CN107421825A - A kind of nano impress device based on GM refrigeration machines - Google Patents
A kind of nano impress device based on GM refrigeration machines Download PDFInfo
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- CN107421825A CN107421825A CN201710329319.2A CN201710329319A CN107421825A CN 107421825 A CN107421825 A CN 107421825A CN 201710329319 A CN201710329319 A CN 201710329319A CN 107421825 A CN107421825 A CN 107421825A
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- G—PHYSICS
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D27/00—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00
- G05D27/02—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00 characterised by the use of electric means
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Abstract
The invention discloses a kind of nano impress device based on GM refrigeration machines, including refrigeration unit, thermal swing units, nano impress unit, data acquisition unit and control unit, wherein refrigeration unit connection thermal swing units, thermal swing units connect nano impress unit, nano impress unit connects data acquisition unit, control unit connects thermal swing units, nano impress unit and data acquisition unit respectively, and the present invention can meet that sample temperature is adjustable in the range of room temperature to liquid helium temperature, and the rate of heat addition is adjustable.For testing the mechanical property of different temperatures and different superconductors, using liquid nitrogen and helium as cooling medium, without liquid helium, cost is reduced, dependence and limitation to liquid helium can be broken away from.Effective influence of the vibration to test result for solving GM refrigeration machines, and fast, registration is responded, accurate change control temp, the Precision measurement of displacement load signal, microcosmic accurate press-in can be realized.
Description
Technical field
The present invention relates to nano indentation test technical field, specifically a kind of nano impress dress based on GM refrigeration machines
Put.
Background technology
In recent years, as new material synthesis and preparation technology improve constantly, its characteristic size is less and less, is using tradition
Code test when carrying out mechanics parameter measurement to it, it may appear that a series of problems, such as clamping, centering.Nanoindentation conduct
A kind of effective means that mechanics characterization is carried out in nanoscale, researcher use for reference traditional hardness test, it is proposed that nanometer pressure
The method of trace test.Micro-nano impression test is due to high load and displacement resolution, being developing progressively as material micro-nano
The mainstream technology of rice Mechanics Performance Testing, leads in material science, semiconductor technology, film, biomethanics, biomedical engineering etc.
Domain shows important scientific meaning and is widely applied prospect.At present, the state such as the U.S., Switzerland, Britain has grasped this technology,
And have commercialized impression/scarification tester device product, and China starts late in terms of impression/cut measuring technology, there is no
The commercialization impression instrument nano-indenter test technology of autonomous production, which mainly passes through, continuously records load and compression distance so as to obtain
Loading-indentation depth relation curve is obtained, the parameters such as the consistency and elasticity modulus of measured material are obtained eventually through analysis curve.Survey
The searching to Indentation position and the measurement of impression residual area are avoided during examination, the error of test can be greatly reduced.It is logical
Cross impression test and obtain loading of pressing in and compression distance data, corresponding load-deepness relation curve is drawn afterwards, by suitable
Mechanical model and derivation, abundant mechanics parameter information can be obtained from the tracing analysis.
The micro-nano impress tester of tradition is all that material is tested at normal temperatures, due to the working environment ten of new material
Divide complexity, inevitably by the direct effect of temperature.Such as, superconductor starts a large amount of use and superconduction material in recent years
The Mechanics Performance Testing of material at low temperature is exactly to need urgently to solve the problems, such as；Equally, people are aided in carry out the one of polar region exploration
A little equipment will also face the test of low temperature environment.Japanese Yan Shou universities Y. Yoshino et al. have developed material in low temperature
Macroscopic view press-in test device, but the problems such as all without the Precision measurement for solving accurate change control temp, displacement load signal, and tie
The more numerous and diverse requirement huge, that the microcosmic accurate press-in of micro-nano impression instrument in traditional sense can not be met of structure.
The content of the invention
It is an object of the invention to overcome above-mentioned deficiency, there is provided a kind of nano impress device based on GM refrigeration machines, can
Accurate alternating temperature, and extent of alternating temperature is big（4.2K-300K）, while the dependence and limitation to liquid helium are broken away from, effectively solve GM systems
Influence of the vibration of cold to test result.
The object of the present invention is achieved like this：A kind of nano impress device based on GM refrigeration machines, including thermal swing units,
Refrigeration unit, nano impress unit, data acquisition unit and control unit, refrigeration unit connection thermal swing units, thermal swing units connect
Nano impress unit, nano impress unit connection data acquisition unit are connect, control unit connects thermal swing units, nano impress respectively
Unit and data acquisition unit,
Refrigeration unit include liquid nitrogen container, outer Dewar, cold screen, cold screen cooling tube, helium tank, GM refrigeration machines, GM refrigerator compressors,
Refrigeration machine coil pipe, aseismatic mechanism, liquid helium vessel, condenser, liquid helium level meter, coil heat exchanger and fixed nitrogen container, GM refrigeration machines
One end is connected with GM refrigerator compressors, and the other end is connected by condenser with liquid helium vessel, and refrigeration machine is wound with condenser
Coil pipe, refrigeration machine coil pipe are connected with helium tank, and liquid helium level meter is vertical to be arranged in liquid helium vessel, and cold screen is cooled down by cold screen
Pipe is connected with liquid nitrogen container, and liquid helium vessel and fixed nitrogen container are installed in cold screen, and cold screen is arranged in outer Dewar, and aseismatic mechanism is set
Put below GM refrigeration machines and be connected with outer Dewar, connected between liquid helium vessel and fixed nitrogen container by coil heat exchanger, GM systems
Cold is by the room temperature helium precooling in helium tank and is condensed into liquid helium, is transferred in liquid helium vessel, liquid helium passes through coil heat exchanger
Indirect heat exchange is carried out with liquid nitrogen, by liquid solidification until fixed nitrogen temperature is arranged under sample stage close to liquid helium temperature, fixed nitrogen container；
Thermal swing units include cold finger, copper braid over braid and heater, and cold finger is arranged in fixed nitrogen container, and heater is arranged on sample stage
Bottom, heater are woven by copper and are connected with cold finger；
Nano impress unit includes vacuum (-tight) housing, sample stage, mobile device, pressure sensor, depression bar, nano impress probe and atom
Force microscope, vacuum (-tight) housing provide an independent vacuum environment for nano impress, and sample stage is used for placing laboratory sample, mobile dress
Put above sample stage, mobile device is used for control pressure sensor, depression bar and AFM and moved in XYZ directions
Dynamic, pressure sensor is used for measuring depression bar stress, and nano impress probe is arranged on depression bar lower end, atomic force microscope observation impression
Point position and Indentation Process；
The information of data acquisition unit collection includes liquid helium liquid level and pressure, the pressure in fixed nitrogen container, sample in liquid helium vessel
The pressure that displacement, impression speed and the pressure sensor that platform temperature, heater power, mobile device are obtained are obtained；
Control unit includes control computer, and control computer is respectively used to show and controls liquid helium liquid level and pressure in liquid helium vessel
Power, the pressure in fixed nitrogen container, the power of heater, sample stage temperature, the displacement of mobile device, impression speed and depression bar pressure
Power.
Further, observation window is provided with sample room, observation window is used to observing and measuring sample Indentation position.
Further, mobile device includes X and shown to, Y-direction and Z-direction shift servo motor and grating scale sensor and atomic force
Micro mirror, X are used for adjusting mobile device X to displacement to servomotor, and Y-direction servomotor is used for adjusting mobile device Y-direction displacement, Z
It is used for adjusting pressure sensor, depression bar and AFM to Z-direction movement to servomotor, grating scale sensor is used to measure
Sample Indentation position, atomic force microscope observation impression point position and Indentation Process.
Preferably, depression bar is invar.
Preferably, coil heat exchanger is length thin tube.
Further, aseismatic mechanism includes bellows and location structure, and shockproof bellows is made up of copper braid over braid.
The advantage of the invention is that：
1st, inventive samples temperature temperature in the range of room temperature to liquid helium temperature is adjustable, and the rate of heat addition is adjustable, and sample can be achieved and exist
Refrigeration and alternating temperature in the range of 4.2K-300K；
2nd, the present invention uses GM refrigeration machines that helium liquefies as liquid helium, without the external world using liquid nitrogen and helium as cooling medium
Liquid helium is directly provided, cost is reduced, dependence and limitation to liquid helium can be broken away from；
3rd, vibration abatement is added, influence of the vibration to test result for effectively solving GM refrigeration machines；
4th, present apparatus response is fast, registration, can realize the accurate Precision measurement, microcosmic for becoming control temp, displacement load signal
Precision press-in.
Brief description of the drawings
Fig. 1 is a kind of front view of the nano impress device based on GM refrigeration machines of the present invention；
Fig. 2 is a kind of front view of the mobile device of the nano impress device based on GM refrigeration machines of the present invention；
Fig. 3 is a kind of structural representation of the nano impress device based on GM refrigeration machines of the present invention；
Wherein, 1- liquid nitrogen containers；2- liquid nitrogen valves；The cold screens of the outer Dewar 4- of 3-；The cold screen cooling tubes of 5-；6- nitrogen atmospheric valves；7- fixed nitrogen
Container entrance pipeline;8- fixed nitrogen container outlet pipelines;9- helium tanks;10-GM refrigerator compressors；11-GM refrigeration machines；12-
Aseismatic mechanism;13- refrigeration machine coil pipes；14- liquid helium vessels;15- condensers；16- liquid helium level meters;17- helium exports;18-
Coil heat exchanger;19- fixed nitrogen containers;20- cold fingers;21- copper braid over braids；22- heaters；23- sample stages；24- samples;
25- vacuum (-tight) housings；26-X is to servomotor；27-Y is to servomotor；28-Z is to servomotor；29- pressure sensors;30- atoms
Force microscope;31- depression bars；32- nano impress is popped one's head in;33- data acquisition units；34- control units.
Embodiment
The invention will be further described below in conjunction with the accompanying drawings.
The present invention is a kind of nano impress device based on GM refrigeration machines, including refrigeration unit, thermal swing units, nano impress
Unit, data acquisition unit and control unit, refrigeration unit connection thermal swing units, thermal swing units connection nano impress unit, receive
Rice impression unit connection data acquisition unit, control unit connect nano impress unit, refrigeration unit, thermal swing units, received respectively
Rice impression unit and data acquisition unit.
Refrigeration unit include liquid nitrogen container 1, outer Dewar 3, cold screen 4, cold screen cooling tube 5, helium tank 9, GM refrigeration machines 11 and its
Compressor 10, refrigeration machine coil pipe 13, aseismatic mechanism 12, liquid helium vessel 14, condenser 15, liquid helium level meter 16, coil heat exchanger
18th, fixed nitrogen container 19 etc., liquid nitrogen container 1 is cold screen 4 and fixed nitrogen container 19 provides liquid nitrogen, outer Dewar 3 provides a vacuum environment,
Cold screen 4 and cold screen cooling tube 5 provide a low temperature environment, and helium tank 9 provides room temperature helium, and the one end of GM refrigeration machines 11 is freezed with GM
Machine compressor 10 is connected, and the other end is connected by condenser 15 with liquid helium vessel 14, and refrigeration machine coil pipe is wound with condenser 15
13, refrigeration machine coil pipe 13 is connected with helium tank 9, and liquid helium level meter 16 is vertical to be arranged in liquid helium vessel 14, and cold screen 4 is by cold
Screen cooling tube 5 is connected with liquid nitrogen container 1, and liquid helium vessel 14 and fixed nitrogen container 19 are installed in cold screen 4, and cold screen 4 is arranged on outer Du
In watts 3, aseismatic mechanism 12 is arranged on the lower section of GM refrigeration machines 11 and is connected with outer Dewar 3, liquid helium vessel 14 and fixed nitrogen container 19 it
Between connected by coil heat exchanger 18, liquid nitrogen is input in fixed nitrogen container 19 by liquid nitrogen container 1 by fixed nitrogen container entrance pipeline 7,
GM refrigeration machines 11 are by the room temperature helium precooling in helium tank 9 and are condensed into liquid helium, are transferred in liquid helium vessel 14, liquid helium passes through disk
Heat exchange of heat pipe 18 carries out indirect heat exchange with liquid nitrogen, by liquid solidification until fixed nitrogen temperature is installed close to liquid helium temperature, fixed nitrogen container 19
Under sample stage 23.
Thermal swing units include cold finger 20, copper braid over braid 21, heater 22, and cold finger 20 is arranged on the top of fixed nitrogen container 19,
For conducting cold to reduce the temperature difference, copper braid over braid 21 is used for connecting cold finger 20 and heater 22, and heater 22 is arranged on sample
The bottom of platform 23, alternating temperature is realized by adjusting power output specimen heating holder 23.
Nano impress unit includes vacuum (-tight) housing 26, sample stage 23, mobile device, pressure sensor 29, depression bar 31 and nanometer
Impression probe 32, AFM 30, vacuum (-tight) housing 26 provide an independent vacuum environment for nano impress, and sample stage 23 is used
To place laboratory sample, mobile device is arranged on above sample stage, and mobile device is used for control pressure sensor 29, the and of depression bar 31
AFM 30 moves in XYZ directions, and pressure sensor 29 is used for measuring the stress of depression bar 31, the installation of nano impress probe 32
In the lower end of depression bar 31, AFM 30 observes impression point position and Indentation Process.
The information that data acquisition unit 33 gathers includes the pressure in liquid helium liquid level and pressure, fixed nitrogen container in liquid helium vessel
The displacement that power, sample stage temperature, heater power, mobile device are obtained is to determine the position of impression point, impression speed, pressure
The information such as the pressure that sensor is obtained,
Control unit 34 includes control computer, control computer be respectively used to show and control in liquid helium vessel liquid helium liquid level and
Pressure, the pressure in fixed nitrogen container, the power of heater, sample stage temperature, the displacement of mobile device, impression speed and depression bar pressure
The information such as power.The present apparatus is realized in function：
1. whole device is placed on air floating platform, prevent extraneous vibration from influenceing measurement accuracy；
2. sample is fixed on experimental bench, is moved by X to Y-direction servo linear motor to both direction, pass through Z-direction electricity
Machine realizes that magnifying glass Z-direction moves, and carries out preliminary observation close to sample, records the locus by control section, then remove
Microscope, indenter device is moved to the position；
3. closing sample room, sample room is vacuumized, is better than 10 to vacuum-4During Pa, stopping vacuumizes closing and taken out very
Empty valve；
4. outer Dewar is vacuumized, when vacuum reaches 10-4During Pa, stop vacuumizing；
5. opening the outlet of cold screen pipeline, be passed through the cold screen of liquid nitrogen cooling from the entrance of cold panel pipe surrounds dress to reduce cold screen
The thermic load put, cold screen temperature is observed, the flow velocity of liquid nitrogen is fixed when cold screen temperature stabilization, is passed through always in whole experiment process
Liquid nitrogen and constant airspeed, the nitrogen of volatilization are arranged to outdoor；
6. opening the check valve of fixed nitrogen container outlet, toward the interior filling liquid nitrogen of fixed nitrogen container, the process observes fixed nitrogen container always
Interior pressure, stop filling when liquid level is close to setting height, should during be located at the check valve of gas outlet outside denitrogen always
Gas；
7. opening GM refrigeration machines, room temperature helium is passed through into the coil pipe on GM refrigeration machines, will by the one-level cold head of GM refrigeration machines
Helium precooling, and then contacted with GM refrigeration machine two level cold heads and continue precooling until condensing, the liquid helium of condensation is in liquid helium vessel inner product
It is poly-, when the liquid helium in liquid helium vessel runs up to a certain amount of, stop being passed through room temperature helium into coil pipe.Simultaneously, liquid helium holds
In device, exchanged heat with the liquid nitrogen in fixed nitrogen container, with the progress of heat exchange, liquid nitrogen temperature gradually reduces, liquid nitrogen solidification, Gu
The temperature of nitrogen continues to decrease up to and stopped close to being exchanged heat during the temperature of liquid helium, and the process fixed nitrogen stores a large amount of colds；
8. the check valve that the gas outlet for opening liquid helium vessel is set, in order to prevent GM refrigeration machines from producing vibration in nano impress,
Now GM refrigeration machines are closed.The helium of volatilization is allowed to be arranged to indoor collection vessel simultaneously；
9. a large amount of colds of fixed nitrogen containers store are delivered into sample stage by the copper braid over braid on cold finger, sample stage is realized
Refrigeration, while adjust heater and can realize nano-indentation experiment under 4.2K-300K different temperatures；
10. starting to test, realize that mobile platform moves to both direction to Y-direction servo linear motor by X, pass through Z-direction electricity
Machine realizes that atomic force magnifying glass Z-direction moves, and observes sample, records the locus by control section, then remove atomic force
Microscope, by movable press head to the position；
11. depression bar is moved into Indentation position by mobile device, depth of cup is determined by setting depth of cup and time,
Pressure sensor measured pressure value；
12. when the measurement for completing a temperature spot and a location point, realized and become by the heater heating of sample stage bottom
Temperature, extent of alternating temperature are about 4.2K-300K, continue the measurement of other temperature values and sampling point；
13. the information such as the pressure, temperature, flow velocity of each several part are detected and shown always in control section in whole experiment process；
14. when the measurement for completing a sample, sample room is opened, sample is changed and continues 2-13 steps, carry out the survey of other samples
Amount.
Finally it should be noted that：Obviously, above-described embodiment is only intended to clearly illustrate the application example, and simultaneously
The non-restriction to embodiment.For those of ordinary skill in the field, can also do on the basis of the above description
Go out other various forms of changes or variation.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn
Among the obvious changes or variations that Shen goes out is still in the protection domain of the application type.
Claims (7)
1. a kind of nano impress device based on GM refrigeration machines, it is characterised in that including nano impress unit, thermal swing units, system
Cold unit, data acquisition unit and control unit, the refrigeration unit connect thermal swing units, and the thermal swing units connect nanometer pressure
Trace unit, the nano impress unit connect data acquisition unit, and described control unit connects the thermal swing units, nanometer respectively
Impression unit and data acquisition unit,
The refrigeration unit includes liquid nitrogen container, outer Dewar, cold screen, cold screen cooling tube, helium tank, GM refrigeration machines, GM refrigeration machine pressures
Contracting machine, refrigeration machine coil pipe, aseismatic mechanism, liquid helium vessel, condenser, liquid helium level meter, coil heat exchanger and fixed nitrogen container, it is described
GM refrigeration machines one end is connected with GM refrigerator compressors, and the other end is connected by condenser with liquid helium vessel, on the condenser
Refrigeration machine coil pipe is wound with, refrigeration machine coil pipe is connected with helium tank, and the liquid helium level meter is vertical to be arranged in liquid helium vessel,
The cold screen is connected by cold screen cooling tube with liquid nitrogen container, and liquid helium vessel and the fixed nitrogen container is installed in cold screen, described
Cold screen is arranged in outer Dewar, and the aseismatic mechanism is arranged on below the GM refrigeration machines and is connected with outer Dewar, liquid helium vessel
It is connected between fixed nitrogen container by coil heat exchanger, liquid nitrogen is input to solid by the liquid nitrogen container by fixed nitrogen container entrance pipeline
In nitrogen cascade, the coil heat exchanger is used to realizing liquid helium with the heat exchange of liquid nitrogen and by liquid nitrogen solidification until fixed nitrogen temperature is close to liquid
Helium temperature, the fixed nitrogen container are arranged under sample stage；
The thermal swing units include cold finger, copper braid over braid and heater, and the cold finger is arranged in fixed nitrogen container, the heater
Installed in sample stage bottom, the heater is woven by copper and is connected with cold finger；
The nano impress unit include vacuum (-tight) housing, sample stage, mobile device, pressure sensor, depression bar, nano impress probe and
AFM, the vacuum (-tight) housing provide an independent vacuum environment for nano impress, and the sample stage is used for placing reality
Sample is tested, the mobile device is arranged on above sample stage, and the mobile device is used for control pressure sensor, depression bar and atom
Force microscope moves in XYZ directions, and the pressure sensor is used for measuring depression bar stress, and the nano impress probe is arranged on pressure
Bar lower end, the atomic force microscope observation impression point position and Indentation Process；
The information of data acquisition unit collection include liquid helium liquid level and pressure in liquid helium vessel, the pressure in fixed nitrogen container,
The pressure that displacement, impression speed and the pressure sensor that sample stage temperature, heater power, mobile device are obtained are obtained；
Described control unit includes control computer, and the control computer is respectively used to show and controls liquid helium in liquid helium vessel
Liquid level and pressure, the pressure in fixed nitrogen container, the power of heater, sample stage temperature, the displacement of mobile device, impression speed and
Presser bar pressure.
A kind of 2. nano impress device based on GM refrigeration machines according to claim 1, it is characterised in that the sample room
On be provided with observation window, the observation window is used to observing and measuring sample Indentation position.
A kind of 3. nano impress device based on GM refrigeration machines according to claim 1, it is characterised in that the GM refrigeration
Machine is by the room temperature helium precooling in helium tank and is condensed into liquid helium, is transferred in liquid helium vessel, liquid helium by coil heat exchanger with
Liquid nitrogen carries out indirect heat exchange, and liquid nitrogen is cooled into the purpose that the larger fixed nitrogen of specific heat capacity reaches cold-storage.
A kind of 4. nano impress device based on GM refrigeration machines according to claim 1, it is characterised in that the mobile dress
Put including X to, Y-direction and Z-direction shift servo motor, X is used for adjusting mobile device X to displacement, Y-direction servomotor to servomotor
For adjusting mobile device Y-direction displacement, Z-direction servomotor is used for adjusting pressure sensor, depression bar and AFM to Z-direction
It is mobile.
5. a kind of nano impress device based on GM refrigeration machines according to claim 1, it is characterised in that the depression bar is
Invar.
6. a kind of nano impress device based on GM refrigeration machines according to claim 1, it is characterised in that the coil pipe changes
Hot device is length thin tube.
A kind of 7. nano impress device based on GM refrigeration machines according to claim 1, it is characterised in that the shockproof machine
Structure includes bellows and location structure, and shockproof bellows is made up of copper braid over braid.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108535129A (en) * | 2018-04-16 | 2018-09-14 | 吉林大学 | The micro-nano impression test system of low temperature that large journey low-temperature floats under micro- component |
| CN109613033A (en) * | 2019-02-25 | 2019-04-12 | 江苏集萃微纳自动化系统与装备技术研究所有限公司 | Nano impress heating device and corresponding nano-indenter test instrument |
| CN109712774A (en) * | 2018-11-20 | 2019-05-03 | 浙江大学 | A kind of superconducting magnet method for rapid cooling and its system |
| CN110319991A (en) * | 2019-07-04 | 2019-10-11 | 合肥中科离子医学技术装备有限公司 | Spring test device based on GM refrigeration machine |
| CN110470555A (en) * | 2019-08-26 | 2019-11-19 | 吉林大学 | The antivacuum atmosphere formula refrigeration system of the micro-nano impression test system of low temperature |
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| CN117346391A (en) * | 2023-12-04 | 2024-01-05 | 万气精仪(苏州)气体设备有限公司 | Condenser for GM refrigerator |
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