CN102288844B - Method for integration of electrode on diamond anvil cell - Google Patents
Method for integration of electrode on diamond anvil cell Download PDFInfo
- Publication number
- CN102288844B CN102288844B CN 201110126216 CN201110126216A CN102288844B CN 102288844 B CN102288844 B CN 102288844B CN 201110126216 CN201110126216 CN 201110126216 CN 201110126216 A CN201110126216 A CN 201110126216A CN 102288844 B CN102288844 B CN 102288844B
- Authority
- CN
- China
- Prior art keywords
- diamond
- anvil
- boron
- electrode
- diamond anvil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Abstract
The invention relates to a method for integration of electrodes on a diamond anvil cell. Boron-doped diamond electrodes are prepared on a diamond anvil by adopting the nano seedling technology, the film deposition technology and the ion beam etching technology. Film deposition comprises deposition of a boron-doped diamond film used as an electrode and deposition of an aluminum oxide film used in a protective layer during preparation. The whole diamond anvil is bombed through argon ion beams, the boron-doped diamond film in insulating strips among the design electrodes are broken finally to form electrodes, the problem of electrode conduction caused by breakage of the cover film formed in selective deposition of the boron-doped diamond film at high temperature can be avoided, and the rate of success in preparation of the diamond electrodes on the metal anvil can be improved.
Description
Technical field
The invention belongs to the technical field of high-tension unit, particularly a kind of method for making for the electrode of original position electric parameter measurement on the diamond anvil cell.
Background technology
Diamond anvil cell (DAC) is the ultra-high pressure apparatus that generally uses in the world at present, is fit to and the supporting in site measurement of carrying out physical quantity under the High Temperature High Pressure of various test.Combine with electrical devices, can carry out the in site measurement of high pressure electrical quantities.Situ high pressure electrical measurement structure of matter phase transformation and electronic structure phase transformation under the reflection extreme condition, survey the metallization phase transformation, find to press and cause aspect the superconducting phenomenon, being proved is a kind of effectively method.
By the end of so far, in the experimental provision about the experiment of high pressure electric parameter measurement of all reports, employed electrode generally is divided into two kinds: a kind of is metal electrode, and another kind is diamond electrode.There is following shortcoming in metal electrode: the first, and when measuring hard material, electrode and insulation course rupture easily in pressurization and the stress-relief process, can not carry out repeated measurement and use; The second, can not be to having corrosive sample or easily being measured by the fluid of electrolysis.The introducing of diamond electrode can prevent that cross shear is to the destruction of electrode, improve the reliability of measuring microcircuit, overcome under the condition of high voltage sample to the corrosion of electrode, so that the in site measurement of the electrical quantities that has the corrosivity sample under the high pressure is become possibility, thereby widened the research field of electrical quantity in-situ measurement under the high pressure, in the high pressure electricity experiments of measuring in future, will be widely used.
Be called " being used for electrode of original position electrical measurement on the diamond anvil cell and preparation method thereof " in name, publication number is in the patent of CN101509947, has stated the method for preparing diamond electrode at diamond anvil.Utilize aluminium oxide to do mask in the preparation process, utilize hot-wire chemical gas-phase deposition selectivity on diamond anvil cell to deposit the boron doped diamond thin of one deck as electrode.The selectivity deposition process of whole Boron-doped diamond is finished under hot conditions.Experiment showed, because the thermal expansivity of diamond anvil and aluminum oxide polycrystal mask there are differences, cause whole experimentation comparatively harsh to temperature requirement.Temperature distributing disproportionation in the hot-wire chemical vapor phase deposition instrument around the filament is even, so that substrate (diamond anvil) temperature distributing disproportionation, makes under the hot conditions aluminum oxide film phenomenon that is damaged easily, causes the mask failure, thereby affects the preparation of electrode.
Summary of the invention
The technical problem to be solved in the present invention is, utilize nano crystal introduction technology, film deposition techniques and ion beam etching technology, with being prepared on the diamond anvil of boron-doped diamond electrode success, overcame in the past in opposed anvils preparation diamond electrode process and caused the difficulty of the failure of an experiment owing to mask breaks, improved the success ratio for preparing diamond electrode at diamond anvil.
Technical scheme of the present invention is as follows.
A kind of on diamond anvil cell the method for Integrated electrode, minute eight steps are finished,
The first step: diamond anvil is put into the mixed liquid dipping of acetone and alcohol to remove surface blot, used deionized water rinsing after taking out, immerse after the oven dry in the nano-diamond powder suspending liquid, take out again oven dry;
Second step: will put into chemical vapor deposition unit with the diamond anvil of nano-diamond powder, and carry out the deposition of boron-doped diamond film;
The 3rd step: the vacuum chamber of magnetic control sputtering device is put into the diamond anvil of boron-doped diamond film in the surface, utilize magnetically controlled sputter method that pellumina is deposited on boron-doped diamond film surface;
The 4th step: the diamond anvil that will be coated with pellumina takes out, smear photoresist on its surface, the graphics shape that utilizes photoetching technique to carve para tape between electrode in anvil face and the side of diamond anvil, the pellumina that under the boiling water bath condition, exposes with phosphoric acid corrosion power down electrode insulation band place;
The 5th step: diamond anvil is inserted in the vacuum chamber of ion beam sputtering device, utilize ar-ion beam that diamond anvil is bombarded; The condition of work of ion beam sputtering device is: operating air pressure 2.4 * 10
-1～3.0 * 10
-1Pa, anode working voltage 62V, working current 0.62A, cathode work current 18A, operating plate voltage 500～600V, line voltage 200V, line electric current 40～50mA accelerates electric current 10mA, bombardment time 3～5 minutes;
The 6th step: be that 1: 1 nitric acid and the mixed liquor of sulfuric acid are made corrosive liquid with volume ratio, the protective layer of alumina on the adamas anvil face is eroded, with alcohol and acetone it is cleaned up respectively;
The 7th step: repeat the process in the 3rd to six step, until the boron-doped diamond film at para tape place is disconnected the electrode that becomes mutual not conducting by bombardment fully between electrode;
The 8th step: copper wire is adhered on the exposed boron-doped diamond membrane electrode in diamond anvil side with the silver slurry.
In the second step of the inventive method, the thickness of deposition boron-doped diamond film can be at 500nm～2 μ m; In the 3rd step, the thickness of deposition of aluminium oxide film can be at 200～300nm; In the 7th step, the process that repeated for the 3rd to six step will repeat 4～28 times like this.
In the first step of the inventive method, diamond anvil immerses in the nano-diamond powder suspending liquid, takes out oven dry again, repeat 5 times, and each oven dry can be carried out under 100 ℃.Make the diamond anvil surface attachment be suitable for the Nano diamond particle of boron-doped diamond growth.
This work is to subsidize the lower achievement that obtains in project of national nature science fund project (10874053,11074094,50802033,91014004) and national basis research project (2011CB808204).Process, the process conditions in first, second, third and fourth step of the present invention and the 8th step are identical with background technology basically.Characteristics of the present invention are to adopt the ion beam sputtering device, utilize ar-ion beam that whole diamond anvil is bombarded, and the boron-doped diamond film at para tape place is disconnected form electrode.The mask that its beneficial effect is to have avoided the selectivity deposition of boron-doped diamond film under hot conditions to cause breaks and makes the problem of conducting between electrode, improves the success ratio at diamond anvil preparation diamond electrode.The method of the present invention's Integrated electrode on diamond anvil cell has wide practical use in situ high pressure electrical measurement field.
Description of drawings
Fig. 1 be of the present invention on diamond anvil cell the method flow synoptic diagram of Integrated electrode.
Among Fig. 1,
1 represents the nano-diamond powder seeding layer; 2 represent the boron-doped diamond film, namely are the boron-doped diamond membrane electrode after completing; 3 represent pellumina.
(f) is the diamond anvil with electrode that completes among Fig. 1.Wherein, 2 is the electrode of boron-doped diamond film, and the boron-doped diamond film is divided into four by crosshair and forms four electrodes; 5 is the silver slurry; 4 is copper conductor, is bonded in the side of diamond anvil.Silver slurry 5 makes copper conductor firmly be connected with the boron-doped diamond membrane electrode, for use in the in site measurement of electrical quantities under the high pressure.
Embodiment
Further specify by reference to the accompanying drawings process means of the present invention [whole process is shown in (a)～(f) among Fig. 1]:
The first step: diamond anvil is put into the mixed liquid dipping 20 minutes of acetone and alcohol to remove surface blot, used deionized water rinsing after the taking-up.After the oven dry, immerse in the nano-diamond powder suspending liquid, take out again under 100 ℃ of conditions and dry, so repeat 5 times.Shown in Fig. 1 (a).
This step purpose is to make diamond anvil surface attachment one deck Nano diamond particle, and these particles are conducive to next step as nucleus and deposit boron doped diamond film.
Second step: will put into chemical vapor deposition (CVD) device with the diamond anvil of nano-diamond powder, and carry out the deposition of boron-doped diamond film.Keeping base reservoir temperature in the deposition process is 750 ℃～950 ℃, and the thickness of boron-doped diamond film is 500nm～2 μ m.Shown in Fig. 1 (b).
The 3rd step: the vacuum chamber of magnetic control sputtering device is put into the diamond anvil of boron-doped diamond film in the surface, utilize magnetically controlled sputter method that pellumina is deposited on the diamond anvil surface, cover the boron-doped diamond film.Shown in Fig. 1 (c).
In sputter procedure, adopt metallic aluminium as target, throughput ratio between 30: 2.0～3.0 oxygen and argon gas as working gas, the pressure in the vacuum chamber remains on 0.8～1.2Pa, underlayer temperature remains on 200 ℃～300 ℃.
The 4th step: the diamond anvil that will deposit pellumina takes out, smear one deck photoresist at its surface uniform, utilize photoetching technique to carve the graphics shape of para tape between electrode at the adamas anvil face, present embodiment is shaped as example with crosshair, then corrode with corrosive liquid that (corrosive liquid is phosphoric acid, the beaker of containing phosphoric acid places boiling water bath), make to present crosshair on the anvil face, the cross hair width can be at 30～100 μ m.Shown in Fig. 1 (d).
The 5th step: will insert in the ion beam sputtering instrument vacuum chamber with the diamond anvil of protective layer of alumina, and utilize ar-ion beam that whole diamond anvil is bombarded.Ion beam instrument condition of work is: operating air pressure is about 2.4～3.0 * 10
-1Pa, anode working voltage 62V, working current 0.62A, cathode work current 18A, operating plate voltage 500～600V, line voltage 200V, line electric current 40～50mA accelerates electric current 10mA.Bombardment time is: 3 minutes.
The loss speed v that the boron-doped diamond film is bombarded under this condition is approximately 25nm/min.The loss speed of pellumina protective seam is about 50nm/min.So be unlikely to that with 3 minutes bombardment times protective layer of alumina is destroyed and lose its protective effect (that is, bombardment to as the boron-doped diamond film of electrode).When the thickness of pellumina is larger, also can bombard 5 minutes, only otherwise lose the protective effect of pellumina.
The 6th step: with corrosive liquid (volume ratio is 1: 1 nitric acid and the mixed liquor of sulfuric acid) the pellumina protective seam on the diamond anvil anvil face is eroded, with alcohol and acetone it is cleaned up.
The 7th step: repeat the process in the 3rd to six step, so that boron doped diamond film is disconnected the electrode that becomes four mutual not conductings by bombardment fully.Shown in Fig. 1 (e).
The frequency n that repeated for the 3rd to six steps depends on the thickness d of boron-doped diamond film, n=d/ (3～5) v (when containing decimal among the n, polishing is integer).
The 8th step: copper wire that will be very thin is adhered on the exposed electrode in diamond anvil side, solidifying about two hours under 150 ℃ the condition, to reach the use desirable strength with the silver slurry.Shown in Fig. 1 (f).
Claims (2)
1. the method for an Integrated electrode on diamond anvil cell divides eight steps to finish,
The first step: diamond anvil is put into the mixed liquid dipping of acetone and alcohol to remove surface blot, used deionized water rinsing after taking out, immerse after the oven dry in the nano-diamond powder suspending liquid, take out again oven dry;
Second step: will put into chemical vapor deposition unit with the diamond anvil of nano-diamond powder, and carry out the deposition of boron-doped diamond film;
The 3rd step: the vacuum chamber of magnetic control sputtering device is put into the diamond anvil of boron-doped diamond film in the surface, utilize magnetically controlled sputter method that pellumina is deposited on boron-doped diamond film surface;
The 4th step: the diamond anvil that will be coated with pellumina takes out, smear photoresist on its surface, the graphics shape that utilizes photoetching technique to carve para tape between electrode in anvil face and the side of diamond anvil, the pellumina that under the boiling water bath condition, exposes with phosphoric acid corrosion power down electrode insulation band place;
The 5th step: diamond anvil is inserted in the vacuum chamber of ion beam sputtering device, utilize ar-ion beam that diamond anvil is bombarded; The condition of work of ion beam sputtering device is: operating air pressure 2.4 * 10
-1～3.0 * 10
-1Pa, anode working voltage 62V, working current 0.62A, cathode work current 18A, operating plate voltage 500～600V, line voltage 200V, line electric current 40～50mA accelerates electric current 10mA, bombardment time 3～5 minutes;
The 6th step: be that 1: 1 nitric acid and the mixed liquor of sulfuric acid are made corrosive liquid with volume ratio, the protective layer of alumina on the diamond anvil anvil face is eroded, with alcohol and acetone the diamond anvil that is corroded is cleaned up;
The 7th step: repeat the process in the 3rd to six step, until the boron-doped diamond film at para tape place is disconnected the electrode that becomes mutual not conducting by bombardment fully between electrode;
The 8th step: copper wire is adhered on the exposed boron-doped diamond membrane electrode in diamond anvil side with the silver slurry.
According to claim 1 on diamond anvil cell the method for Integrated electrode, it is characterized in that in second step, the thickness of deposition boron-doped diamond film is at 500nm～2 μ m; In the 3rd step, the thickness of deposition of aluminium oxide film is at 200～300nm; In the 7th step, the process that repeated for the 3rd to six step will repeat 4～28 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110126216 CN102288844B (en) | 2011-05-17 | 2011-05-17 | Method for integration of electrode on diamond anvil cell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110126216 CN102288844B (en) | 2011-05-17 | 2011-05-17 | Method for integration of electrode on diamond anvil cell |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102288844A CN102288844A (en) | 2011-12-21 |
| CN102288844B true CN102288844B (en) | 2013-10-23 |
Family
ID=45335422
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110126216 Expired - Fee Related CN102288844B (en) | 2011-05-17 | 2011-05-17 | Method for integration of electrode on diamond anvil cell |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102288844B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105261555B (en) * | 2015-08-28 | 2018-04-20 | 中国科学院高能物理研究所 | A kind of method that metal electrode is prepared on diamond anvil |
| CN110095505A (en) * | 2019-03-13 | 2019-08-06 | 东北电力大学 | A kind of method of Transition-metal dichalcogenide energy gap regulation |
| CN110687151A (en) * | 2019-11-05 | 2020-01-14 | 中国工程物理研究院材料研究所 | Preparation method of fine sample for diamond opposite-vertex anvil press |
| CN113777142A (en) * | 2021-09-15 | 2021-12-10 | 湖南新锋科技有限公司 | Carbon material/metal modified doped diamond particle integrated sensor and preparation method and application thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH073401B2 (en) * | 1985-02-25 | 1995-01-18 | 株式会社豊田中央研究所 | Ion sensor manufacturing method |
| CN1192691C (en) * | 2002-06-16 | 2005-03-09 | 吉林大学 | Process for integrating metal electrodes to diamond stock |
| CN100545646C (en) * | 2007-06-22 | 2009-09-30 | 吉林大学 | Be used for adamas opposed anvils of electrical quantity in-situ measurement and preparation method thereof |
| CN101509947B (en) * | 2008-12-30 | 2011-05-04 | 吉林大学 | Electrode for in-situ electrical measurement for diamond anvil cell and method for producing the same |
-
2011
- 2011-05-17 CN CN 201110126216 patent/CN102288844B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102288844A (en) | 2011-12-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101509947B (en) | Electrode for in-situ electrical measurement for diamond anvil cell and method for producing the same | |
| CN102288844B (en) | Method for integration of electrode on diamond anvil cell | |
| Meng et al. | Effect of microstructures on corrosion behavior of nickel coatings:(II) competitive effect of grain size and twins density on corrosion behavior | |
| CN102262989B (en) | Method for manufacturing anodic aluminum oxide template and method for manufacturing field emission cathode array material by using template | |
| JP4464041B2 (en) | Columnar structure, electrode having columnar structure, and manufacturing method thereof | |
| CN100593015C (en) | Surface nano tip array and its preparing method | |
| CN105898907A (en) | Graphene heating film and preparation method thereof | |
| CN100545646C (en) | Be used for adamas opposed anvils of electrical quantity in-situ measurement and preparation method thereof | |
| CN105870405B (en) | A kind of method that alloy is welded and taken off using Alloy by Laser Surface Remelting technology composite diffusion and prepares lithium ion battery silicium cathode | |
| CN205902105U (en) | Graphite alkene heating film | |
| CN102288824A (en) | Electrode for high-voltage in-situ impedance measurement and preparation method and application of same | |
| CN111354615B (en) | Transmission electron microscope in-situ electro-thermal coupling chip and preparation method thereof | |
| CN108470777B (en) | Preparation method of material testing unit with nano-scale interval small electrodes for in-situ power-on chip of transmission electron microscope | |
| CN103904186A (en) | Semiconductor device based on graphene electrode and manufacturing method thereof | |
| CN105448621A (en) | Graphene film electronic source, manufacture method for the same, and vacuum electronic device | |
| CN102492924A (en) | Autologous ion bombardment assisted electron beam evaporation device, and method for coating film by using same | |
| CN111521656A (en) | High-sensitivity high-stability boron-doped diamond microelectrode and preparation method and application thereof | |
| CN102183693B (en) | Electrodes for high pressure in situ resistivity survey and manufacturing method of electrodes | |
| Tao et al. | Microstructure and electrical conductivity of electroless copper plating layer on magnesium alloy micro-arc oxidation coating | |
| CN106803570A (en) | A kind of lithium battery SiCO carbon nano-tube coextruded film electrodes | |
| Lee et al. | Direct electrodeposition of thin metal films on functionalized dielectric layer and hydrogen gas sensor | |
| CN105702942A (en) | Silicon-based negative electrode material and preparation method and application thereof | |
| CN108390013A (en) | A kind of lithium ion battery electrode material nano surface metal-modified method | |
| CN101150028A (en) | Large area electron field emission nano structure array and its preparation method | |
| CN102243967B (en) | Preparation method for cathode of ballistic field-emitting display device based on porous dielectric material thin film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20131023 Termination date: 20140517 |