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CN104131330B - needle electrode and preparation method thereof - Google Patents

needle electrode and preparation method thereof Download PDF

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Publication number
CN104131330B
CN104131330B CN201410379919.6A CN201410379919A CN104131330B CN 104131330 B CN104131330 B CN 104131330B CN 201410379919 A CN201410379919 A CN 201410379919A CN 104131330 B CN104131330 B CN 104131330B
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rod
corrosion
electrode
conductor
bucket
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CN104131330A (en
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王钊
罗乐
李传锋
黄运锋
曹冬阳
郭光灿
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University of Science and Technology of China USTC
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Abstract

The present invention relates to a kind of method preparing needle electrode, said method comprising the steps of: a. puts into aqueous slkali as electrolyte in electrolytic vessel, place two corrosion-resistant buckets of the conductor varied in size the most with one heart, negative electrode is set outside the corrosion-resistant bucket of big conductor;B. W rod is placed in described electrolyte as anode so that W rod and liquid level are perpendicular to and at the center of the corrosion-resistant bucket of conductor, the diameter of electrolytic etching to the most required needle electrode;The insulative pipe sleeve of the diameter that c. internal diameter is slightly larger than required needle electrode forms the position of needle point in W rod lower end to expection, and lifting W is excellent but still keeps the position forming needle point to be still immersed in described electrolyte;D. electrolytic etching W rod is continued until W rod ruptures.

Description

Needle electrode and preparation method thereof
Technical field
Technical field: the invention belongs to quantum information technology field, is specifically related to a kind of needle electrode Preparation, it is adaptable to the applications such as the quantum information of ion trap systems, quantum calculation.
Background technology
Ion trap is as one of the system of quantum information and quantum calculation, because being in ultra-high vacuum environment, Make that ion degree of being environmentally isolated with is good, the decoherence time is long, and recognized because its extensibility is good For being the system having most practical prospect.Ion trap application rf electric field carrys out bound atom, applies laser pair Bound ion manipulates, and applies the collection optics such as PMT, CCD to carry out the receipts of optical signal Collection.Wherein ion trap electrodes is device the most direct with atomic interaction, penetrating used by bound atom Frequently electric field is applied on ion by this needle electrode.
The needle electrode manufacture method before applied is mainly machining: made with grinding by machine cut Obtain electrode and gradually become most advanced and sophisticated by oval rod shape.But its method is complicated, cycle length, precision be the highest, Cost is high and makes making electrode very inconvenient.
The second is to make probe electrode in the corrosion of STM field Applied Electrochemistry.But its requirement Tip diameter change is very violent, and is not applied for ion trap.And because the electronics system of its complexity System so that apparatus for preparation prepares complexity.
Summary of the invention
A kind of preparation method carrying out ion trap needle electrode of our main inventive, employing can be easily obtained Equipment and simple step, prepare the needle electrode being applicable to ion trap.Electrode is gradient-thickness And smooth surface, rather than STM probe is the same, diameter change is acutely.
One aspect of the present invention relates to a kind of method preparing needle electrode, and described method includes following Step:
A. in electrolytic vessel, put into aqueous slkali as electrolyte, place two the most with one heart simultaneously The individual corrosion-resistant bucket of the conductor varied in size, arranges negative electrode outside the corrosion-resistant bucket of big conductor;
B. W rod is placed to described electrolyte as anode so that W rod also position vertical with liquid level In the center of the corrosion-resistant bucket of conductor, the diameter of electrolytic etching to required needle electrode;
C. internal diameter is slightly larger than the insulative pipe sleeve of diameter of required needle electrode in W rod lower end extremely Expection forms the position of needle point, promotes W rod but still keeps the position forming needle point to be still immersed in described In electrolyte;
D. electrolytic etching W rod is continued until W rod ruptures.
In one embodiment of the invention, the corrosion-resistant bucket of conductor is stainless steel cask.
In one embodiment of the invention, insulation tube is plastic tube.
In one embodiment of the invention, the described corrosion-resistant bucket of big conductor is higher than liquid level of solution;With / or a diameter of 5mm to 10mm of the corrosion-resistant bucket of little conductor, preferably 1mm to 10mm, further preferably 5mm to 9mm, most preferably 8mm.
In one embodiment of the invention, the height of the corrosion-resistant bucket of little conductor is 6mm to 12mm, Preferably 5mm to 15mm, further preferably 10mm to 12mm, most preferably 12mm.
In one embodiment of the invention, aqueous slkali is NaOH solution or KOH solution.
In one embodiment of the invention, the concentration of aqueous slkali is 2mol/L to 3.5mol/L, Preferably 1mol/L to 3.5mol/L, further preferably 2mol/L to 2.5mol/L, most preferably 2mol/L.
In one embodiment of the invention, not corrosion-resistant with the big conductor bucket of negative electrode directly contacts.
In one embodiment of the invention, negative electrode is graphite electrode.
In one embodiment of the invention, in stepb the placement of W rod is made to electrolyte Obtain the length 2mm to 5mm longer than the length of required needle electrode of electrolyte submergence W rod, Preferably 2mm to 6mm, further preferably 2mm to 4mm, most preferably 3mm.
In one embodiment of the invention, electrolytic etching is in the voltage zone corresponding to electrochemical polish Territory is carried out.
In one embodiment of the invention, the voltage in electrolytic etching is 5V to 7V, preferably 5V to 7V, further preferably 5.5V to 6.5V, most preferably 6V.
In one embodiment of the invention, step b is made up of following two step:
B1. W rod is immersed 5mm-10mm longer than the length of required needle electrode in electrolyte, Preferably 5 to 9mm, further preferably 5 to 8mm, most preferably 6mm, electrolytic etching 30 to 120 points Clock;
B2. W rod is taken out after cleaning, then W rod is immersed in electrolyte than required needle-like The long 2mm-5mm of length of electrode, preferably 1mm to 5mm, further preferably 2mm to 4mm, Preferably 3mm, the diameter of electrolytic etching to required needle electrode.
In one embodiment of the invention, step c promotes W rod 1mm to 2mm, excellent Select 1mm to 2mm, further preferably 1mm to 2mm, most preferably 2mm.
Another aspect of the present invention relates to a kind of device for preparing needle electrode, described device bag Include: electrolytic vessel;
Electrolyte, described electrolyte is aqueous slkali, is arranged in described electrolytic vessel;
The big corrosion-resistant bucket of conductor and the corrosion-resistant bucket of little conductor, the described corrosion-resistant bucket of big conductor and little conductor are resistance to Corrosion bucket is arranged concentrically on the center of described electrolytic vessel;
Insulated sleeve, the diameter of described insulated sleeve is slightly larger than the diameter of required needle electrode;
Negative electrode, described negative electrode is arranged on outside the corrosion-resistant bucket of conductor;
Anode, described anode is the W rod of needle electrode to be made, and is arranged on electrolytic vessel center.
Prepared according to the methods of the invention needle electrode is related in another aspect of the invention.
Preparation method of the present invention is simple, it is easy to draw materials, and yield rate is high, it is easy to large-scale production.And The electrode produced is grading profile, and the RF fields near ion apply ion trap is less. Under full manual operation state, a skilled student, make 10 electrodes, finished product averagely can have 8-10.Owing at solution and air interface, corrosion rate for corrosion material is faster than inside solution, So electrode can first corrode disconnected in gas-liquid intersection, the electrode dropped is enclosed in below liquid level, keeps away simultaneously Exempt from the air corrosion to electrode, ensure that electrode surface is not oxidized the most simultaneously.
Owing to adding 304 stainless steel casks of large size, strengthen electric field, and be that electric field becomes axle pair Claim distribution, electrode is placed in bucket central authorities simultaneously so that corrode the electrode and be also distributed for axial symmetry.If Aforementioned condition is unsatisfactory for, then the shape that electrode corrosion goes out is not the most axisymmetric.The electric field strengthened, makes The W rod to be prepared that length is identical must be had close corrosion potentials (such as 40mm, 50mm, 60mm It is 6V).
Accompanying drawing explanation
Fig. 1 is that the eletrode tip diameter of example 1 preparation averagely only has 100nm
Fig. 2 is experimental provision schematic diagram
Fig. 3 is the electrode that the embodiment 1 that optical microscope shoots prepares
Fig. 4 is the electrode difference that contrast STM is prepared with this method.The left side is STM manufacture method The electrode of lower preparation, right-hand member is the electrode that a process for preparing.
Fig. 5 is test data of experiment, and applying voltage of the present invention should make to be in polishing during electrode corrosion District.
Fig. 6 is ion trap electrodes schematic diagram
Fig. 7 is the optical microscope photograph of the electrode of embodiment 2.
Fig. 8 is the SEM electron scanning micrograph of the electrode of embodiment 2.
Fig. 9 is the optical microscope photograph of the electrode of embodiment 3
Figure 10 is the SEM electron scanning micrograph of the electrode of embodiment 3.
Figure 11 is the corruption rough for 3V30mm2mol/L NaOH of optical microscope shooting Erosion result
Detailed description of the invention
For solving above technical problem, the present invention proposes a kind of needle electrode preparation method.Method is divided into Two pieces, first is the making of electrode body, and second is the making of electrode needle point.
Corrosion principle:
Using electrode as anode, it is immersed in alkaline electrolyte (such as NaOH), adds DC direct current inclined Pressure, W rod occurs to react as follows:
Anode: 6H2O+6e-→3H2(g)+6OH-
Negative electrode: W(s)+8OH-→WO4 2-+4H2O+6e-
Overall: W(s)+2OH-+2H2O→WO4 2-+3H2(g)。 (1)
Final result is that anode W is oxidized to WO4 entrance solution, removes from W rod surface;Cloudy Pole produces hydrogen.Owing to reaction rate reaches maximum, as the latter half W at liquid level air interface Rod weight is more than corroding the stress that the fastest cervical region can bear, and breaking at liquid level intersection is two joints, often Part all forms a needle point.
Comprise the following steps:
1. with ethanol and distilled water, tungsten bar carried out surface cleaning, and use dust-free paper wiped clean.
2. step up to be installed on the one-dimensional translation stage of vertical direction by electrode drill chuck, and corruption will be treated The tungsten bar of erosion is connected with positive source.
3. the NaOH solution preparing 2mol/L is placed in 500mL beaker.Beaker is put with one heart Put small one and large one two 304 rustless steel steel drums, big height be higher than liquid level of solution, little diameter 10mm, Highly 8mm.Between big stainless steel cask and beaker, (electrode can not be with big rustless steel for placing graphite electrode Bucket has directly contact), and graphite electrode is connected with power cathode.
4. adjusting one-dimensional translation stage makes W rod to be corroded go deep into the following certain length of liquid level of solution.This Length is prepared and is added 5mm-10mm required by electrode required for being.
5. turn on the power, adjust voltage and (make to be in corresponding to electrochemical polish when clicking on corrosion Voltage regime) tungsten bar carried out pre-etching, time 1min.
6. take out W rod, and with distilled water, surface NaOH is cleaned up.Measure W rod diameter, And be again placed in corroding on platform, adjust one-dimensional translation stage and make W rod go deep into liquid level system claimed below Standby length adds 2mm-5mm again.
7. adjustment W rod is vertical with liquid level (observes its inverted image below liquid level, with the tungsten in air Rod overlap be can determine whether during a straight line modulated whole good), and be in big 304 stainless steel cask middles, The most just to 304 little stainless steel casks.
8. adjust appropriate voltage (to make to be in the voltage zone corresponding to electrochemical polish when clicking on corrosion Territory), turn on the power, start corrosion.
9., after a period of time, taking out its diameter of electrode measurement, if reaching requirement, then carrying out next step Suddenly, this step is otherwise repeated.
10. after electrode diameter reaches requirement, by internal diameter slightly larger than the plastics with required electrode diameter Pipe box, in W rod lower end, adjusts appropriate length, in order to stop the electrode reaching diametric requirements to continue Corrosion.Being reduced by the electrode packaging pipe clips on drill chuck, is raised above behind the position before being adjusted to Electrode bar 1-2mm (prevents treating that before electrode prepares completely corrosion electrode has been eclipsed disconnected), starts Corrosion needle point.
11. turn on the power so that electrode starts corrosion, until W rod to be corroded ruptures and drops to In the little stainless steel cask of lower section, whole electrode preparation work completes.
12. electrodes prepared with observation by light microscope, measurement, check whether to reach requirement.
The W rod used is pure tungsten tungsten bar and NaOH solution.In order to prepare the concordance of electrode with Success rate, electrode must be in 304 stainless steel cask middles, and vertical with liquid level.
Embodiment
The preparation of ion trap electrodes is described with an example below.
Embodiment 1
Choose pure tungsten tungsten bar, diameter 1.6mm, 30V, 3A voltage source.Need to prepare 50mm length The electrode of dt=0.500mm diameter.
The first step: measure tungsten bar diameter d0=1.564mm, and clean with distilled water.
Second step: be placed in by tungsten bar on corrosion platform, take out after pre-etching 1min is straight after measuring corrosion Footpath d1=1.555mm.Diameter after measurement should prepare electrode diameter needed for being not less than.Calculate in 1min The electrode diameter change that corrosion causes, then corrosion rate is about (d0-d1)=0.009mm/min.
Second step: again place and treat that corrosion electrode, on a translation stage, adjusts electrode position and makes leaching Entering the following electrode length of liquid level is 40mm.
3rd step: adjust voltage source output voltage 6V, and turn on the power.About a period of time (d1-dt)/(d0-d1)=(1.555-0.500)/(1.564-1.555)=117min (the actual waiting time is 110min, Maximum time 117min less than estimating) after again measure W rod diameter, if not up to requiring, continue corruption Erosion, until reaching diametric requirements.
4th step: intercept 40mm long internal diameter 0.5mm-0.7mm plastic tube, be placed on tungsten bar lower end to be corroded. It is replaced on corrosion platform and corrodes, turn on the power, until corrosion electrode is dropped little with following In 304 stainless steel casks.
Experiment condition: diameter 1.6mm tungsten bar, 6V voltage, 2mol/LNaOH solution, submergence 40mm Measurement result:
Away from distance between two tips Measure diameter
0nm 113nm
193.7nm 462.7nm
613.4nm 655.7nm
1.5um 772.2nm
1mm 153.8um
15mm 0.509mm
30mm 0.508mm
45mm 0.505mm
Embodiment 2
Choose diameter 0.5mm, submergence 40mm, NaOH concentration 2mol/L, voltage 5V, according to In embodiment one, step makes, it is possible to obtaining finished product needlepoint electrode, measurement result is as follows:
Away from distance between two tips Measure diameter
0nm 153.2nm
326nm 619.4nm
1.2um 701.2nm
3.1um 947.2nm
10mm 0.489mm
20mm 0.478mm
30mm 0.491mm
40mm 0.475mm
Embodiment 3
Choose diameter 0.5mm, submergence 40mm, NaOH concentration 2mol/L, voltage 7V, according to In embodiment one, step makes, it is possible to obtaining finished product needlepoint electrode, measurement result is as follows:
Away from distance between two tips Measure diameter
0nm 142.5nm
165.1nm 495.4nm
726.6nm 1.046um
1.2um 1.108um
2.8um 1.131um
10mm 0.476mm
20mm 0.493mm
30mm 0.484mm
40mm 0.473mm
Embodiment 4
Choose diameter 0.5mm, submergence 30mm, NaOH concentration 2mol/L, voltage 7V, according to In embodiment one, step makes, it is possible to obtaining finished product needlepoint electrode, measurement result is as follows:
Away from distance between two tips Measure diameter
0nm 91.06nm
200nm 364.3nm
566.7nm 571.9nm
1.4um 765.2nm
2.4um 768.9nm
10mm 0.496mm
20mm 0.495mm
30mm 0.495mm
Embodiment 5
Choose diameter 0.5mm, submergence 50mm, NaOH concentration 2mol/L, voltage 7V, according to In embodiment one, step makes, it is possible to obtaining finished product needlepoint electrode, measurement result is as follows:
Away from distance between two tips Measure diameter
65.8nm 134.0nm
263.2nm 137.0nm
565.8nm 320.6nm
881.6nm 443.1nm
1.4um 565.3nm
10mm 0.499mm
20mm 0.496mm
30mm 0.497mm
40mm 0.478mm
50mm 0.487mm

Claims (13)

1. the method preparing needle electrode, said method comprising the steps of:
A. in electrolytic vessel, put into aqueous slkali as electrolyte, place two the most with one heart The corrosion-resistant bucket of conductor varied in size, the corrosion-resistant bucket of big conductor is higher than liquid level of solution, at big conductor corrosion resistant Outside erosion bucket, negative electrode is set, and not corrosion-resistant with the big conductor bucket of described negative electrode directly contacts;
B. W rod is placed to described electrolyte as anode so that W rod also position vertical with liquid level In the center of the corrosion-resistant bucket of conductor, the diameter of electrolytic etching to required needle electrode;
C. internal diameter is slightly larger than the insulative pipe sleeve of diameter of required needle electrode in W rod lower end extremely Expection forms the position of needle point, promotes W rod but still keeps the position forming needle point to be still immersed in described In electrolyte;
D. electrolytic etching W rod is continued until W rod ruptures;
The W rod dropped in the corrosion-resistant bucket of little conductor of lower section is required needle electrode.
Method the most according to claim 1, a diameter of 5mm of its corrosion-resistant bucket of medium and small conductor To 10mm;The height of the corrosion-resistant bucket of little conductor is 6mm to 10mm.
Method the most according to claim 1, wherein said aqueous slkali is NaOH solution or KOH Solution.
Method the most according to claim 1, the concentration of wherein said aqueous slkali be 2mol/L extremely 3.5mol/L。
Method the most according to claim 1, wherein said negative electrode is graphite electrode.
Method the most according to claim 1, places W rod to electrolysis the most in stepb Liquid makes the length 2mm longer than the length of required needle electrode of electrolyte submergence W rod extremely 5mm。
Method the most according to claim 1, wherein said electrolytic etching is corresponding to W rod electricity The voltage regime of chemical polishing is carried out.
Method the most according to claim 1, the voltage in wherein said electrolytic etching be 5V extremely 7V。
Method the most according to claim 1, wherein step b is made up of following two step:
B1. W rod is immersed 5mm-10mm longer than the length of required needle electrode in electrolyte, Electrolytic etching 30 to 120 minutes;
B2. W rod is taken out after cleaning, then W rod is immersed in electrolyte than required needle-like The long 2mm-5mm of length of electrode, the diameter of electrolytic etching to required needle electrode.
Method the most according to claim 1, promotes W rod 1mm in wherein said step c To 2mm.
11. methods according to claim 1, the most in stepb, adjust W rod and liquid level Vertically, observe W rod inverted image below liquid level, adjust W rod and make inverted image and the tungsten bar in air Coincidence is a straight line, to ensure equally distributed electric field around W rod.
12. 1 kinds of devices being used for preparing needle electrode, described device includes:
Electrolytic vessel;
Electrolyte, described electrolyte is aqueous slkali, is arranged in described electrolytic vessel;
The big corrosion-resistant bucket of conductor and the corrosion-resistant bucket of little conductor, the described corrosion-resistant bucket of big conductor and little conductor are resistance to Corrosion bucket is arranged concentrically on the center of described electrolytic vessel, and the described corrosion-resistant bucket of big conductor is higher than molten Liquid liquid level;
Insulated sleeve, the diameter of described insulated sleeve is slightly larger than the diameter of required needle electrode;
Negative electrode, described negative electrode is arranged on outside the corrosion-resistant bucket of conductor, and described negative electrode is not resistance to big conductor Corrosion bucket directly contacts;
Anode, described anode is the W rod of needle electrode to be made, and is arranged on electrolytic vessel center.
13. 1 kinds of needle electrodes, arbitrary by according in claim 1 to 11 of described needle electrode Prepared by the method described in Xiang.
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CN118016376B (en) * 2024-04-08 2024-08-13 国开启科量子技术(安徽)有限公司 Method for preparing needle electrode of ion trap

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