CN103901232A - Low-temperature scanning tunneling microscope using closed-cycle refrigerator to achieve refrigeration - Google Patents
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- CN103901232A CN103901232A CN201410091094.8A CN201410091094A CN103901232A CN 103901232 A CN103901232 A CN 103901232A CN 201410091094 A CN201410091094 A CN 201410091094A CN 103901232 A CN103901232 A CN 103901232A
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Abstract
The invention discloses a low-temperature scanning tunneling microscope using a closed-cycle refrigerator to achieve refrigeration. The low-temperature scanning tunneling microscope comprises a closed-cycle refrigerator system, a helium heat exchange gas refrigeration vibration isolation interface system, a low-temperature scanning tunneling microscope scanning head system, a vacuum system, a vibration reduction platform and a scanning tunnel microscope control system. According to the low-temperature scanning tunneling microscope, under the condition that no liquid helium is consumed, atomic-scale resolution low-temperature ultrahigh-vacuum scanning tunnel microscopy space imaging and high-energy resolution scanning tunnel spectrum accurate measurement can be achieved like a liquid helium refrigeration system. The technical scheme of closed-cycle refrigeration can also be used for other applications needing lower temperature and low-vibration environments like other members of scanning probe microscope families. Large-range temperature changes can also be achieved through feedback combination of heating elements and temperature measuring elements.
Description
Technical field
The invention belongs to scanning probe microscopy field, be specifically related to a kind of low-temperature scanning tunneling microscope of closed circuit refrigeration machine refrigeration without consumption liquid helium that utilize.
Technical background
Scanning tunnel microscope (Scanning Tunneling Microscope, STM) be scanning probe microscopy (Scanning Probe Microscope, SPM) Major Members in family, is invented in nineteen eighty-two by the people such as Binnig and Rohrer of Zurich, SUI IBM Corporation.Its principle of work has been utilized the electron tunneling effect in quantum mechanics.Specifically, when a sharp-pointed metal needle point infinite approach of atom level is detected sample surfaces, until while only having the distance of several or an atom, if apply a bias voltage between sample and metal needle point being detected, electrons tunnelling in needle point or sample is crossed vacuum barrier between the two, thereby forms tunnelling current.Because the size of tunnelling current is exponential decay with the distance between needle point and sample, metal needle point just can form at the scanning probe of sample surfaces the surface topography map that atom level is differentiated.Simultaneously, because tunnelling current also extremely depends on electronic state and the atomic structure of sample and needle point, variation by measuring tunnelling current in the bias voltage changing between needle point and sample surfaces also can analytic sample or local electronic state, molecular vibration state or the surface phonon state of needle point, the scanning tunnel spectrum (Scanning Tunneling Spectroscopy) that Here it is says conventionally.Therefore, scanning tunnel microscope is searching surface pattern and the powerful tool of studying electronics, atomic structure in Surface Science.
Because tunnelling current in scanning tunnel microscope reaches subatomic rank (generally right or following at 0.01 Izod) to the distance sensitive degree between needle point and sample, the running environment of scanning tunnel microscope often needs the conditions such as ultrahigh vacuum, low temperature or utmost point low temperature.Ultra-high vacuum environment is realize and keep laboratory sample and the clean of needle point to provide safeguard.And cryogenic conditions can make poor the greatly reducing of thermal drift between scanning tunnel microscope internal part, meet preferably the requirement that instrument atom level is accurate and stable; What is more important can effectively reduce the broadening being caused by the Electron Heat temperature in sample and needle point, impels laboratory sample to present novel interesting low temperature physics phenomenon.Therefore, advanced high-end scanning tunnel microscope often all operates in low temperature/utmost point low temperature and ultra-high vacuum environment.
At present, low-temperature scanning tunneling microscope is mostly positioned in Dewar thermostat or continuous stream thermostat, adopts liquid refrigerants to lower the temperature as the latent heat of phase change of liquid helium or liquid nitrogen carrys out refrigeration.The phase transition temperature of liquid nitrogen under an atmospheric pressure is 77 K, is not enough to meet the low temperature requirement of experimental study toward contact.And the 4.2K phase transition temperature of liquid helium can satisfy the demands preferably, but its global resources are rare, and price is extremely expensive.In recent years, non-renewable due to helium resource, liquid helium price climbs up and up especially.Therefore, some Cryo Equipments start to adopt the refrigeration machine without consuming liquid helium to lower the temperature as GM closed circuit refrigeration machine or vascular closed circuit refrigeration machine etc. carry out refrigeration one after another.But conventional closed circuit refrigeration facility have stronger mechanical vibration and noise.Also cannot simply adopt the cooling of closed circuit refrigeration machine to the instrument of vibration and noise sensitivity, scanning tunnel microscope just belongs to this class.Taking GM closed circuit refrigeration machine on market as example, place sample refrigeration head end vibration displacement generally 1 micron or more than.And in scanning tunnel microscope the range accuracy between needle point and sample surfaces to require to be controlled at 0.01 Izod right or following, in order to use in scanning tunnel microscope, closed circuit refrigeration machine refrigeration cooling is this has brought great challenge without the mode that uses liquid helium for this.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of low-temperature scanning tunneling microscope that utilizes the refrigeration of closed circuit refrigeration machine, it carries out refrigeration without consuming liquid helium, there is atomic resolution, solve the micron order left and right of closed circuit refrigeration machine or the problem of mechanical vibration above, thereby realized the scanning tunnel spectrum precision measurement of low temperature space imaging and high energy resolution.
A kind of low-temperature scanning tunneling microscope that utilizes the refrigeration of closed circuit refrigeration machine provided by the invention, comprising: comprise closed circuit refrigeration machine system, helium exchange gas refrigeration vibration isolation interface system, low-temperature scanning tunneling microscope scanner head system, vacuum system, vibration reduction platform and scanning tunnel microscope control system; Described vibration reduction platform passes the vibration of coming for isolating from ground; Described scanning tunnel microscope control system is for inserting needle, the measurement of gated sweep head.
Described helium heat interchange gas refrigeration vibration isolation interface system comprises the refrigeration vibration isolation interface being connected on ultrahigh vacuum cavity, soft rubber and helium heat-exchange gas; The refrigeration head of described closed circuit refrigeration machine system stretches in refrigeration vibration isolation interface, between refrigeration head and refrigeration vibration isolation interface, fills helium heat-exchange gas as refrigeration cool-down medium; Described soft rubber connects upper end and the refrigeration head at sealing refrigeration vibration isolation interface, when its sealing helium exchange gas, can isolate the vibration of refrigeration head; Described low-temperature scanning tunneling microscope scanner head system comprises scanner head, spring, temperature element, heating element, temperature control system and inside and outside heat radiation screening cover; Described scanner head hangs on by spring on the interior heat radiation screening cover being connected with the cold junction in refrigeration vibration isolation interface; Outer heat radiation screening covers on the outside of interior heat radiation screening cover, and outer heat radiation screening cover is also fixed on refrigeration vibration isolation interface.
In such scheme, helium heat interchange gas refrigeration vibration isolation interface system also comprises air release, ball valve, reduction valve and the high-pure helium gas pressure gas of controlling helium heat interchange gas air pressure.
In such scheme, low-temperature scanning tunneling microscope scanner head system also comprises electric signal cable and the thermometric heating cable of scanning tunnel microscope.
In such scheme, vacuum system comprises ultrahigh vacuum cavity, also comprises vacuum pump, the vacuum gauge etc. realizing and maintain vacuum.
In such scheme, scanning tunnel microscope control system comprises preposition micro current amplifier, Z feedback control circuit, piezoelectric ceramics high pressure transport and placing device, analog-digital conversion data collector etc.
In such scheme, the internal heat shield that temperature element and heating element are arranged on low-temperature scanning tunneling microscope scanner head system covers cover top; Temperature element, heating element and temperature control system are connected, and temperature control system is by the temperature of FEEDBACK CONTROL scanner head.
In such scheme, described refrigeration vibration isolation interface adopts stainless steel and oxygenless copper material to process, can be with to realize the needed heated baking condition of ultra-high vacuum environment compatible mutually.
The present invention has following beneficial effect:
1. the problem that the scheme of mechanical vibration more than micron order of effectively having isolated refrigeration machine in utilizing closed circuit refrigeration machine refrigeration cooling provided by the invention has solved traditional low-temperature scanning tunneling microscope and consumes in a large number reserves rareness, expensive liquid helium.This without consuming the scheme cooling-down effect of liquid helium and using liquid helium system suitable.
2. the scheme that realizes the low vibration of low temperature under the condition without liquid helium consumption provided by the invention not only can realize the scanning tunnel microscope that atom level is differentiated, also can need for other application of low temperature and low vibration environment, as other members of scanning probe microscopy family.
3. provided by the inventionly differentiate low-temperature scanning tunneling microscope in the atom level of utilizing the refrigeration of closed circuit refrigeration machine and not only can under low temperature environment, move, also can realize large-scale alternating temperature by the feedback composition of heating element and temperature element and measure.
4. the scheme that realizes the low vibration of low temperature under the condition without liquid helium consumption provided by the invention also can realize ultra-high vacuum environment, can be with to realize the condition that ultra-high vacuum environment needs heated baking compatible mutually.
Brief description of the drawings
Fig. 1 is that the atom level of utilizing the refrigeration of closed circuit refrigeration machine that the present invention proposes is differentiated the structural representation of low-temperature scanning tunneling microscope.
Fig. 2 is the assembly structural representation of closed circuit refrigeration mechanism cold head member in the preferred embodiment of the present invention, helium heat interchange gas refrigeration vibration isolation interface system and scanning tunnel microscope scanner head system.
Fig. 3 utilizes the preferred embodiment of the present invention at low temperature (20 K) and ultrahigh vacuum (6 × 10
-11torr) Au(110 surveying under condition) coronene (coronene) molecule of 2 × 1 reconstructing surfaces.
Number in the figure: 1-closed circuit refrigeration machine system; 2-helium heat interchange gas refrigeration vibration isolation interface system; 3-low-temperature scanning tunneling microscope scanner head system; 4-ultrahigh vacuum cavity; 5-vibration reduction platform; 6-scanning tunnel microscope control system; The 7-head that freezes; 8-bracing frame; 9-soft rubber; 10-refrigeration vibration isolation interface; 11-temperature element and heating element; 12-spring; 13-scanner head; Heat radiation screening cover in 14-; The outer heat radiation screening cover of 15-; 16-helium heat interchange gas; 17-vacuum pump; 18-helium compressor; 19-helium tube; 20-temperature control system; 21-high-pure helium gas pressure gas.
Embodiment
In order to make the object, technical solutions and advantages of the present invention more cheer and bright, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
Nearly all low-temperature scanning tunneling microscope all uses Dewar thermostat or the refrigeration of continuous stream thermostat based on liquid helium at present.This makes system operation need the liquid helium amount of consumption considerable, and operating cost is high.Obtain the low temperature comparable with liquid helium refrigeration system and do not use liquid helium, effective way is the cooling method that adopts closed circuit refrigeration machine.But closed circuit refrigeration facility have stronger mechanical vibration and noise, this has limited the application of closed circuit refrigeration machine in the low-temperature scanning tunneling microscope field of Atomic Resolution.
Figure 1 shows that the structural representation that utilizes the atom level of closed circuit refrigeration machine refrigeration to differentiate low-temperature scanning tunneling microscope system provided by the invention.It shown in Fig. 2, is the assembly structural representation of closed circuit refrigeration mechanism cold head member, helium heat interchange gas refrigeration vibration isolation interface system and scanning tunnel microscope scanner head system.
For closed circuit refrigeration machine is applied in the low-temperature scanning tunneling microscope of Atomic Resolution, apparatus of the present invention comprise: for obtaining the closed circuit refrigeration machine system 1 of low temperature; For the helium heat interchange gas refrigeration vibration isolation interface system 2 at refrigeration cooling while isolating vibration; Low-temperature scanning tunneling microscope scanner head system 3; Vacuum system; Vibration reduction platform 5 and scanning tunnel microscope control system 6; Wherein:
Closed circuit refrigeration machine system 1 comprises the bracing frame 8 of refrigeration 7, helium compressor 18, refrigeration 7 and helium tube 19, service cable, water cooling unit and fixing refrigeration 7.The type of closed circuit refrigeration machine comprises G-M circulating refrigerator, vascular refrigerator and the improvement refrigeration machine based on these principles.The refrigeration work consumption of closed circuit refrigeration machine and minimum temperature can be looked actual needs configuration.General minimum temperature can reach 4.2 K even below.
Helium heat interchange gas refrigeration vibration isolation interface system 2 comprises the refrigeration vibration isolation interface 10 that is arranged on ultrahigh vacuum cavity 4, connect refrigeration 7 and refrigeration vibration isolation interface 10 for sealing helium heat interchange gas 16 between soft rubber 9, refrigeration vibration isolation interface 10 and the refrigeration 7 of vibration isolation, control air release, ball valve, reduction valve and the high-pure helium gas pressure gas 21 of helium heat interchange gas 16 air pressure.
Helium heat interchange gas 16 in helium heat interchange gas refrigeration vibration isolation interface system 2 may have a certain amount of gas liquid to change into liquid helium according to the refrigerating capacity size of closed circuit refrigeration machine system 1.The generation of liquid helium does not affect the performance of isolation of system refrigeration machine vibration; With regard to refrigeration cooling, effect is better on the contrary.
The interior heat radiation screening cover 14 that low-temperature scanning tunneling microscope scanner head system 3 comprises scanner head 13, be fastenedly connected with refrigeration vibration isolation interface 10 and outer heat radiation screening cover 15, the spring 12 that hangs scanner head 13, electric signal cable, temperature element and heating element 11, temperature control system 20 and the cable of scanning tunnel microscope.Low-temperature scanning tunneling microscope scanner head 13 hangs on the interior heat radiation screening cover 14 contacting with the cold junction in refrigeration vibration isolation interface 10 by spring 12.Outer heat radiation screening cover 15 is in the outside of interior heat radiation screening cover 14, and outer heat radiation screening cover 15 is also fixed on refrigeration vibration isolation interface 10.Above internal heat shield covers cover 14, temperature element and heating element 11 are installed.Temperature element is connected with temperature control system 20 with heating element 11, and temperature control system 20 is by the temperature of FEEDBACK CONTROL scanner head 13.The operation such as inserting needle, scanning of scanning tunnel microscope control system 6 gated sweeps 13.
Vacuum system comprises ultrahigh vacuum cavity 4 and vacuum pump 20.
Adopt helium heat interchange gas 16 as the refrigeration cooling medium between scanner head 13 in refrigeration in closed circuit refrigeration machine system 17 and low-temperature scanning tunneling microscope scanner head system 3, the soft rubber 9 that is provided for being tightly connected between refrigeration vibration isolation interface 10 and refrigeration 7, has also effectively isolated the mechanical vibration more than micron order of refrigeration 7 when its sealing helium exchange gas 16.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect have been done to further detailed explanation; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; every within the present invention spirit and principle, any amendment of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (3)
1. a low-temperature scanning tunneling microscope that utilizes the refrigeration of closed circuit refrigeration machine, is characterized in that: it comprises closed circuit refrigeration machine system, helium exchange gas refrigeration vibration isolation interface system, low-temperature scanning tunneling microscope scanner head system, vacuum system, vibration reduction platform and scanning tunnel microscope control system; Described vibration reduction platform passes the vibration of coming for isolating from ground; Described scanning tunnel microscope control system is for inserting needle, the measurement of gated sweep head;
Described helium heat interchange gas refrigeration vibration isolation interface system comprises the refrigeration vibration isolation interface being connected on ultrahigh vacuum cavity, soft rubber and helium heat-exchange gas; The refrigeration head of described closed circuit refrigeration machine system stretches in refrigeration vibration isolation interface, between refrigeration head and refrigeration vibration isolation interface, fills helium heat-exchange gas as refrigeration cool-down medium; Described soft rubber connects upper end and the refrigeration head at sealing refrigeration vibration isolation interface, when its sealing helium exchange gas, can isolate the vibration of refrigeration head; Described low-temperature scanning tunneling microscope scanner head system comprises scanner head, spring, temperature element, heating element, temperature control system and inside and outside heat radiation screening cover; Described scanner head hangs on by spring on the interior heat radiation screening cover being connected with the cold junction in refrigeration vibration isolation interface; Outer heat radiation screening covers on the outside of interior heat radiation screening cover, and outer heat radiation screening cover is also fixed on refrigeration vibration isolation interface.
2. low-temperature scanning tunneling microscope according to claim 1, is characterized in that: the internal heat shield that described temperature element and heating element are arranged on low-temperature scanning tunneling microscope scanner head system covers cover top; Temperature element, heating element and temperature control system are connected, and temperature control system is by the temperature of FEEDBACK CONTROL scanner head.
3. according to the low-temperature scanning tunneling microscope described in right 1, it is characterized in that; Described refrigeration vibration isolation interface adopts stainless steel and oxygenless copper material to process.
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