CN107741449B - testing device for martensite volume fraction in austenitic stainless steel - Google Patents
testing device for martensite volume fraction in austenitic stainless steel Download PDFInfo
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Abstract
The invention relates to the technical field of metallographic detection, and aims to provide a device for testing the volume fraction of martensite in austenitic stainless steel. In the device, a hydrogen cylinder group and an argon cylinder group are respectively connected to a pneumatic booster pump; the pneumatic booster pump is connected to the test environment box through a gas pipeline, and a buffer tank, a mass spectrometer and a vacuum system are arranged on the gas pipeline; the test environment box consists of an upper end cover and a box body which are fixedly connected by fastening bolts; the box body is provided with a hollow inner cavity, and a heat exchange jacket is arranged on the outer side of the box body; the end cover is provided with a through end cover through hole, and the tail end of the gas circuit pipeline is connected with the end cover through hole; a sample support is arranged in a cavity of the box body, a heating assembly is arranged on a platform of the sample support, and the upper surface of the heating assembly is used for placing a sample. The testing device provided by the invention can be used for accurately measuring the integral martensite volume fraction in the austenitic stainless steel, and compared with the existing testing method, the testing device provided by the invention has the advantages that the obtained measurement data is more accurate, and the real condition of the sample can be reflected better.
Description
Technical Field
The invention belongs to the technical field of metallographic detection, and particularly relates to a device for testing the volume fraction of martensite in austenitic stainless steel.
Background
Austenitic stainless steels are widely used in modern industry due to their good corrosion resistance and mechanical properties. Austenitic stainless steels typically undergo a martensitic transformation during the manufacturing process due to plastic deformation. After martensite phase transformation occurs due to the difference of the mechanical properties and corrosion resistance of martensite and austenite, the performance of the austenitic stainless steel is also changed. In order to control the properties of austenitic stainless steels, it is important to know the volume fraction of martensite inside them. At present, methods commonly used for measuring the volume fraction of martensite in austenitic stainless steel are divided into three types, one type is that the martensite and the austenite present different colors by adopting a corrosion method, and then the volume fraction of the martensite is approximately estimated by carrying out area statistics on corresponding color areas, the methods are easy to introduce human errors, the test area selection randomness is large, and the test accuracy is low; the other type is a testing means based on technologies such as X-ray diffraction or electron back scattering diffraction, although the technology can relatively accurately measure the volume fraction of martensite on the surface or near surface of a tested area, the testing result cannot accurately represent the volume fraction condition of the martensite in a sample, and the testing result has great one-sidedness; in addition, equipment such as a ferrite measuring instrument can be used for estimating the martensite content in the sample, but the method belongs to an indirect testing means, and not only needs other direct testing means to carry out data calibration, but also has lower testing precision.
disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provides a device for testing the volume fraction of martensite in austenitic stainless steel.
in order to solve the technical problem, the solution of the invention is as follows:
The device for testing the volume fraction of martensite in the austenitic stainless steel comprises a hydrogen cylinder group for providing hydrogen for testing and an argon cylinder group for providing replacement gas; the hydrogen cylinder group and the argon cylinder group are respectively connected to the inlet end of the pneumatic booster pump; the pneumatic booster pump is also connected to the test environment box through a gas pipeline, and a buffer tank, a flow regulating valve, a mass spectrometer, a vacuum system and an emptying valve are arranged on the gas pipeline;
The test environment box consists of an upper end cover and a lower box body which are fixedly connected through fastening bolts; the box body is provided with a hollow inner cavity, and a heat exchange jacket is arranged on the outer side of the box body; the heat exchange jacket is provided with a heat medium outlet and a heat medium inlet which are respectively connected to the heat exchange system through pipelines; the end cover is provided with a through end cover through hole, and the tail end of the gas circuit pipeline is connected with the end cover through hole; a sample support is arranged in a cavity of the box body, a heating assembly is arranged on a platform of the sample support, and the upper surface of the heating assembly is used for placing a sample;
the device also comprises a control system which is respectively connected to power ends of the pneumatic booster pump, the heat exchange system and the vacuum system through signal lines; a temperature detection probe is arranged in the heat exchange jacket and is connected to a control system through a signal wire.
in the invention, an O-shaped ring made of alloy material for sealing is arranged at the connecting part between the end cover and the box body.
In the invention, the sample support is made of quartz, and is suspended below the end cover or fixedly supported at the bottom of the box body or on the inner wall of the box body.
In the invention, the surface of the inner wall of the box body is provided with a glass lining layer with the thickness of not less than 10 mm.
when the device is applied to the volume fraction test of martensite in austenitic stainless steel, the device specifically comprises the following steps:
(1) Placing a sample to be tested on a heating assembly of the sample support, and screwing a fastening bolt to enable the end cover to be in airtight joint with the box body;
(2) Pumping out air in the test environment box and the connected gas circuit pipeline by using a vacuum system until the vacuum degree of the system reaches a set value; hydrogen filling is carried out on the test environment box by using a pneumatic booster pump until the pressure of the hydrogen in the test environment box reaches 20-30 MPa and is stabilized at a certain fixed value P in the interval;
(3) Controlling a heat exchange system to heat a heating medium in a heat exchange jacket to 250-350 ℃ and stabilizing the temperature at a certain fixed value T within a range1(ii) a Keeping the temperature for not less than 72 hours, and carrying out hot hydrogen filling on the sample to be tested;
(4) Controlling the heat exchange system to reduce the temperature of the heating medium in the heat exchange jacket to-50 to-100 ℃ at a speed of not less than 50 ℃/min and stabilize the temperature at a certain fixed value T in the interval2(ii) a Opening an emptying valve to discharge hydrogen in the test environment box and the buffer tank while cooling, and performing at least 3 times of replacement on the system by using argon after discharging; then closing the emptying valve and vacuumizing the system; the vacuum degree reaches 1.0 multiplied by 10-6Pa or below and the temperature of the heat medium is stabilized at T2Then, starting a mass spectrometer to monitor the real-time content of hydrogen in the atmosphere environment in the test environment box;
(5) The heating assembly was run and ramped up to 500 ℃ at a constant ramp rate and held at temperatureover 30 minutes; in the process, the real-time content of hydrogen in the atmosphere environment in the test environment box is always monitored, and the temperature of the heat medium in the heat exchange jacket is kept at T2and stopping monitoring work of the mass spectrometer after 30 minutes, integrating the real-time content data of the hydrogen monitored by the mass spectrometer with time, and calculating to obtain the total release quantity Q of the hydrogen in the sample to be detected1；
(6) closing the heating assembly, the mass spectrometer and the vacuum system in sequence, and setting a heat exchange system to enable the temperature of a heating medium in the heat exchange jacket to reach room temperature finally;
(7) Separating the end cover and the box body, and taking out a sample to be tested; loading pure austenite standard sample with the same material grade and the same shape and size as the sample to be detected, and repeating the operations in the steps (1) to (6) to obtain the total hydrogen release amount Q of the standard sample in the step (5)2；
in the operation process of the step, the pressure value P of the test environment box and the temperature T during hot hydrogen charging in the two tests are ensured1And temperature T at the time of hydrogen evolution2The numerical values of the two are kept consistent;
(9) According to the data measured by the two tests, the volume fraction of martensite in the sample to be measured is calculated as follows:
(Q2-Q1)/Q2，％。
In the invention, the heating temperature of the heating assembly is not lower than 500 ℃, and the heating rate is not lower than 30 ℃/min; the heat exchange temperature range of the heat exchange system is-100 to 350 ℃.
preferably, the end cover and the box body are made of A286 alloy material with good hydrogen embrittlement resistance. The mass spectrometer is a triple quadrupole mass spectrometer, and the mass number of the triple quadrupole mass spectrometer ranges from 0amu to 50 amu. The vacuum system consists of a mechanical vacuum pump and a molecular pump, and the flow rate of the vacuum system can ensure that the vacuum degree in the test environment box reaches 1.0 multiplied by 10-6Pa and below. The buffer tank is made of austenitic stainless steel S31603 with good hydrogen embrittlement resistance, and the design pressure is not lower than 70 MPa. The shape of the sample is a square thin sheet, the thickness is 0.5-1 mm, and the length of the sample is not less than 10 mm.
Description of the inventive principles:
The volume fraction of martensite is determined by utilizing the difference of hydrogen solubility in two phases of austenite and martensite. The solubility of hydrogen in austenite is about one thousand times of that of hydrogen in martensite, so that for a piece of martensite-containing austenitic stainless steel, after the austenite stainless steel is subjected to hydrogen charging treatment, the total content of hydrogen in a sample is determined by the volume fraction of austenite in the sample, the content of hydrogen dissolved in martensite can be ignored, and the volume fraction of martensite can be calculated after the volume fraction of austenite is obtained according to the content of hydrogen in the sample.
Based on the principle, firstly, carrying out high-temperature and high-pressure hydrogen charging treatment on a sample to be measured (because the diffusion coefficient of hydrogen in austenite at normal temperature is particularly low, the only feasible hydrogen charging method is high-temperature and high-pressure hydrogen charging) until the hydrogen is saturated in the sample, then immediately measuring the hydrogen content in the sample, wherein the hydrogen content measurement adopts a method of heating up and hydrogen desorption in vacuum; and then, carrying out hydrogen charging treatment on a pure austenite standard sample with the same material grade and the same shape and size as the sample to be tested, testing the hydrogen content in the standard sample, and calculating the volume fraction of martensite in the sample to be tested by comparing the hydrogen content in the sample to be tested with the hydrogen content in the standard sample.
Compared with the prior art, the invention has the beneficial effects that:
The testing device provided by the invention can be used for testing, the integral martensite volume fraction in the austenitic stainless steel can be accurately obtained, and compared with the prior testing method which only can realize the determination technology of the martensite volume fraction on the surface or near surface of the sample, the testing device provided by the invention can obtain more accurate measurement data and can reflect the real condition of the sample.
drawings
FIG. 1 is a schematic view of the overall apparatus of the present invention;
FIG. 2 is a view showing the construction of the test environment chamber and the internal structure thereof according to the present invention.
In the figure: the device comprises a hydrogen cylinder group 1, a pneumatic booster pump 2, a buffer tank 3, a flow regulating valve 4, an emptying valve 5, a vacuum system 6, a mass spectrometer valve 7, a mass spectrometer 8, a test environment box 9, a heat exchange system 10, a control system 11, an argon cylinder group 12, a fastening bolt 13, an end cover 14, an O-shaped ring 15, a sample support 16, a heat exchange jacket 17, a heat medium inlet 18, a box body 19, a glass lining layer 20, a heat medium outlet 21, a heating component 22, a sample 23 and an end cover through hole 24.
Detailed Description
Fig. 1 shows a volume fraction testing apparatus for martensite in austenitic stainless steel in the present embodiment, which includes a hydrogen cylinder group 1 for supplying hydrogen gas for testing, and an argon cylinder group 12 for hydrogen gas replacement in the system. The outlets of the hydrogen cylinder group 1 and the argon cylinder group 12 are both connected to the pneumatic booster pump 2, and the outlet of the pneumatic booster pump 2 is connected to the buffer tank 3. The buffer tank 3 is made of austenitic stainless steel S31603 with good hydrogen embrittlement resistance, and the design pressure is not lower than 70 MPa. In order to control the gas flow, a flow regulating valve 4 is arranged in an outlet pipeline of the buffer tank 3. The gas flowing through the flow control valve 4 is sent to a test environment box 9 in one path, and is connected with a vent valve 5 in the other path. A vacuum system 6, a mass spectrometer valve 7 and a mass spectrometer 8 are also arranged in the pipeline between the flow regulating valve 4 and the test environment box 9. Wherein the vacuum system 6 is composed of a mechanical vacuum pump and a molecular pump, and the flow rate of the vacuum system 6 can make the vacuum degree in the test environment box 9 reach 1.0 multiplied by 10-6Pa and below. The mass spectrometer 8 is a triple quadrupole mass spectrometer with a mass number ranging from 0amu to 50amu, and the mass spectrometer 8 is mainly used for monitoring the hydrogen content in the test environment box 9 in a vacuum environment. The heat exchange system 10 is connected with a heat exchange jacket 17 on the outer side of the test environment box 9 to realize the regulation and control of the temperature of the test environment box 9, the heat exchange temperature range of the heat exchange system 10 is-100-350 ℃, and the whole system is monitored and controlled by the control system 11.
as shown in fig. 2, the main body of the test environment box 9 is composed of an end cover 14 and a box body 19, the end cover 14 and the box body 19 are made of a286 alloy steel having excellent hydrogen embrittlement resistance, the two parts are connected by a fastening bolt 13, an O-ring 15 for sealing is provided at the connecting part, and the O-ring 15 is made of a high temperature resistant alloy. The end cover 14 is provided with an end cover through hole 24, and the end cover through hole 24 is used for the inlet and outlet of gas in the test environment box 9 and the monitoring of gas concentration. The lower end of the end cover 14 is connected with a sample support 16, the sample support 16 is made of quartz which does not absorb hydrogen, and a heating assembly 22 and a sample 23 are sequentially arranged on the sample support 16. The heating temperature of the heating assembly 22 is not lower than 500 ℃, the heating rate is not lower than 30 ℃/min, the sample 23 is a square thin sheet, the thickness is 0.5-1 mm, and the length of the sample is not less than 10 mm. The inner surface of the box body 19 is provided with a glass lining layer 20 to avoid the absorption of hydrogen, the thickness of the glass lining layer 20 is not less than 10mm, the outer part of the box body 19 is provided with a heat exchange jacket 17, and the heat exchange jacket 17 is respectively provided with a heat medium inlet 18 and a heat medium outlet 21.
The method for testing by using the device for testing the volume fraction of martensite in the austenitic stainless steel is described as follows:
(1) Firstly, separating an end cover 14 from a box body 19, and after a sample 23 to be tested is arranged, hermetically connecting the end cover 14 with the box body 19 by using a fastening bolt 13;
(2) And (3) pumping out residual air in the test environment box 9 and the auxiliary pipeline by using a mechanical vacuum pump of the vacuum system 6, and closing the vacuum system 6 until the vacuum degree in the system reaches a set value. Filling high-pressure hydrogen into the test environment box 9 by using a pneumatic booster pump 2 until the pressure of the hydrogen in the test environment box 9 reaches a certain fixed value P within the interval of 20-30 MPa;
(3) adjusting the set temperature of the heat exchange system 10 to a certain fixed value T within the range of 250-350 DEG C1Then, the temperature is kept for not less than 72 hours, so that the thermal hydrogen charging of the sample 23 to be tested is realized, and the hydrogen content in the sample 23 can be saturated;
(4) The temperature of the heat exchange system 10 is set to be reduced to a certain fixed value T within the range of-50 to-100 ℃ at the speed of not less than 50 ℃/min2And then the temperature remains unchanged. And (3) opening the emptying valve 5 to discharge the high-pressure hydrogen in the test environment box 9 and the buffer tank 3 while cooling, and performing at least 3 times of replacement on the hydrogen in the system by using the argon bottle group 12 after the discharge is completed. The air release valve 5 is closed, then the vacuum system 6 is opened, and when the vacuum degree in the test environment box 9 reaches 1.0 multiplied by 10-6Pa below and the temperature of the heat exchange system 10 is stabilized at T2Then, opening a mass spectrometer valve 7, and starting a mass spectrometer 8 to monitor the real-time content of hydrogen in the atmosphere environment in the test environment box 9;
(5) The heating assembly 22 is operated and brought up to 500 c at a constant ramp rate, maintaining the temperature of 500 c above 500 c30 minutes; in the process, the real-time content of hydrogen in the atmosphere environment in the test environment box 9 is always monitored, and the temperature of the heating medium in the heat exchange jacket 17 is kept at T2and stopping the monitoring work of the mass spectrometer 8 after 30 minutes, and calculating the total release quantity Q of the hydrogen in the sample 23 to be detected by integrating the real-time content data of the hydrogen monitored by the mass spectrometer 8 with time1。
(6) And closing the heating component 22, the mass spectrometer 8, the mass spectrometer valve 7 and the vacuum system 6 in sequence, and setting the temperature of the heat exchange system 10 to be the room temperature until the temperature in the test environment box 9 reaches the room temperature.
(7) Separating the end cover 14 and the box body 19, installing a pure austenite standard sample with the same material grade and the same shape and size as the sample 23 to be tested, and then connecting the end cover 14 and the box body 19 in a sealing way by using a fastening bolt 13. Repeating the above processes to obtain total hydrogen gas emission amount Q2P, T in two tests should be kept in the process1And T2Is constant; the volume fraction of martensite in the sample 23 to be measured is (Q)2-Q1)/Q2％。
As described above, the volume fraction of martensite in the sample to be tested is calculated by comparing the dissolved hydrogen amounts of the sample to be tested and the standard sample under the same hydrogen charging condition, and the whole martensite volume fraction in one austenitic stainless steel can be more accurately obtained by utilizing the testing device and the testing method provided by the invention, rather than the existing testing method which only can realize the measurement of the martensite volume fraction on the surface or near surface of the sample; according to the invention, the hydrogen charging and hydrogen content measurement of the sample 23 are completed in the same test environment box 9, so that the release of hydrogen in the sample 23 in the hydrogen charging and hydrogen releasing interval process is reduced to the maximum extent, and the test reliability is improved; the inner surface of the test environment box 9 and the sample support 16 are made of the glass lining layer 20 or quartz which does not absorb hydrogen, and the materials do not absorb hydrogen in the hydrogen charging process and do not discharge hydrogen in the hydrogen discharging process, so that the influence on the hydrogen content test result is avoided, in the hydrogen content test process, the heating assembly 22 is used for locally heating the sample 23, and the heat exchange system 10 is used for cooling the test environment box 9, so that the release of hydrogen in other members which are not the sample is reduced to the maximum extent, and the test reliability is improved.
Although the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Any simple modification, equivalent change and modification made to the above embodiment according to the technical essence of the present invention are still within the technical scope of the present invention, unless the content of the technical solution of the present invention is departed from.
Claims (4)
1. a testing device for martensite volume fraction in austenitic stainless steel comprises a hydrogen cylinder group for providing hydrogen for test and an argon cylinder group for providing replacement gas; the device is characterized in that the hydrogen cylinder group and the argon cylinder group are respectively connected to the inlet ends of the pneumatic booster pumps; the pneumatic booster pump is also connected to the test environment box through a gas pipeline, and a buffer tank, a flow regulating valve, a mass spectrometer, a vacuum system and an emptying valve are arranged on the gas pipeline;
The test environment box consists of an upper end cover and a lower box body which are fixedly connected through fastening bolts; the box body is provided with a hollow inner cavity, and the outer side of the box body is provided with a heat exchange jacket; the heat exchange jacket is provided with a heat medium outlet and a heat medium inlet which are respectively connected to the heat exchange system through pipelines; the end cover is provided with a through end cover through hole, and the tail end of the gas circuit pipeline is connected with the end cover through hole; a sample support is arranged in a cavity of the box body, a heating assembly is arranged on a platform of the sample support, and the upper surface of the heating assembly is used for placing a sample;
The device also comprises a control system which is respectively connected to power ends of the pneumatic booster pump, the heat exchange system and the vacuum system through signal lines; a temperature detection probe is arranged in the heat exchange jacket and is connected to a control system through a signal wire.
2. The apparatus of claim 1, wherein an O-ring of an alloy material for sealing is provided at a connection portion between the end cap and the case.
3. the apparatus of claim 1, wherein the sample holder is made of quartz, and the sample holder is suspended below the end cap or is fixedly supported on the bottom of the box body or the inner wall of the box body.
4. The apparatus according to claim 1, wherein the inner wall surface of the tank body has a glass-lined layer having a thickness of not less than 10 mm.
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