CN206002561U - A kind of Pt Ir needle point corrosion device - Google Patents
A kind of Pt Ir needle point corrosion device Download PDFInfo
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- CN206002561U CN206002561U CN201620799645.0U CN201620799645U CN206002561U CN 206002561 U CN206002561 U CN 206002561U CN 201620799645 U CN201620799645 U CN 201620799645U CN 206002561 U CN206002561 U CN 206002561U
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Abstract
The utility model discloses a kind of Pt Ir needle point corrosion device, including mechanical component, operating circuit and automatic circuit control system；Described automatic circuit control system includes AC signal and occurs module, ac voltage signal collection and amplification module, ac voltage signal virtual value to extract and display circuit, ac current signal acquisition module, ac current signal absolute value processing circuit, AC-DC conversion and display circuit, threshold value setting module, sampled signal comparison circuit module, signal processing power module and power switch unit.This utility model is loaded with ac current signal absolute value processing circuit in automatic circuit control system, ac current signal is converted into the d. c. voltage signal that can directly observe, it is compared by sampled signal comparison circuit module with preset value, determines the action of power switch unit.During making Pt Ir needle point according to method of the present utility model, never found the Pt Ir tinsel rupturing in beaker bottom.
Description
Technical field
This utility model is related to the manufacturing technology of PSTM, particularly a kind of Pt- of PSTM
The producing device of Ir (platinoiridita) needle point.
Background technology
PSTM is a kind of high Surface Science research meanses of resolution.It is scanned into as to sample surfaces
The direct part of picture, needle point plays important role in PSTM work process, and strong influence
The quality of imaging and the stability of operation.
Because the d electronic state of sophisticated atomic is obtained in that higher lateral resolution, W (tungsten) and Pt-Ir (platinoiridita) are mesh
Front two kinds of the most frequently used tip point material.Comparatively speaking, W needle point is easier to be corroded so typically using under vacuum conditions, and
Pt and Ir is noble metal and is difficult oxidized, chemical property is more stable, can be used under atmospheric environment, in addition Pt is softer,
Adding Ir can increase hardness, so that it is difficult damaged.
Both materials, W is harder and crisp, generally uses unidirectional current (DC) caustic solution and is processed.Pt-Ir is softer,
Both can also be made of alternating current (AC) caustic solution using cutting method, specifically be used which kind of method, depending on general
Environment to be applied.For example, due to the release of stress, the needle point profile of shearing is coarse, typically can form the small of multiple projections
Tip, is used for the scanning of flat surfaces, and the needle surface more rule that chemical corrosion method makes can be used for rougher
Surface scan.
The research in presently relevant field is concentrated mainly on circuit exploitation, corrosion device improves and response parameter is for corrosion
Three aspects of the impact of effect.In order to obtain more sharp needle point, most design needs the auxiliary of automatic control circuit.
Chinese patent CN 201410836854.3 discloses a kind of needle tip of scanning tunnel microscope corrosion tester, this corrosion tester
Including mechanical component, operating circuit and control power supply.Power supply is controlled to include control circuit and control panel.Control circuit includes adjusting
Pressure Voltage stabilizing module, voltage measurement module, current measurement module, threshold value setting module, sampling comparison module and voltage output module,
Sampling resistor R2 used by voltage-regulation voltage-stabilization module is located at high potential, and sampling comparison module adopts LM319 type comparator.Due to this corruption
Control circuit designed by erosion instrument is by the sampling resistor in conventional needle point corrosion tester control circuit from whole load voltage acquisition system
In remove, change at high potential, can be with accurate measurement real-time current by such mode, proof load resistance two ends simultaneously
Constant voltage exports, and electric current is gradually reduced with the increase of load resistance, and the change of such Radix Salviae Miltiorrhizae amount is to be easily controlled and analyze
, enhance the stability of corrosion process, thus improve the success rate of needle point making.
But, there is a certain partial reaction and comparatively fast cause wire breakage in this corrosion tester in corrosion process, therefore only
W needle point can be made using DC corrosion method it is impossible to the corrosion for Pt-Ir needle point makes.
Utility model content
For solving the problems referred to above that prior art exists, this utility model will design one kind and not result in corrosion process
A certain partial reaction comparatively fast causes the Pt-Ir needle point corrosion device of wire breakage.
To achieve these goals, the technical solution of the utility model is as follows：A kind of Pt-Ir needle point corrosion device, including
Mechanical component, operating circuit and automatic circuit control system；
Described mechanical component includes base, support, Shang Gai, top cover knob, copper sheathing A, threaded rod, pointer, lifting fixation
Block, anode electrode bar, fixed knob, electrode fixing end, three-jaw fixture A, knob, three-jaw fixture B, cathode electrode bar, disk, stone
Electrode ink ring, beaker and copper sheathing B.
Described base is fixed using mode connects for screw with support, disk respectively, plays overall supporting role；Described upper lid with
Support is fixed using mode connects for screw；Described threaded rod two ends are coordinated with copper sheathing A and copper sheathing B gap respectively, and copper sheathing A and copper sheathing B divides
It is not fixed on lid and bottom seat；Described top cover knob is marked with scale, is fastenedly connected with threaded rod using screw；Described pointer
It is fixed by screws in and covers, the scale on its cooperation top cover knob determines the anglec of rotation of top cover knob.Described electrode is solid
Fixed end is fixed by screws on lifting fixed block, coordinates for screw thread, anode electrode bar between fixed knob and electrode fixing end
It is fixed in electrode fixing end by fixed knob；Described three-jaw fixture A and three-jaw fixture B is fixed by screws in anode respectively
On electrode stem, three-jaw fixture A and three-jaw fixture B is by tungsten filament vertical clamping；Described cathode electrode bar is fixed on base using screw
On, knob is coordinated with cathode electrode bar screw thread, and electrode retaining collar is fixedly clamped on cathode electrode bar rotary knob；Described disk is adopted
Be screwed on base, the beaker filling etchant solution is placed among the circular hole of disk, electrode retaining collar submerge beaker contained molten
Below liquid liquid level；Described etchant solution is CaCl2, the mixed solution of HCl and acetone；Set between described beaker and disk
Put vibration damper plate；
Described operating circuit includes anode electrode bar, electrode fixing end, three-jaw fixture A, knob, three-jaw fixture B, negative electrode
Etchant solution in electrode stem, disk, graphite electrode ring and beaker；Electrode fixing end connects positive source by electric wire, and electric current leads to
Cross the anode electrode bar being connected with electrode fixing end and be transmitted to the Pt-Ir silk clamped by three-jaw fixture A and three-jaw fixture B；Described
Cathode electrode bar connects power cathode, and is connected by screw with graphite electrode ring；Clamped by three-jaw fixture A and three-jaw fixture B
Pt-Ir silk and graphite electrode ring are co-located in the etchant solution that beaker is contained, but Pt-Ir silk is not directly connect with graphite electrode ring
Touch, during energising, Pt-Ir silk occurs cell reaction to constitute circuit loop in etchant solution.
Described automatic circuit control system includes AC signal and module, ac voltage signal collection occurs and amplifies mould
At block, the extraction of ac voltage signal virtual value and display circuit, ac current signal acquisition module, ac current signal absolute value
Reason circuit, AC-DC conversion and display circuit, threshold value setting module, sampled signal comparison circuit module, signal processing power supply mould
Block and power switch unit, described AC signal occurs module to be connected with ac voltage signal collection and amplification module, described
Ac voltage signal collection and amplification module respectively with ac voltage signal virtual value extract and display circuit, alternating current letter
Number acquisition module and anode electrode bar connect, described ac current signal acquisition module successively with ac current signal absolute value
Process circuit, AC-DC conversion and display circuit and sampled signal comparison circuit module connect, and described sampled signal is more electric
Road module is connected with threshold value setting module and power switch unit respectively, described power switch unit and cathode electrode bar and stone
Electrode ink ring connects.
Further, described damping plate thickness is 20-30mm.
Compared with prior art, this utility model has the advantages that：
1st, for the ease of monitoring, this utility model is loaded with ac current signal absolute value in automatic circuit control system
Reason circuit (similar to the part of commutator), ac current signal is converted into the d. c. voltage signal that can directly observe, adopts
It is compared by sample signal comparator circuit module with preset value, determines the action of power switch unit.
2nd, traditional automatic circuit control system is general all to be switched come control circuit with relay, and shortcoming is automatic reaction
Speed is slow, and this utility model adopts very sensitive electrical switch, i.e. power switch unit, and its function is about as much as one
Bi-directional MOS pipe in parallel, response speed, in 100ns magnitude, can control the two-way break-make of alternating current simultaneously.
3rd, during making Pt-Ir needle point according to method of the present utility model, never found fracture in beaker bottom
Pt-Ir tinsel (even if the Pt-Ir filament length of immersion solution reaches 1.5mm, also not finding phenomenon of rupture), meanwhile, alternating current is rotten
Etching method corrosion Pt-Ir silk is actually much the same in the response speed along major axis (X-axis) direction each several part, will not be as W pin
Equally there is a certain partial reaction and comparatively fast cause wire breakage in sharp corrosion process, but because top has sharp part,
Electric field intensity is stronger, and corrosion efficiency is very fast (along Y-axis), defines satisfactory tip.And As time goes on, immersion is molten
Length in liquid is gradually shortened, and eventually disengages from liquid level, and reaction stops.
Brief description
Fig. 1 is mechanical component structural representation of the present utility model.
Fig. 2 is automatic circuit control system composition schematic diagram of the present utility model.
Fig. 3 is workflow schematic diagram of the present utility model.
Fig. 4 is the needle point effect diagram that this utility model makes.
In figure：1st, base；2nd, support；3rd, Shang Gai；4th, top cover knob；5th, copper sheathing A；6th, threaded rod；7th, pointer；8th, lift admittedly
Determine block；9th, anode electrode bar；10th, fixed knob；11st, electrode fixing end；12nd, three-jaw fixture A；13rd, knob；14th, three-jaw fixture
B；15th, cathode electrode bar；16th, disk；17th, graphite electrode ring；18th, beaker；19th, copper sheathing B.
Specific embodiment
Below in conjunction with the accompanying drawings this utility model is further described through.As Figure 1-3, a kind of Pt-Ir needle point is rotten
Erosion device, including mechanical component, operating circuit and automatic circuit control system；
Described mechanical component include base 1, support 2, upper lid 3, top cover knob 134, copper sheathing A5, threaded rod 6, pointer 7,
Lifting fixed block 8, anode electrode bar 9, fixed knob 10, electrode fixing end 11, three-jaw fixture A12, knob 13, three-jaw fixture
B14, cathode electrode bar 15, disk 16, graphite electrode ring 17, beaker 18 and copper sheathing B19.
Described base 1 is fixed using mode connects for screw with support 2, disk 16 respectively, plays overall supporting role；On described
Lid 3 is fixed using mode connects for screw with support 2；Described threaded rod 6 two ends are coordinated with copper sheathing A5 and copper sheathing B19 gap respectively, copper sheathing
A5 and copper sheathing B19 is separately fixed on lid 3 and base 1；Described top cover knob 134 is marked with scale, using screw and screw thread
Bar 6 is fastenedly connected；Described pointer 7 is fixed by screws on lid 3, and the scale on its cooperation top cover knob 134 determines top cover
The anglec of rotation of knob 134.Described electrode fixing end 11 is fixed by screws on lifting fixed block 8, fixed knob 10 and electricity
Coordinate for screw thread between pole fixing end 11, anode electrode bar 9 is fixed in electrode fixing end 11 by fixed knob 10；Described three
Pawl fixture A12 and three-jaw fixture B14 is fixed by screws on anode electrode bar 9 respectively, three-jaw fixture A12 and three-jaw fixture
B14 is by tungsten filament vertical clamping；Described cathode electrode bar 15 is fixed on base 1 using screw, knob 13 and cathode electrode bar 15
Screw thread coordinates, and electrode retaining collar is fixedly clamped on cathode electrode bar 15 rotary knob 13；Described disk 16 is fixed on using screw
On base 1, the beaker 18 filling etchant solution is placed among the circular hole of disk 16, and electrode retaining collar submerges the contained liquid level of solution of beaker 18
Below；Described etchant solution is CaCl2, the mixed solution of HCl and acetone；Arrange between described beaker 18 and disk 16
Vibration damper plate；
Described operating circuit includes anode electrode bar 9, electrode fixing end 11, three-jaw fixture A12, knob 13, three-jaw card
Etchant solution in tool B14, cathode electrode bar 15, disk 16, graphite electrode ring 17 and beaker 18；Electrode fixing end 11 passes through electricity
Line connects positive source, and electric current is transmitted to three-jaw fixture A12 and three-jaw card by the anode electrode bar 9 being connected with electrode fixing end 11
Pt-Ir silk clamped by tool B14；Described cathode electrode bar 15 connects power cathode, and is connected by screw with graphite electrode ring 17；
Pt-Ir silk clamped by three-jaw fixture A12 and three-jaw fixture B14 and graphite electrode ring 17 are co-located on the corrosion that beaker 18 is contained
In solution, but Pt-Ir silk is not directly contacted with graphite electrode ring 17, and during energising, Pt-Ir silk occurs electrolysis anti-in etchant solution
Circuit loop should be constituted.
Described automatic circuit control system includes AC signal and module, ac voltage signal collection occurs and amplifies mould
At block, the extraction of ac voltage signal virtual value and display circuit, ac current signal acquisition module, ac current signal absolute value
Reason circuit, AC-DC conversion and display circuit, threshold value setting module, sampled signal comparison circuit module, signal processing power supply mould
Block and power switch unit, described AC signal occurs module to be connected with ac voltage signal collection and amplification module, described
Ac voltage signal collection and amplification module respectively with ac voltage signal virtual value extract and display circuit, alternating current letter
Number acquisition module and anode electrode bar 9 connect, and described ac current signal acquisition module is absolute with ac current signal successively
Value process circuit, AC-DC conversion and display circuit and sampled signal comparison circuit module connect, and described sampled signal compares
Circuit module is connected with threshold value setting module and power switch unit respectively, described power switch unit and cathode electrode bar 15
Connect with graphite electrode ring 17.
Further, described damping plate thickness is 20-30mm.
Method of work of the present utility model, comprises the following steps：
A, by the collection of the ac voltage signal of automatic circuit control system and amplification module and power switch unit respectively with
Anode electrode bar 9 and cathode electrode bar 15 connect, and beaker 18 is filled etchant solution and is positioned on the vibration damper plate of disk 16, and
The depth that Pt-Ir silk immerses etchant solution is adjusted by top cover knob 134；
B, AC signal occur module produce one group of AC signal, AC signal is continuous or pulsed, frequency and
Adjustable amplitude, reloads anode electrode bar 9 and cathode electrode bar after amplifying through ac voltage signal collection and amplification module
Between 15；Meanwhile, ac voltage signal virtual value is extracted and display circuit carries out virtual value extraction to the voltage signal after amplifying
And show, the AC signal voltage effective value that ac voltage signal collection and amplification module are exported is obtained by show value；
C, ac current signal absolute value processing circuit gather the exchange after amplification module amplifies to through ac voltage signal
After signal is acquired and makees absolute value process, it is transported to AC-DC conversion and display circuit；AC-DC conversion and display circuit
On the one hand AC signal is converted to and after direct current, passes through sampled signal comparison circuit module and the threshold set by threshold value setting module
Value is compared, and passes through to control power switch unit after comparing again；Another aspect display AC electric signal absolute value processes electricity
Size of current after the process of road is to judge to Pt-Ir silk needle point corrosion process；
D, it is compared by the threshold value set by sampled signal comparison circuit module and threshold value setting module, work as alternating current
When electric current after stream signal absolute value processing circuit process reaches the current value of threshold value setting module setting, corrosion terminates.
With reference to Fig. 4, corrosive effect of the present utility model is further described：In the corrosion process of W needle point,
Reaction efficiency highest region can break to form needle point in this place close to solution surface, therefore W silk, and the needle point profile being formed is
Hyperbolic type, drops in the electrolytic solution in the latter half after fracture.Also really it is found that much tiny in experiment in beaker bottom
W silk.But, in the manufacturing process of Pt-Ir silk, never found the Pt-Ir silk rupturing (even if immersion is molten in beaker bottom
The Pt-Ir filament length of liquid reaches 1.5mm, does not also find phenomenon of rupture), the image in Fig. 4 lower left corner is W silk and the corrosion of Pt-Ir silk respectively
Shape contrast afterwards.
The shape in needle point after the corrosion to 70 minute 7 time period in 10 minutes for the Pt-Ir silk is listed on the right side of Fig. 4,
These needle point images show, corrode Pt-Ir silk using alternating current method real in the response speed along major axis (X-axis) direction each several part
It is much the same on border, will not there is a certain partial reaction as W needle point corrosion process and comparatively fast cause wire breakage, but
Because top has sharp part, electric field intensity is stronger, and corrosion efficiency is very fast (along Y-axis), defines the tip of needs.And with
The passage of time, the length in immersion solution is gradually shortened, and eventually disengages from liquid level, and reaction stops, the needle point of formation is most advanced and sophisticated outer
Sigmoid curves is parabolic type.In current experiment, Pt-Ir silk top is the strongest due to electric field, and corrosion is the fastest, removes sharp first
Top becomes round and smooth arc, and simultaneously with the prolongation in response time, the wire length in solution also gradually shortens, more gradually
Needle point required for being formed is most advanced and sophisticated.
When Pt-Ir silk initially immerse length be 0.5mm when, by threshold value setting module sets end kinetic current as
40mA.This numerical value is by repeatedly testing obtaining it is ensured that obtaining the most advanced and sophisticated shape of preferable needle point with this understanding.
If the cut-off kinetic current of automatic shutdown circuit larger it is possible to lead to needle point tip not formed, 30 minutes in such as Fig. 4
Situation, cut-off current setting is slightly smaller, and shape impact that may be most advanced and sophisticated on needle point is not too large, but corrosion process is just
The extremely long time can be consumed, be also lose more than gain.
This utility model is not limited to the present embodiment, the equivalent concepts in any technical scope in this utility model disclosure
Or change, be all classified as protection domain of the present utility model.
Claims (2)
1. a kind of Pt-Ir needle point corrosion device, including mechanical component, operating circuit and automatic circuit control system；
Described mechanical component includes base (1), support (2), upper lid (3), top cover knob (13) (4), copper sheathing A (5), threaded rod
(6), pointer (7), lifting fixed block (8), anode electrode bar (9), fixed knob (10), electrode fixing end (11), three-jaw fixture A
(12), knob (13), three-jaw fixture B (14), cathode electrode bar (15), disk (16), graphite electrode ring (17), beaker (18) and
Copper sheathing B (19)；
Described base (1) is fixed using mode connects for screw with support (2), disk (16) respectively, plays overall supporting role；Described
Upper lid (3) and support (2) are fixed using mode connects for screw；Described threaded rod (6) two ends are respectively and between copper sheathing A (5) and copper sheathing B (19)
Gap coordinates, and copper sheathing A (5) and copper sheathing B (19) is separately fixed on lid (3) and base (1)；On described top cover knob (13) (4)
Indicate scale, be fastenedly connected with threaded rod (6) using screw；Described pointer (7) is fixed by screws on lid (3), and it is joined
Close the anglec of rotation that the scale on top cover knob (13) (4) determines top cover knob (13) (4)；Described electrode fixing end (11) is passed through
Screw is fixed in lifting fixed block (8), coordinates for screw thread, anode electrode between fixed knob (10) and electrode fixing end (11)
Bar (9) is fixed in electrode fixing end (11) by fixed knob (10)；Described three-jaw fixture A (12) and three-jaw fixture B (14)
It is fixed by screws in respectively on anode electrode bar (9), three-jaw fixture A (12) and three-jaw fixture B (14) are by tungsten filament vertical clamping；
Described cathode electrode bar (15) is fixed on base (1) using screw, and knob (13) is coordinated with cathode electrode bar (15) screw thread, rotation
Rotate button (13) electrode retaining collar is fixedly clamped on cathode electrode bar (15)；Described disk (16) is fixed on base using screw
(1) on, the beaker (18) filling etchant solution is placed among the circular hole of disk (16), and electrode retaining collar submerges the contained solution of beaker (18)
Below liquid level；Described etchant solution is CaCl2, the mixed solution of HCl and acetone；Described beaker (18) and disk (16)
Between arrange vibration damper plate；
Described operating circuit include anode electrode bar (9), electrode fixing end (11), three-jaw fixture A (12), knob (13), three
Etchant solution in pawl fixture B (14), cathode electrode bar (15), disk (16), graphite electrode ring (17) and beaker (18)；Electrode
Fixing end (11) connects positive source by electric wire, and electric current is by anode electrode bar (9) conduction being connected with electrode fixing end (11)
To the Pt-Ir silk clamped by three-jaw fixture A (12) and three-jaw fixture B (14)；Described cathode electrode bar (15) connects power cathode, and
It is connected by screw with graphite electrode ring (17)；Pt-Ir silk clamped by three-jaw fixture A (12) and three-jaw fixture B (14) and stone
Electrode ink ring (17) is co-located in the etchant solution that beaker (18) is contained, but Pt-Ir silk is not direct with graphite electrode ring (17)
Contact, during energising, Pt-Ir silk occurs cell reaction to constitute circuit loop in etchant solution；
It is characterized in that：
Described automatic circuit control system includes AC signal and module, ac voltage signal collection and amplification module, friendship occurs
Stream voltage signal virtual value is extracted and display circuit, ac current signal acquisition module, ac current signal absolute value process electricity
Road, AC-DC conversion and display circuit, threshold value setting module, sampled signal comparison circuit module, signal processing power module and
Power switch unit, described AC signal occurs that module is gathered with ac voltage signal and amplification module is connected, described friendship
Stream voltage signal acquisition and amplification module are adopted with the extraction of ac voltage signal virtual value and display circuit, ac current signal respectively
Collection module and anode electrode bar (9) connect, described ac current signal acquisition module successively with ac current signal absolute value
Process circuit, AC-DC conversion and display circuit and sampled signal comparison circuit module connect, and described sampled signal is more electric
Road module is connected with threshold value setting module and power switch unit respectively, described power switch unit and cathode electrode bar (15)
Connect with graphite electrode ring (17).
2. a kind of Pt-Ir needle point corrosion device according to claim 1 it is characterised in that：Described damping plate thickness is
20-30mm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620799645.0U CN206002561U (en) | 2016-07-27 | 2016-07-27 | A kind of Pt Ir needle point corrosion device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620799645.0U CN206002561U (en) | 2016-07-27 | 2016-07-27 | A kind of Pt Ir needle point corrosion device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093473A (en) * | 2016-07-27 | 2016-11-09 | 大连交通大学 | A kind of Pt Ir needle point corrosion device and method of work thereof |
| CN108196093A (en) * | 2017-12-26 | 2018-06-22 | 北京阳光凯特科技有限公司 | A kind of auxiliary device of preparation for metallic nano detecting probe |
-
2016
- 2016-07-27 CN CN201620799645.0U patent/CN206002561U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093473A (en) * | 2016-07-27 | 2016-11-09 | 大连交通大学 | A kind of Pt Ir needle point corrosion device and method of work thereof |
| CN108196093A (en) * | 2017-12-26 | 2018-06-22 | 北京阳光凯特科技有限公司 | A kind of auxiliary device of preparation for metallic nano detecting probe |
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| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170308 Termination date: 20190727 |