CN114674859A - Sample holder for measuring surface segregation volatilization amount and using method thereof - Google Patents
Sample holder for measuring surface segregation volatilization amount and using method thereof Download PDFInfo
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- CN114674859A CN114674859A CN202210248070.3A CN202210248070A CN114674859A CN 114674859 A CN114674859 A CN 114674859A CN 202210248070 A CN202210248070 A CN 202210248070A CN 114674859 A CN114674859 A CN 114674859A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/227—Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
- G01N23/2276—Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM] using the Auger effect, e.g. Auger electron spectroscopy [AES]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2204—Specimen supports therefor; Sample conveying means therefore
Abstract
A sample holder for measuring surface polarization volatilization amount and a using method thereof. The method comprises the steps of utilizing a mode of combining an induction coil and a thermosensitive element to carry out in-situ heating and temperature control, adopting a high-purity platinum sheet to collect volatilized solutes or impurities, utilizing a low-temperature medium to be introduced into a clamping device to be cooled so as to effectively cool the platinum sheet and condense the volatilized solutes or impurities, and utilizing a rotating table in an analysis chamber to enable the platinum sheet to be in a test position, so that the types, the concentrations and the sequence of the volatilized elements can be directly measured. The sample rack can realize in-situ heating and accurate temperature control; the liquid nitrogen cooling system of the equipment can be directly utilized or other low-temperature media are introduced; the adopted platinum sheet has stable physical and chemical properties, and can be recycled by virtue of the argon ion cleaning function of the equipment. The sample holder can be used as a measurement accessory of advanced instrument equipment with high precision, ultrahigh vacuum environment and limited measurement room space, and has good application prospect.
Description
The application is divided application of application No. CN201910675137.X, application date 20190724, title of invention sample holder for measuring surface segregation volatilization amount and use method thereof
Technical Field
The invention belongs to an element concentration measuring device, relates to the measurement of volatile content of volatile elements, and is particularly suitable for being used as a measuring accessory of advanced instruments and equipment with high precision, ultrahigh vacuum environment and limited measuring room space.
Background
The surface of a metal or alloy, due to its surface energy, produces significant surface enrichment of solutes or foreign elements at a certain temperature. The solute or impurity elements enriched on the surface can have important influence on the elastic property, the optical property, the corrosion property, the catalytic property, the oxidation property, the stress corrosion property, the frictional wear property and the melting point of the alloy, thereby becoming a means for improving the material property in extensive research and application. However, when the vapor pressure of the solute or impurity element enriched on the surface is higher than the ambient pressure, the enriched solute or impurity may volatilize from the surface of the material, thereby directly affecting their concentration on the surface and the surface mechanical, physical and chemical properties of the material.
In 1966, the phenomenon of Li volatilization from the surface of polycrystalline Si was reported in the literature (Phys. status solidi (B)13(1966) 169). In 2017, a document (j. alloys comp.710 (2017)762) reported that Zn volatilizes from the surface of ZnSb particles to deteriorate the thermoelectric properties of ZnSb alloy. In 2019, the literature (j. alloys comp.797 (2019)640) theoretically studies the surface segregation kinetics of solutes or impurities under volatilization conditions, and verifies the theoretical correctness by taking an Al — Mg alloy and an IF steel as examples.
At present, advanced instruments such as an auger electron spectrometer and an X-ray photoelectron spectrometer are mainly used for judging the surface volatilization phenomenon, the change rule of the surface solute or impurity concentration along with the time or the temperature is measured under the environmental pressure of a vacuum analysis chamber, and whether the surface volatilization phenomenon exists is judged according to the descending trend of the surface concentration. Obviously, the method is an indirect determination method, and cannot accurately obtain the volatilization sequence of various volatilized solutes or impurities, and further cannot quantify volatilization dynamics according to volatilization quantities measured at different temperatures and different times, so that specific data of important physical parameters such as volatilization activation energy, volatilization flux and the like cannot be obtained. In addition, the law of the change of surface solutes or impurities, which is not done in the analysis chamber, does not allow in-situ heating and immediate analysis, which increases the error in the test results. Therefore, it is desirable to achieve in situ heating and directly measure the content of solutes or impurities volatilized from the surface. However, the solute or impurities volatilized from the surface are dispersed in the high vacuum environment of the vacuum analysis chamber, and are often removed from the vacuum analysis chamber by a molecular pump or the like at a low concentration, so that the volatilization amount cannot be accurately measured in the volatilization process. Therefore, it is necessary to develop a device that not only can heat the sample in situ, but also can be used to collect the solute or impurities volatilized from the surface, thereby providing support for quantitative measurement and research of the surface volatilization phenomenon.
The applicant finds out by studying the structural characteristics of the surface segregation testing instrument and summarizing the volatilization characteristics of the solute or impurities after the surface segregation: an induction coil can be added on the sample table to heat the sample table in situ, and a thermosensitive element is installed to control the temperature; suspending a metal sheet above the sample for collecting volatilized solutes or impurities; one side of the metal sheet, which is opposite to the sample, is used for collecting solute or impurities volatilized from the surface of the sample, and the other side of the metal sheet is welded with the clamping device so as to achieve the purpose that the metal sheet is suspended above the sample; in order to collect volatilized solutes or impurities more effectively, a clamping device welded with the metal sheet adopts a thin tube, a cooling medium is introduced during testing, and the metal sheet is cooled so as to condense the volatilized solutes or impurities; the amount of solute or impurities collected by condensation can then be measured by placing the metal sheet in the test position by means of a rotating table in the analysis chamber.
Disclosure of Invention
The invention provides a sample holder for measuring surface segregation volatilization, which can realize in-situ heating and solve the problem that instrument equipment can not directly measure surface volatile solute or impurities.
A sample holder for measuring surface segregation volatilization consists of a sample table 1, an induction coil 2, a segregation atom 3, a sample 4, a thermosensitive element 5, a volatilization atom 6, a condensation atom 7, a platinum sheet 8, a clamping and cooling device 9 and liquid nitrogen 10. The sample holder design is based on the sample table. The induction coil is arranged below the sample table and connected with the sample table in a spot welding mode, so that the temperature required for generating surface segregation and volatilization of a sample is provided for in-situ heating of the sample table, the problem that the previous test is transferred into an analysis chamber for testing after being heated in a sample conveying chamber is solved, the operation flow is reduced, and the interruption process of the test is also avoided. The thermosensitive element is implanted in the side surface of the sample table, so that the heating state of the induction coil and the heating temperature of the sample table can be controlled, the requirements of different heating temperatures are met, and the limited space occupied by the analysis chamber can be reduced. A sample is placed on the upper part of the sample table for detection and analysis. The platinum sheet is suspended above the sample and used as a condensation collection component, and the thermal stability and the chemical stability of the platinum sheet are utilized to prevent the condensation sheet from softening due to thermal radiation in the heating process of the sample or a sample table and also prevent volatile solute or impurities from generating chemical reaction with the condensation sheet, so that the characteristics of volatile substances are changed; meanwhile, the thickness is determined, the platinum sheet is guaranteed to be used for multiple times, the clamping and cooling device is prevented from being damaged due to repeated assembly and disassembly of the platinum sheet (if cooling media such as liquid nitrogen leak, the test equipment is damaged), and the vacuum degree in the analysis chamber is prevented from being reduced due to repeated assembly and disassembly. The clamping and cooling device is made of corrosion-resistant alloy thin tubes, so that the aim of preventing the volatilized solute or impurities from being corroded can be fulfilled; the platinum sheet is connected with the platinum sheet in a spot welding mode, so that the platinum sheet is suspended above the sample; the pipe is used as a clamping device, and a liquid nitrogen cooling system of the equipment can be used for cooling the platinum sheet, so that the condensation and collection effects of the platinum sheet are better; according to the cooling speed or the desublimation temperature of volatile solute and impurities, U-shaped, S-shaped, W-shaped welding modes and the like are adopted, and thin tubes with different inner diameters are selected, so that the temperature uniformity of the platinum sheet is ensured, and the requirements of the cooling speed and the cooling temperature under different test conditions are met; when the clamping device is turned over and the concentration of the solute or the impurity on the surface of the platinum sheet is tested, the heating of the induction coil can be stopped, so that the surface segregation of the sample and the volatilization process of the solute or the impurity are not interrupted, and the continuity of the test and the reliability of the result are ensured.
A method of using a sample holder as described above for measuring the amount of surface polarized evaporation, comprising the steps of:
(1) and an induction coil is arranged at the bottom of the sample table.
(2) Holes are drilled on the side of the sample table, and the thermosensitive element is implanted.
(3) And (4) selecting a high-purity platinum sheet for condensation and collection.
(4) A corrosion-resistant alloy thin tube is selected as a clamping device.
(5) A platinum sheet was spot welded to the alloy tubule.
(6) And introducing a cooling medium into the alloy thin tube to cool the platinum sheet.
(7) And stopping cooling when the preset time for heating the sample is reached, turning over the clamping device and testing the concentration of the solute or the impurity on the surface of the platinum sheet to obtain corresponding data.
In the step (1), the induction coil is arranged at the bottom of the sample table and can heat the sample table in situ, so that the temperature required by the surface segregation and volatilization of the sample is provided, the problem that the previous test is transferred into an analysis chamber for testing after being heated in a sample conveying chamber is solved, the operation flow is reduced, and the test interruption process is also avoided.
And (3) implanting a thermosensitive element in the step (2), so that the heating state of the induction coil and the heating temperature of the sample table can be controlled, the requirements of different heating temperatures are met, and the limited space occupied by the analysis chamber can be reduced.
In the step (3), the platinum sheet is selected as the condensation collecting component, and the thermal stability and the chemical stability of the platinum sheet are utilized to prevent the condensation sheet from softening caused by heat radiation in the heating process of the sample or the sample platform and also prevent the volatile solute or impurities from generating chemical reaction with the condensation sheet, thereby changing the characteristics of the volatile substances. The platinum sheet needs to have a certain thickness, so that the platinum sheet can be used for many times, the clamping and cooling device is prevented from being damaged by repeated dismounting and mounting of the platinum sheet (if cooling media such as liquid nitrogen leak, the test equipment is damaged), and the vacuum degree in the analysis chamber is prevented from being reduced due to repeated dismounting and mounting. The length and the width of the platinum sheet are selected according to the size of the sample or a sample table, but the size is not smaller than the length and the width of the sample, so that solutes or impurities volatilized from the surface of the sample are prevented from being collected by the condensation sheet, and the accuracy of a test result is influenced.
In the step (4), the corrosion-resistant alloy thin tube is selected as a clamping device, so that the aim of preventing the corrosion of volatilized solutes or impurities can be fulfilled; in addition, the pipe is used as a clamping device, and a liquid nitrogen cooling system of the equipment can be used for cooling the platinum sheet, so that the condensation and collection effects of the platinum sheet are better; meanwhile, U-shaped, S-shaped and W-shaped welding modes and thin tubes with different inner diameters are adopted according to the cooling speed or the desublimation temperature of volatile solutes and impurities, the uniformity of the temperature of the platinum sheet is guaranteed, and the requirements of the cooling speed and the cooling temperature under different test conditions are met.
In the step (5), the platinum sheet is spot-welded to the corrosion-resistant alloy pipe, so that the platinum sheet can be suspended, and the platinum sheet can be accurately suspended above the sample by adjusting the length of the alloy pipe, so that the volatilized solute or impurities can be collected more effectively.
In the step (6), besides introducing liquid nitrogen by using a liquid nitrogen cooling system of the device, different cooling media (such as a mixed solution of liquid nitrogen and alcohol) can be selected to collect volatilized solutes or impurities from the platinum sheet at different temperatures.
In the step (7), when the clamping device is turned over and the concentration of the solute or the impurity on the surface of the platinum sheet is tested, the heating of the induction coil can be stopped, so that the surface segregation of the sample and the volatilization process of the solute or the impurity are not interrupted, and the continuity of the test and the reliability of the result are ensured. In the conventional test method, the heating and cooling of the sample table are required to be stopped when the preset time is reached, then the surface concentration of the sample is measured, and the heating and time accumulation are carried out after the measurement, so that the obtained test result not only indirectly reflects the surface volatilization process, but also interrupts the test when each datum is measured, thereby causing great data error; and after the clamping device is adopted, the multiple interruption processes of the test are avoided, and the reliability of the test result is ensured.
The invention utilizes the combination of the induction coil and the thermosensitive element to carry out in-situ heating and temperature control, adopts the high-purity platinum sheet to collect volatilized solutes or impurities, utilizes the low-temperature medium to be introduced into the clamping device for cooling, thereby effectively cooling the platinum sheet and condensing the volatilized solutes or impurities, and utilizes the rotating table in the analysis chamber to enable the platinum sheet to be positioned at a test position, thereby directly measuring the types, concentrations and sequence of the volatilized elements. The sample holder can realize in-situ heating and accurate temperature control; the liquid nitrogen cooling system of the equipment can be directly utilized or other low-temperature media are introduced; the adopted platinum sheet has stable physical and chemical properties, and can be recycled by virtue of the argon ion cleaning function of the equipment; the clamping and cooling device is made of corrosion-resistant alloy, so that the purpose of corrosion resistance can be achieved. The sample holder for measuring the surface segregation volatilization amount, which is prepared by the method, can be used as a measuring accessory of advanced instruments and equipment with high precision, ultrahigh vacuum environment and limited measuring room space, and has good application prospect.
Drawings
FIG. 1 is a schematic diagram of solute surface segregation and solute diffusion within a matrix under volatilization conditions.
FIG. 2 is a schematic view of a measuring apparatus for surface-volatilized solutes or impurities prepared in the present invention.
The device comprises a sample table 1, an induction coil 2, a segregation atom 3, a sample 4, a thermosensitive element 5, a volatile atom 6, a condensation atom 7, a platinum sheet 8, a clamping and cooling device 9 and liquid nitrogen 10.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments.
The measuring device for the surface volatile solute or the impurity prepared by the invention comprises the following steps:
(1) mounting a spiral induction coil at the bottom of the sample table, and spot-welding the spiral induction coil at the bottom of the sample table; and repeatedly heating to the highest temperature, and checking the highest heating temperature, the heating speed and the point welding reliability of the induction coil.
(2) A hole is drilled in the side of the sample table, the diameter and depth of the drilled hole are determined according to the size of the thermosensitive element, and the thermosensitive element is implanted and connected to an external temperature display device.
(3) The segregation and volatilization of Mg elements on the surface of Al-Mg alloy is an alloy system which is most widely researched internationally, and the Al-Mg alloy has obvious representativeness; selecting a high-purity platinum sheet with the thickness not less than 1mm and the length and width not less than 20mm for condensing and collecting.
(4) The common nickel-based corrosion-resistant alloy Inconel600 thin tube is selected as a clamping device, the Inconel600 is widely applied to manufacturing of various complex equipment capillary tubes, the existing products are optional, low-temperature brittleness at the temperature of liquid nitrogen is not generated, and the purpose of good corrosion resistance can be achieved; as the sublimation temperature of Mg element is not high, the inner diameter of the Inconel600 tube can be 1-5 mm, and platinum sheets are spot-welded by adopting U-shaped, S-shaped, W-shaped and other modes.
(5) After a platinum sheet is spot-welded to an Inconel600 alloy thin tube, the platinum sheet is installed in a vacuum analysis chamber of an Auger electron spectrometer PHI595 type, liquid nitrogen is introduced and turned over for 3 times repeatedly, the time ratio of introducing the liquid nitrogen every time is less than 30min, and the spot welding firmness is verified.
(6) Connecting the Inconel600 alloy thin tube with the platinum sheet spot-welded to a cooling medium input system interface, sealing the interface by adopting an elastic gasket and a screwing nut, repeatedly introducing liquid nitrogen into the alloy thin tube for not less than 3 times, keeping the introduction time of the liquid nitrogen not less than 30min each time, ensuring that the interface has no leakage under the cold-hot alternating condition, and ensuring that the cooling temperature of the platinum sheet is lower than-80 ℃.
(7) Placing a sheet Al-Mg alloy sample in the middle of a sample table, starting an induction coil heating function, heating the Al-Mg alloy in an Auger electron spectrometer vacuum analysis chamber, heating to 300 ℃, and then preserving heat; argon ion sputtering is carried out on the platinum sheet collecting side for no less than 30 seconds in the heating process; stopping cooling when the preset heating time of the Al-Mg alloy is reached, turning over the clamping device, and testing the concentration of solute or impurity on the surface of the platinum sheet to obtain a corresponding Auger electron energy spectrogram, and obtaining corresponding concentration data through the energy spectrogram.
Example 1
(1) Installing a spiral induction coil at the bottom of the sample table, and fixing the spiral induction coil at the bottom of the sample table in a spot welding manner; repeatedly heating to the maximum temperature of 600 ℃, respectively heating at 5 ℃/min, 10 ℃/min, 20 ℃/min and the fastest heating speed, and finding that the heating capacity of the induction coil meets the requirement after inspection, and the spot welding fixation is firm.
(2) Drilling on the side of the sample table
The heat sensitive element is implanted and connected to an external temperature display device.
(3) Selecting Al-0.8 wt% Mg alloy as a test object; 4N high-purity platinum sheets are selected as condensation metal sheets, the thickness of the condensation metal sheets is 1mm, and the length and the width of the condensation metal sheets are 25mm and used for condensation collection.
(4) A widely-used nickel-based corrosion-resistant alloy Inconel600 thin tube is selected as a clamping device, the inner diameter of the thin tube is selected to be 2mm, and a platinum sheet is spot-welded in a U-shaped mode.
(5) And spot-welding a platinum sheet to the Inconel600 alloy thin tube, installing the platinum sheet in an Auger electron energy spectrometer PHI595 type vacuum analysis chamber, repeatedly introducing liquid nitrogen and overturning for 3 times, wherein the liquid nitrogen introduction time is 30min each time, and finding out that the spot-welded joint is firm after testing.
(6) Connecting the Inconel600 alloy thin tube subjected to spot welding of the platinum sheet to a cooling medium input system interface of an Auger electron spectrometer in-situ breaking device, and sealing the interface by adopting an elastic gasket and a screwed nut; and (3) repeatedly introducing liquid nitrogen into the alloy thin tube for 3 times, wherein the introduction time of the liquid nitrogen is 30min each time, the interface is found to have no leakage under the cold and hot alternating condition, and an electronic thermometer detects the cooling temperature of the platinum sheet to be-85 ℃.
(7) Placing a thin Al-Mg alloy sample with the thickness of 3mm and the length and the width of 10mm at the middle position of a sample table, starting the heating function of an induction coil, heating the Al-Mg alloy in a vacuum analysis chamber of an Auger electron spectrometer, heating to 300 ℃, and then preserving heat; performing argon ion sputtering on the platinum sheet collecting side for 30 seconds in the heating process; stopping cooling when the preset heating time of the Al-Mg alloy is reached for 10min, 30min and 60min respectively, turning over the clamping device, testing the concentration of solute or impurity on the surface of the platinum sheet to obtain corresponding Auger electron spectrograms, and obtaining the concentrations of 10.3 at%, 13.4 at% and 15.9 at% through the auger electron spectrograms.
Claims (5)
1. A sample holder for measuring surface segregation volatilization is characterized by consisting of a sample table (1), an induction coil (2), segregation atoms (3), a sample (4), a thermosensitive element (5), volatilization atoms (6), condensation atoms (7), a platinum sheet (8), a clamping and cooling device (9) and liquid nitrogen (10); the design of the sample rack takes a sample table as a reference; the induction coil is positioned below the sample table and connected with the sample table in a spot welding manner; implanting a thermosensitive element on the side surface of the sample table, controlling the heating state of the induction coil and the heating temperature of the sample table, and meeting the requirements of different heating temperatures; placing a sample on the upper part of the sample table for detection and analysis; the platinum sheet is suspended above the sample and used as a condensation collection component, and the thermal stability and the chemical stability of the platinum sheet are utilized to prevent the condensation sheet from softening due to thermal radiation in the heating process of the sample or a sample table and also prevent volatile solute or impurities from generating chemical reaction with the condensation sheet, so that the characteristics of volatile substances are changed; the clamping and cooling device is made of corrosion-resistant alloy thin tubes, so that the corrosion of volatilized solutes or impurities is prevented; and the platinum sheet is connected with the platinum sheet in a spot welding mode, so that the platinum sheet is suspended above the sample.
2. A method of using a sample holder for measuring the amount of surface-biased volatilization according to claim 1, comprising the steps of:
(1) installing a spiral induction coil at the bottom of the sample table, and spot-welding the spiral induction coil at the bottom of the sample table; repeatedly heating to the highest temperature, and checking the highest heating temperature, the heating speed and the firmness of spot welding of the induction coil;
(2) drilling a hole on the side surface of the sample table, determining the diameter and the depth of the drilled hole according to the size of the thermosensitive element, implanting the thermosensitive element, and connecting to an external temperature display device;
(3) the segregation and volatilization of Mg elements on the surface of the Al-Mg alloy are the most widely researched alloy systems internationally, and the Al-Mg alloy has obvious representativeness; selecting a high-purity platinum sheet, wherein the thickness is not less than 1mm, and the length and the width are not less than 20mm, and the high-purity platinum sheet is used for condensing and collecting;
(4) a common nickel-based corrosion-resistant alloy Inconel600 thin tube is selected as a clamping device, so that low-temperature brittleness at the temperature of liquid nitrogen is not generated, and a good corrosion prevention purpose can be achieved; in view of the fact that the sublimation temperature of Mg element is not high, 1-5 mm of the inner diameter of the Inconel600 pipe is selected, and a platinum sheet is spot-welded in a U-shaped mode, an S-shaped mode and a W-shaped mode;
(5) spot-welding a platinum sheet to an Inconel600 alloy thin tube, then installing the thin tube in an Auger electron spectrometer PHI595 type vacuum analysis chamber, repeatedly introducing liquid nitrogen for no less than 3 times and overturning, wherein the time ratio of introducing liquid nitrogen for each time is less than 30min, and verifying the firmness of spot welding;
(6) Connecting an Inconel600 alloy thin tube with a platinum sheet spot-welded to a cooling medium input system interface, sealing the interface by adopting an elastic gasket and a screwing nut, repeatedly introducing liquid nitrogen into the alloy thin tube for not less than 3 times, keeping the introduction time of the liquid nitrogen not less than 30min each time, ensuring that the interface has no leakage under the condition of alternating cold and heat, and ensuring that the cooling temperature of the platinum sheet is lower than-80 ℃;
(7) placing a sheet Al-Mg alloy sample in the middle of a sample table, starting an induction coil heating function, heating the Al-Mg alloy in an Auger electron spectrometer vacuum analysis chamber, heating to 300 ℃, and then preserving heat; argon ion sputtering is carried out on the platinum sheet collecting side for no less than 30 seconds in the heating process; stopping cooling when the preset heating time of the Al-Mg alloy is reached, turning over the clamping device, and testing the concentration of solute or impurity on the surface of the platinum sheet to obtain a corresponding Auger electron energy spectrogram, and obtaining corresponding concentration data through the energy spectrogram.
3. The method for using the sample holder for measuring the surface segregation volatilization amount according to claim 2, wherein the platinum sheet is selected as the condensation collection component in the step (3), and the thermal stability and the chemical stability of the platinum sheet are utilized to prevent the condensation sheet from softening due to the heat radiation in the sample or sample stage heating process, and prevent the volatilized solute or impurities from reacting with the condensation sheet chemically, thereby changing the characteristics of the volatilized substances; meanwhile, the platinum sheet has a certain thickness, so that the platinum sheet can be used for many times, the clamping and cooling device is prevented from being damaged by repeated assembly and disassembly of the platinum sheet, and the vacuum degree in the analysis chamber is prevented from being reduced due to repeated assembly and disassembly; in addition, the size of the platinum sheet is not less than the length and the width of the sample, and the phenomenon that solute or impurities volatilized from the surface of the sample are not collected by the condensation sheet to influence the accuracy of a test result can be prevented.
4. The use method of the sample holder for measuring the surface segregation volatilization amount according to claim 2, wherein the corrosion-resistant alloy thin tube is selected as the clamping device in the step (4), so that low-temperature brittleness at the temperature of liquid nitrogen is not generated, and the purpose of corrosion resistance can be achieved; in addition, the pipe is used as a clamping device, and a liquid nitrogen cooling system of the equipment can be used for cooling the platinum sheet, so that the condensation and collection effects of the platinum sheet are better; meanwhile, U-shaped, S-shaped and W-shaped welding modes and thin pipes with different inner diameters are adopted according to the cooling speed or the desublimation temperature of volatile solute and impurities, the uniformity of the temperature of the platinum sheet is guaranteed, and the requirements of the cooling speed and the cooling temperature under different test conditions are met.
5. The method for using the sample holder for measuring the surface segregation volatilization amount according to the claim 2, wherein when the clamping device is turned over and the concentration of the solute or the impurity on the surface of the platinum sheet is tested in the step (7), the heating of the induction coil is not stopped, so that the surface segregation of the sample and the volatilization process of the solute or the impurity are not interrupted, and the continuity of the test and the reliability of the result are ensured.
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| CN201910675137.XA CN110487834A (en) | 2019-07-24 | 2019-07-24 | It is a kind of for measuring the sample frame and its application method of Surface Segregation volatile quantity |
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| CN110487834A (en) * | 2019-07-24 | 2019-11-22 | 北京科技大学 | It is a kind of for measuring the sample frame and its application method of Surface Segregation volatile quantity |
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| CN110487834A (en) * | 2019-07-24 | 2019-11-22 | 北京科技大学 | It is a kind of for measuring the sample frame and its application method of Surface Segregation volatile quantity |
| CN210487657U (en) * | 2019-07-24 | 2020-05-08 | 北京科技大学 | Sample holder for measuring surface segregation volatilization amount |
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2019
- 2019-07-24 CN CN201910675137.XA patent/CN110487834A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110487834A (en) * | 2019-07-24 | 2019-11-22 | 北京科技大学 | It is a kind of for measuring the sample frame and its application method of Surface Segregation volatile quantity |
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