile, the oxygen has strong affinity with active elements in the high-temperature alloy, such as Al, Ti and the like, so that inclusions are generated, and the strengthening effect of strengthening elements is weakened, therefore, the accurate measurement of the oxygen content in the nickel-based high-temperature alloy is crucial to the product quality, and the oxygen content is required to be accurately measured, so that the influence on the accuracy of a measurement result caused by the fact that external oxygen is brought into a sample is reduced to the maximum extent in the first step; the nickel-based superalloy forms a compact protective oxide film at room temperature, the protective body is further oxidized, so that external oxygen is brought to influence the determination of the oxidation amount, and the higher the temperature is, the higher the content of the external oxygen brought by a sample is.
GB/T11261 pulse heating melting inert gas melting-infrared absorption method for measuring the oxygen content of steel is a common method for measuring the nickel-based superalloy, but the technical reason of the terms is not explained in all national standards, including the GB/T11261, and the technical principle of the terms and the technical principle behind the terms is not fully understood by operators, so that external oxygen is brought in the sample preparation process, and the oxygen content in the nickel-based superalloy cannot be accurately measured.
Disclosure of Invention
The invention aims to overcome and supplement the defects in the prior art and provide a sample preparation method for measuring the oxygen content of a nickel-based superalloy. The technical scheme adopted by the invention is as follows:
a sample preparation method for measuring oxygen content of nickel-based superalloy is disclosed, wherein: the method comprises the following steps:
a) digging a primary sample by using a wire cutting machine;
b) carrying out turning on the primary sample by a lathe, adding cooling liquid in the turning, and turning off 15-25 mu m to obtain a first sample;
c) carrying out turning on the first sample through a lathe, adding cooling liquid in the turning, and turning off 10-15 microns to obtain a second sample;
d) carrying out turning on the second sample by a lathe, adding cooling liquid in the turning, and turning off the second sample by 3-5 microns to obtain a third sample;
e) grinding and polishing the third sample to obtain a fourth sample;
f) cutting off the head and the tail of the fourth sample, then cutting the rest part into a sheet sample, and placing the sheet sample in a container filled with a solvent for ultrasonic cleaning;
g) and putting the sheet sample into a container filled with acetone, ultrasonically cleaning and drying to obtain a sample to be detected.
Preferably, the sample preparation method for measuring the oxygen content of the nickel-based superalloy is as follows: the shape of the primary sample in the step a) is a round bar shape, the length is 50-80 mm, and the diameter is 4.5-5 mm.
Preferably, the sample preparation method for measuring the oxygen content of the nickel-based superalloy is as follows: and the vehicle speed in the step b) is 850-1000 r/min.
Preferably, the sample preparation method for measuring the oxygen content of the nickel-based superalloy is as follows: and c) the vehicle speed in the vehicle manufacturing in the step c) is 600-750 r/min.
Preferably, the sample preparation method for measuring the oxygen content of the nickel-based superalloy is as follows: the vehicle speed in the step d) is 400-600 r/min, and the surface roughness Ra of the third sample is 1.5-2.5 mu m.
Preferably, the sample preparation method for measuring the oxygen content of the nickel-based superalloy is as follows: the step e) of grinding and polishing comprises the following steps:
holding the third sample, starting a lathe at the rotating speed of 400-600 r/min, and grinding and polishing the rotating sample once by using 100-200-mesh silicon carbide abrasive cloth or sand paper, wherein the surface roughness Ra of the ground and polished sample is 0.5-1.0 mu m;
and carrying out secondary grinding and polishing on the primarily ground and polished third sample through polishing cloth, wherein the surface roughness Ra of the sample after grinding and polishing is 0.1-0.5 mu m.
Preferably, the sample preparation method for measuring the oxygen content of the nickel-based superalloy is as follows: the solvent in the step f) is carbon tetrachloride or diethyl ether, and the ultrasonic cleaning time is 4-6 min.
Preferably, the sample preparation method for measuring the oxygen content of the nickel-based superalloy is as follows: and g) ultrasonic cleaning for 4-6 min.
Preferably, the sample preparation method for measuring the oxygen content of the nickel-based superalloy is as follows: and g) measuring the oxygen content of the sample to be measured in the step g) within 0-10 min.
The invention has the advantages that:
(1) the sample preparation method for measuring the oxygen content of the nickel-based superalloy is convenient to operate, can be used for accurately measuring the oxygen content of the nickel-based superalloy, reduces instability in subsequent turning through turning of a shorter primary sample length, and is high in operability.
(2) According to the sample preparation method for measuring the oxygen content of the nickel-based superalloy, the progressive turning is adopted, the reasonable vehicle speed is combined, the sample is greatly reduced from external oxygen caused by high temperature, the operation is simple, the surface smoothness of the sample can be improved, and an oxide film formed on the surface of the sample at room temperature can be conveniently removed in cooperation with subsequent polishing; the slice weight of each test is controlled in a narrow range, so that the stability and the accuracy of the oxygen content measurement result are better; the sheet sample is placed in a beaker filled with acetone for storage, oxygen is isolated, the exposure time of the sample in the air before the test is strictly controlled, the interference of external oxygen on the detection of the oxygen content of the sample is basically avoided, and the sample preparation is made for truly measuring the oxygen content of the nickel-based superalloy.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1:
a sample preparation method for measuring oxygen content of a nickel-based superalloy selects an ingot with the mark of Inconel 600 to prepare a sample, and comprises the following steps:
a. digging a round bar-shaped primary sample by using linear cutting, wherein the length of the round bar-shaped primary sample is 50mm, and the diameter of the round bar-shaped primary sample is 4.5 mm;
b. carrying out turning on the primary sample by a lathe, wherein the turning is carried out for 15 microns at the speed of 850r/min under the condition of adding cooling liquid to obtain a first sample;
c. turning the first sample by a lathe, wherein the turning is carried out for 10 mu m at the speed of 600r/min, and the turning is carried out under the condition of adding cooling liquid to obtain a second sample;
d. turning the second sample by a lathe, wherein the turning is carried out for 3 micrometers, the vehicle speed is 400r/min, the turning is carried out under the condition of adding cooling liquid, and the surface roughness Ra of the sample is 1.7 micrometers to obtain a third sample;
e. holding the third sample by a lathe, starting the lathe at the rotating speed of 400r/min, grinding and polishing the rotating sample by using 100-mesh silicon carbide abrasive cloth or sand paper, wherein the surface roughness Ra of the sample is 0.8 mu m, polishing by using polishing cloth, and obtaining a fourth sample, wherein the surface roughness Ra of the polished sample is 0.3 mu m;
f. immediately cutting off the head and the tail of the fourth sample by using wire cutting pliers wiped by carbon tetrachloride or ether, cutting the rest part into small flaky samples, dropping the small flaky samples into a beaker filled with the carbon tetrachloride or the ether, wherein the weight of each small flaky sample is 0.1-0.5 g, the flaky samples are relatively consistent in size and stable in quality, each small flaky sample is kept at 0.3 +/-0.1 g, putting the beaker filled with the small flaky samples into an ultrasonic cleaning tank for cleaning for 4min,
g. clamping the sample into a beaker filled with acetone by using tweezers, putting the beaker into an ultrasonic cleaning tank again for cleaning for 4min, clamping the sample into the beaker filled with acetone by using tweezers wiped clean by carbon tetrachloride or ether, covering and storing the beaker, taking out the tweezers wiped clean by carbon tetrachloride or ether after test conditions are prepared, drying the tweezers to obtain a sample to be tested, and putting the sample to be tested into the test within 10 min.
The oxygen content of the sample to be tested in example 1 is measured according to GB/T11261-2006 "determination of oxygen content of steel-pulse heating melting inert gas melting-infrared absorption method", which is specifically shown in Table 1:
TABLE 1
As can be seen from Table 1, the sample prepared by the method has low oxygen content, which indicates that the sample brings little external oxygen, is close to the true value of the oxygen content in the material, the standard deviation and variance results have better stability, and the numerical deviation degree and the dispersion degree are low, so that the result of the oxygen content measured by the method is reliable.
Example 2:
a sample preparation method for measuring oxygen content of a nickel-based superalloy selects an ingot with the mark of Inconel 600 to prepare a sample, and comprises the following steps:
a. digging a round bar-shaped primary sample by using linear cutting, wherein the length of the round bar-shaped primary sample is 80mm, and the diameter of the round bar-shaped primary sample is 5 mm;
b. carrying out turning on the primary sample by a lathe, wherein the turning is carried out for 25 mu m at the speed of 1000r/min under the condition of adding cooling liquid to obtain a first sample;
c. turning the first sample by a lathe, wherein the turning is carried out for 15 microns at the speed of 750r/min, and the turning is carried out under the condition of adding cooling liquid to obtain a second sample;
d. turning the second sample by a lathe, wherein the turning is carried out for 5 micrometers, the vehicle speed is 600r/min, the turning is carried out under the condition of adding cooling liquid, and the surface roughness Ra of the sample is 1.5 micrometers to obtain a third sample;
e. holding the third sample by a lathe, starting the lathe at the rotating speed of 600r/min, and grinding and polishing the rotating sample by using 200-mesh silicon carbide abrasive cloth or sand paper, wherein the surface roughness Ra of the sample is 0.7 mu m; polishing with polishing cloth to obtain a fourth sample, wherein the surface roughness Ra of the polished sample is 0.2 mu m;
f. immediately cutting off the head and the tail of the fourth sample by using wire cutting pliers wiped by carbon tetrachloride or ether, cutting the rest part into small flaky samples, and dropping the small flaky samples into a beaker filled with the carbon tetrachloride or ether, wherein the weight of each small flaky sample is 0.1-0.5 g, the flaky samples are relatively consistent in size and stable in quality, each small flaky sample is kept at 0.2 +/-0.1 g, and the beaker filled with the small flaky samples is placed into an ultrasonic cleaning tank for cleaning for 6 min;
g. clamping the sample into a beaker filled with acetone by using tweezers, putting the beaker into an ultrasonic cleaning tank again for cleaning for 6min, clamping the sample into a new beaker filled with acetone by using tweezers wiped clean by carbon tetrachloride or ethyl ether, covering and storing the beaker, taking out the sample by using the tweezers wiped clean by carbon tetrachloride or ethyl ether for drying after test conditions are prepared, and putting the sample into a test within 10 min.
The oxygen content of the sample to be measured in example 2 is measured according to GB/T11261-2006 "determination of oxygen content of steel-pulse heating melting inert gas melting-infrared absorption method", which is specifically shown in Table 2:
table 2:
as can be seen from Table 2, the sample prepared by the method of the present invention has a low oxygen content, which indicates that the sample has little external oxygen and is close to the true value of the oxygen content in the material; from the standard deviation and variance results, the sample prepared by the method has better stability and lower numerical deviation degree and dispersion degree, and the result of the oxygen content measured by the method is reliable.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (9)
1. A sample preparation method for measuring oxygen content of nickel-based superalloy is characterized by comprising the following steps: the method comprises the following steps:
a) digging a primary sample by using a wire cutting machine;
b) carrying out turning on the primary sample by a lathe, adding cooling liquid in the turning, and turning off 15-25 mu m to obtain a first sample;
c) carrying out turning on the first sample through a lathe, adding cooling liquid in the turning, and turning off 10-15 microns to obtain a second sample;
d) carrying out turning on the second sample by a lathe, adding cooling liquid in the turning, and turning off the second sample by 3-5 microns to obtain a third sample;
e) grinding and polishing the third sample to obtain a fourth sample;
f) cutting off the head and the tail of the fourth sample, then cutting the rest part into a sheet sample, and placing the sheet sample in a container filled with a solvent for ultrasonic cleaning;
g) and putting the sheet sample into a container filled with acetone, ultrasonically cleaning and drying to obtain a sample to be detected.
2. The method of sample preparation for oxygen content measurement of nickel-base superalloys of claim 1, further comprising: the shape of the primary sample in the step a) is a round bar shape, the length is 50-80 mm, and the diameter is 4.5-5 mm.
3. The method of sample preparation for oxygen content measurement of nickel-base superalloys of claim 1, further comprising: and the vehicle speed in the step b) is 850-1000 r/min.
4. The method of sample preparation for oxygen content measurement of nickel-base superalloys of claim 1, further comprising: and c) the vehicle speed in the vehicle manufacturing in the step c) is 600-750 r/min.
5. The method of sample preparation for oxygen content measurement of nickel-base superalloys of claim 1, further comprising: the vehicle speed in the step d) is 400-600 r/min, and the surface roughness Ra of the third sample is 1.5-2.5 mu m.
6. The method of sample preparation for oxygen content measurement of nickel-base superalloys of claim 1, further comprising: the step e) of grinding and polishing comprises the following steps:
holding the third sample, starting a lathe at the rotating speed of 400-600 r/min, and grinding and polishing the rotating sample once by using 100-200-mesh silicon carbide abrasive cloth or sand paper, wherein the surface roughness Ra of the ground and polished sample is 0.5-1.0 mu m;
and carrying out secondary grinding and polishing on the primarily ground and polished third sample through polishing cloth, wherein the surface roughness Ra of the sample after grinding and polishing is 0.1-0.5 mu m.
7. The method of sample preparation for oxygen content measurement of nickel-base superalloys of claim 1, further comprising: the solvent in the step f) is carbon tetrachloride or diethyl ether, and the ultrasonic cleaning time is 4-6 min.
8. The method of sample preparation for oxygen content measurement of nickel-base superalloys of claim 1, further comprising: and g) ultrasonic cleaning for 4-6 min.
9. The method of sample preparation for oxygen content measurement of nickel-base superalloys of claim 1, further comprising: and g) measuring the oxygen content of the sample to be measured in the step g) within 0-10 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113532979A (en) * | 2021-06-08 | 2021-10-22 | 先导薄膜材料有限公司 | Preparation method of aluminum scandium target material sample |
| CN114112590A (en) * | 2021-11-26 | 2022-03-01 | 山东钢铁股份有限公司 | Treatment method of gear steel oxygen content detection sample |
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