CN206740554U - 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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- CN206740554U CN206740554U CN201720519950.4U CN201720519950U CN206740554U CN 206740554 U CN206740554 U CN 206740554U CN 201720519950 U CN201720519950 U CN 201720519950U CN 206740554 U CN206740554 U CN 206740554U
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Abstract
The utility model 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, the utility model 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
It the utility model is related to nano indentation test technical field, specifically a kind of nanometer pressure based on GM refrigeration machines
Trace device.
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.
Utility model content
The purpose of this utility model is 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
Influence of the vibration of GM refrigeration machines to test result.
What the purpose of this utility model was realized in：A kind of nano impress device based on GM refrigeration machines, including alternating temperature
Unit, refrigeration unit, nano impress unit, data acquisition unit and control unit, refrigeration unit connection thermal swing units, alternating temperature list
Member connection nano impress unit, nano impress unit connection data acquisition unit, control unit connect thermal swing units, nanometer respectively
Impression unit and data acquisition unit,
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, GM systems
Cold one end is connected with GM refrigerator compressors, and the other end is connected by condenser with liquid helium vessel, and system is wound with condenser
Cold 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 passes through cold screen
Cooling tube 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, shockproof machine
Structure is arranged on below GM refrigeration machines and is connected with outer Dewar, is connected between liquid helium vessel and fixed nitrogen container by coil heat exchanger,
GM refrigeration machines are by the room temperature helium precooling in helium tank and are condensed into liquid helium, are transferred in liquid helium vessel, liquid helium is changed by coil pipe
Hot device carries out indirect heat exchange with liquid nitrogen, by liquid solidification until fixed nitrogen temperature is arranged on sample stage close to liquid helium temperature, fixed nitrogen container
Under；
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
Sample platform bottom, heater are woven by copper and are connected with cold finger；
Nano impress unit include vacuum (-tight) housing, sample stage, mobile device, pressure sensor, depression bar, nano impress probe and
AFM, vacuum (-tight) housing provide an independent vacuum environment for nano impress, and sample stage is used for placing laboratory sample, moved
Dynamic device is arranged on above sample stage, and mobile device is used for control pressure sensor, depression bar and AFM in XYZ directions
Mobile, pressure sensor is used for measuring depression bar stress, and nano impress probe is arranged on depression bar lower end, atomic force microscope observation pressure
Trace 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；
Control unit includes control computer, and control computer is respectively used to show and controls liquid helium liquid level in liquid helium vessel
With pressure, the power of heater, sample stage temperature, the displacement of mobile device, impression speed and the depression bar in pressure, fixed nitrogen container
Pressure.
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 utility model has the advantage of：
1st, the utility model sample temperature temperature in the range of room temperature to liquid helium temperature is adjustable, and the rate of heat addition is adjustable, can be real
Existing refrigeration and alternating temperature of the sample in the range of 4.2K-300K；
2nd, the utility model is used as cooling medium using liquid nitrogen and helium, uses GM refrigeration machines by helium liquefaction for liquid helium,
Liquid helium is directly provided without extraneous, 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 it is accurate become control temp, displacement load signal Precision measurement,
Microcosmic accurate 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 utility model；
Fig. 2 is a kind of front view of the mobile device of the nano impress device based on GM refrigeration machines of the utility model；
Fig. 3 is a kind of structural representation of the nano impress device based on GM refrigeration machines of the utility model；
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 freezes
Machine；12- aseismatic mechanisms;13- refrigeration machine coil pipes；14- liquid helium vessels;15- condensers；16- liquid helium level meters;17- helium goes out
Mouthful;18- coil heat exchangers;19- fixed nitrogen containers;20- cold fingers;21- copper braid over braids；22- heaters；23- sample stages；24- samples
Product;25- vacuum (-tight) housings；26-X is to servomotor；27-Y is to servomotor；28-Z is to servomotor；29- pressure sensors;30-
AFM;31- depression bars；32- nano impress is popped one's head in;33- data acquisition units；34- control units.
Embodiment
The utility model is further described below in conjunction with the accompanying drawings.
The utility model is a kind of nano impress device based on GM refrigeration machines, including refrigeration unit, thermal swing units, nanometer
Impression unit, data acquisition unit and control unit, refrigeration unit connection thermal swing units, thermal swing units connection nano impress list
Member, nano impress unit connection data acquisition unit, control unit connect nano impress unit, refrigeration unit, alternating temperature list respectively
Member, nano impress 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, and control computer is respectively used to show and controls liquid helium liquid in liquid helium vessel
Position and pressure, the pressure in fixed nitrogen container, the power of heater, sample stage temperature, the displacement of mobile device, impression speed and pressure
The information such as rod pressure
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
Motor realizes that magnifying glass Z-direction moves, and carries out preliminary observation close to sample, the locus, Ran Houyi are recorded by control section
Microscope is driven, 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
Vacuum 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 is surrounded with reducing cold screen
The thermic load of device, cold screen temperature is observed, the flow velocity of liquid nitrogen is fixed when cold screen temperature stabilization, one is straight-through in whole experiment process
Enter liquid nitrogen and constant airspeed, the nitrogen of volatilization is 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 always
Pressure in container, stop filling when liquid level is close to setting height, the check valve that gas outlet is located at during being somebody's turn to do is outside always
Denitrogen gas；
7. opening GM refrigeration machines, room temperature helium is passed through into the coil pipe on GM refrigeration machines, the one-level by GM refrigeration machines is cold
Helium precooling is contacted and continues precooling until condensing by head with GM refrigeration machine two level cold heads, and the liquid helium of condensation is in liquid helium vessel
Interior accumulation, 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
In helium vessel, exchanged heat with the liquid nitrogen in fixed nitrogen container, with the progress of heat exchange, liquid nitrogen temperature gradually reduces, and liquid nitrogen coagulates
Gu the temperature of fixed nitrogen continues to decrease up to and stopped close to being exchanged heat during the temperature of liquid helium, 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 produce in nano impress from shaking
It is dynamic, 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 is realized
The refrigeration of platform, 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
Realize that atomic force magnifying glass Z-direction moves to motor, observe sample, the locus is recorded by control section, then removes original
Sub- force microscope, by movable press head to the position；
11. depression bar is moved into Indentation position by mobile device, the depth of cup is determined by setting depth of cup and time
Degree, pressure sensor measured pressure value；
12. when the measurement for completing a temperature spot and a location point, heated and realized by the heater of sample stage bottom
Alternating 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 other samples
Measurement.
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720519950.4U CN206740554U (en) | 2017-05-11 | 2017-05-11 | A kind of nano impress device based on GM refrigeration machines |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720519950.4U CN206740554U (en) | 2017-05-11 | 2017-05-11 | A kind of nano impress device based on GM refrigeration machines |
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| CN206740554U true CN206740554U (en) | 2017-12-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201720519950.4U Expired - Fee Related CN206740554U (en) | 2017-05-11 | 2017-05-11 | A kind of nano impress device based on GM refrigeration machines |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107421825A (en) * | 2017-05-11 | 2017-12-01 | 兰州大学 | A kind of nano impress device based on GM refrigeration machines |
| CN109030232A (en) * | 2018-08-14 | 2018-12-18 | 兰州大学 | Neutron scattering cryogenic tensile Dewar |
| CN110531802A (en) * | 2019-05-29 | 2019-12-03 | 长春因赛图精密仪器设备有限公司 | A kind of continuous changing device and its control method for nano-hardness tester |
-
2017
- 2017-05-11 CN CN201720519950.4U patent/CN206740554U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107421825A (en) * | 2017-05-11 | 2017-12-01 | 兰州大学 | A kind of nano impress device based on GM refrigeration machines |
| CN109030232A (en) * | 2018-08-14 | 2018-12-18 | 兰州大学 | Neutron scattering cryogenic tensile Dewar |
| CN110531802A (en) * | 2019-05-29 | 2019-12-03 | 长春因赛图精密仪器设备有限公司 | A kind of continuous changing device and its control method for nano-hardness tester |
| CN110531802B (en) * | 2019-05-29 | 2024-03-15 | 长春因赛图精密仪器设备有限公司 | Continuous temperature changing device for nanometer indentation instrument and control method thereof |
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