CN107144483B - Nanometer indentation multi-field test system based on liquid nitrogen refrigeration - Google Patents
Nanometer indentation multi-field test system based on liquid nitrogen refrigeration Download PDFInfo
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- CN107144483B CN107144483B CN201710329318.8A CN201710329318A CN107144483B CN 107144483 B CN107144483 B CN 107144483B CN 201710329318 A CN201710329318 A CN 201710329318A CN 107144483 B CN107144483 B CN 107144483B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/54—Performing tests at high or low temperatures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0076—Hardness, compressibility or resistance to crushing
- G01N2203/0078—Hardness, compressibility or resistance to crushing using indentation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
- G01N2203/0222—Temperature
- G01N2203/0226—High temperature; Heating means
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
- G01N2203/0222—Temperature
- G01N2203/0228—Low temperature; Cooling means
Abstract
The application discloses a nano indentation multi-field test system based on liquid nitrogen refrigeration, which comprises a nano indentation device unit, a temperature changing unit, a refrigeration unit, a digital display and regulator unit, a temperature acquisition unit and a control computer unit, wherein the refrigeration unit is sealed in a sealed cavity, the nano indentation device unit is respectively connected with the temperature changing unit, the temperature acquisition unit and the digital display and regulator unit, the temperature changing unit is connected with the refrigeration unit, and the control computer unit is connected between the digital display and regulator unit and the temperature acquisition unit.
Description
Technical Field
The application relates to the technical field of nanoindentation tests, in particular to a nanoindentation multi-field test system based on liquid nitrogen refrigeration.
Background
In recent years, as new materials are synthesized and preparation processes are continuously improved, the characteristic dimensions of the materials are smaller and smaller, and a series of problems of clamping and centering can occur when the materials are subjected to mechanical parameter measurement by using a traditional standard test. For this reason, researchers have proposed a method of nano indentation test by referring to the conventional hardness test.
The nano indentation test technology is mainly characterized in that a load-indentation depth relation curve is obtained by continuously recording load and indentation depth, and finally mechanical parameters such as hardness, elastic modulus and the like of a tested material are obtained by analyzing the curve. During the test, the searching of the indentation position and the measurement of the indentation residual area are avoided, and the test error can be greatly reduced. The indentation load and indentation depth data are obtained through indentation test, then a corresponding load-depth relation curve is drawn, and rich mechanical parameter information can be obtained from the curve analysis through proper mechanical model and deduction.
The traditional micro-nano indentation tester tests materials at normal temperature, and the working environment of the new materials is very complex and can not be directly affected by temperature. For example, in recent years, superconducting materials are used in large quantities, and mechanical property testing of superconducting materials at low temperature is a problem to be solved urgently; also, some devices that assist in the tremendous exploration of people are also subject to low temperature environments. The Japanese university of rock-hand Y.Yoshino et al develops a macroscopic indentation testing device for materials at low temperature, but the problems of accurate temperature control and displacement load signal detection and the like are not solved, and the structure is complicated and huge and can not meet the requirement of microscopic precise indentation of a micro-nano indentation instrument in the traditional sense.
Disclosure of Invention
The application aims to overcome the defects, and provides a nano indentation multi-field test system based on liquid nitrogen refrigeration, which can measure the mechanical properties of superconducting materials in a low-temperature and variable-temperature environment and provide reliable experimental conditions for describing the mechanical properties of the superconducting materials along with temperature changes.
The purpose of the application is realized in the following way: the system comprises a nanoindentation device unit, a temperature changing unit, a refrigerating unit, a digital display and regulator unit, a temperature acquisition unit and a control computer unit, wherein the refrigerating unit is sealed in a sealed cavity, the nanoindentation device unit is respectively connected with the temperature changing unit, the temperature acquisition unit and the digital display and regulator unit, the temperature changing unit is connected with the refrigerating unit, the control computer unit is connected between the digital display and regulator unit and the temperature acquisition unit, the nanoindentation device unit comprises a test bed for mounting a low-temperature or high-temperature superconducting sample to be tested, the upper part of the test bed is in an opening form so as to facilitate the direct contact of the nanoindentation head, the opening part is connected with a replacement device, the replacement device is used for replacing air in an opening part of a test bed and preventing sample frosting and mist from affecting observation and measurement in the experimental process, the replacement device comprises a pressure gauge II and a helium bottle II, the pressure gauge II is connected between the helium bottle II and the test bed, the pressure gauge II is further connected with a digital display and regulator unit, the temperature changing unit comprises a cryostat, the cryostat comprises a heater and a thermometer, the heater is used for heating the test bed through adjusting output power to achieve temperature changing, the refrigeration unit comprises a low-temperature valve, a pressure gauge I, a helium bottle I and a liquid nitrogen tank, the low-temperature valve is respectively connected with the temperature changing unit, the digital display and regulator unit, the liquid nitrogen tank and the helium bottle I, and the pressure gauge I is connected between the low-temperature valve and the helium bottle I, and the low-temperature valve is used for regulating flow of refrigeration media.
The heater and the thermometer adopt separate vacuum plugs, and the leads are arranged separately so as not to generate mutual interference.
The sealing cavity is made of nonmagnetic stainless steel 316L, the pipeline surface of the refrigerating unit is wrapped by a plurality of layers of heat insulation materials, and the number of layers of the wrapped heat insulation materials is not less than 40.
The test bed is made of high-purity copper, and the support for supporting the test bed is made of G10 material.
The cryostat is mounted on a suspension pad which is movable with the movement of the test bed.
Four holes are symmetrically formed in the periphery of the upper end of the test bed, and the four holes are used for introducing helium into the test bed.
The application has the advantages that:
1. the temperature change measurement of the sample temperature range from room temperature 300K to liquid nitrogen 77K (under standard atmospheric pressure) is realized, and the temperature error is controlled at 1K;
2. the temperature of the experimental sample is reduced and raised rapidly, and the experimental sample can be maintained for about 20 minutes at a certain temperature measuring point in the measuring temperature range;
3. the low-temperature refrigeration part has compact design structure and easy sample replacement. The mode of opening holes is adopted to meet the requirements of observation and normal operation of the pressure head of the nanoindentation instrument, the design of the gas circuit is reasonable, and the measurement cannot be interfered;
4. helium is adopted as a replacement and purging medium, the air at the opening part of the experimental sample table is purged and replaced, fog and frosting are not generated in the whole observation and experiment process, and the air inflow of the helium is controllably regulated and digitally displayed;
5. the low-temperature refrigerating unit is enclosed in the sealed cavity, and the vacuum degree is better than 1 multiplied by 10 -4 Pa, integral vacuum leak detection, leak rate superior to 1×10 -8 Pam 3 /s；
6. The operation is simple and convenient in the experimental process, the structural design is reliable, the device is suitable for long-term use, and the maintenance is convenient; the material of the low-temperature refrigeration part is uniform in material quality and good in thermal stability; the system temperature has a wider adjusting range; simple manufacturing process, easy material acquisition, low price and other basic principles.
Drawings
FIG. 1 is a schematic diagram of the structure of the present application;
FIG. 2 is a flow chart of the operation of the present application;
FIG. 3 is a cross-sectional view of the laboratory bench of the present application;
fig. 4 is a view showing the installation effect of the present application.
Detailed Description
The application is further described below with reference to the accompanying drawings.
The application relates to a nano indentation multi-field test system based on liquid nitrogen refrigeration, which comprises a nano indentation device unit, a temperature changing unit, a refrigeration unit, a digital display and regulator unit, a temperature acquisition unit and a control unitThe system comprises a computer unit, a nano indentation device unit, a temperature changing unit, a temperature acquisition unit, a digital display and regulator unit, a refrigerating unit, a control computer unit, a test bed and a replacement device, wherein the nano indentation device unit comprises a test bed and a replacement device, the test bed is made of high-purity copper with higher thermal conductivity, the upper part of the test bed is in an opening form, four small holes are symmetrically formed in the periphery of the upper end of the test bed, the four small holes are connected with the replacement device, the replacement device comprises a pressure gauge II and a digital display and regulator bottle II, the pressure gauge II is connected between the pressure gauge II and the test bed, the pressure gauge II is additionally connected with the digital display and regulator unit, the temperature changing unit is respectively connected with the test bed and the refrigerating unit, and comprises cryostats consisting of a heater and a thermometer, wherein the heater and the thermometer respectively adopt independent vacuum plugs, leads are separately arranged, the cryostat is arranged on a suspension pad, the suspension pad is arranged below the test bed and can move along with the movement of the test bed, the refrigerating unit is sealed in a sealed cavity made of nonmagnetic stainless steel 316L, the connecting and transition parts in the refrigerating unit adopt copper woven belts, the inner pipeline surface is wrapped by a plurality of layers of heat insulation materials, the number of the heat insulation materials is 50, the supporting parts for supporting the refrigerating unit adopt G10 materials, and the vacuum degree in the cavity is superior to 1X 10 -4 Pa, refrigerating unit includes low temperature valve, manometer I, helium bottle I and liquid nitrogen container, and low temperature valve connects low temperature thermostat, digital display and regulator unit, liquid nitrogen container and helium bottle I respectively, is connected with manometer I between low temperature valve and the helium bottle I, and control computer connects between temperature acquisition unit and digital display and regulator unit.
The application is realized by the following steps:
firstly, placing a tested superconducting material sample (hereinafter referred to as a sample) on a test bed on a nano indentation test device, regulating a low-temperature valve to control the flow of liquid nitrogen to be maximum, wherein the temperature of the test bed is 77K (the temperature of a real-time display system can be displayed from a digital display and regulator), observing the sample through an opening at the upper part of the test bed, and introducing helium in the replacement device into the test bed for replacing air in the test bed to prevent the sample from frosting and generating fog to influence the observation and measurement in the test process, and keeping micro positive pressure; when the output power of the heater is regulated, the temperature of the test bed can be quickly increased, the temperature change control is realized, the temperature change range reaches-77K to 300K, and the temperature can be maintained for about 20 minutes at a certain temperature measuring point.
Finally, it should be noted that: it is apparent that the above examples are only illustrative of the present application and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications which may be extended therefrom are within the scope of the present application.
Claims (6)
1. The utility model provides a many fields of nanometer indentation test system based on liquid nitrogen refrigeration, its characterized in that includes nanometer indentation device unit, alternating temperature unit, refrigerating unit, digital display and regulator unit, temperature acquisition unit and control computer unit, refrigerating unit seals in sealed cavity, the alternating temperature unit is connected respectively to nanometer indentation device unit, temperature acquisition unit and digital display and regulator unit, alternating temperature unit connects refrigerating unit, be connected with control computer unit between digital display and regulator unit and the temperature acquisition unit, sealed cavity material adopts nonmagnetic stainless steel 316L, supports the supporting part adoption G10 material of sealed cavity, the vacuum is better than 1×10 in the cavity -4 Pa；
The nanometer indentation device unit comprises a nanometer indentation device, a test bed and a replacement device, wherein the test bed is used for installing a low-temperature or high-temperature superconductive sample to be tested, the upper part of the test bed is in an opening form so as to facilitate the direct contact of the nanometer indentation pressure head, the opening part is connected with the replacement device, helium in the replacement device is introduced into the test bed and is used for replacing air in an opening part of the test bed, the observation and measurement of the sample affected by frosting and fog are prevented in the experimental process, the replacement device comprises a pressure gauge II and a helium bottle II, the pressure gauge II is connected between the helium bottle II and the test bed, the pressure gauge II is also connected with the digital display and regulator unit,
the temperature changing unit comprises a cryostat, the cryostat comprises a heater and a thermometer, the heater heats the experiment table by adjusting output power to realize temperature changing,
the refrigerating unit comprises a low-temperature valve, a pressure gauge I, a helium bottle I and a liquid nitrogen tank, wherein the low-temperature valve is respectively connected with the temperature changing unit, the digital display and regulator unit, the liquid nitrogen tank and the helium bottle I, the pressure gauge I is connected between the low-temperature valve and the helium bottle I, and the low-temperature valve is used for regulating the flow of refrigerating medium.
2. The nano-indentation multi-field test system based on liquid nitrogen refrigeration according to claim 1, wherein the heater and the thermometer are separate vacuum plugs, and leads are arranged separately so as not to interfere with each other.
3. The nano indentation multi-field test system based on liquid nitrogen refrigeration as claimed in claim 1, wherein the pipeline surface of the refrigeration unit is wrapped by a plurality of layers of heat insulation materials, the number of layers of the wrapped heat insulation materials is not less than 40, and the connection and transition parts of all the components in the refrigeration unit are woven by copper braids.
4. The nano indentation multi-field test system based on liquid nitrogen refrigeration as claimed in claim 1, wherein the test bed is made of high-purity copper, and the support for supporting the test bed is made of G10 material.
5. The nano-indentation multi-field test system based on liquid nitrogen refrigeration according to claim 1, wherein the cryostat is mounted on a suspension pad which is movable with the movement of the test bed.
6. The nano indentation multi-field test system based on liquid nitrogen refrigeration according to claim 1 or 4, wherein four holes are symmetrically formed in the periphery of the upper end part of the test bed, and the four holes are used for introducing helium into the test bed.
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| CN107144483B true CN107144483B (en) | 2023-10-03 |
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| CN108535129B (en) * | 2018-04-16 | 2022-04-01 | 吉林大学 | Low-temperature micro-nano indentation testing system with large stroke and low temperature drift under microscopic assembly |
| CN110470555B (en) * | 2019-08-26 | 2022-04-01 | 吉林大学 | Non-vacuum atmosphere type refrigerating system of low-temperature micro-nano indentation testing system |
| CN110779818A (en) * | 2019-10-22 | 2020-02-11 | 中国科学院合肥物质科学研究院 | Superconducting conductor low-temperature mechanical performance testing method |
| CN110736672B (en) * | 2019-11-13 | 2022-05-24 | 吉林大学 | Normal-pressure immersed type continuous low-temperature micro-nano indentation testing device |
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| CN107144483A (en) | 2017-09-08 |
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