CN107796959A - Different oxygen fugacity in-situ control methods in a kind of diamond anvil cell electrical measurement - Google Patents
Different oxygen fugacity in-situ control methods in a kind of diamond anvil cell electrical measurement Download PDFInfo
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- CN107796959A CN107796959A CN201710954014.0A CN201710954014A CN107796959A CN 107796959 A CN107796959 A CN 107796959A CN 201710954014 A CN201710954014 A CN 201710954014A CN 107796959 A CN107796959 A CN 107796959A
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- diamond anvil
- oxygen fugacity
- buffering ring
- fugacity
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- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
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Abstract
The invention discloses different oxygen fugacity in-situ control methods in a kind of diamond anvil cell electrical measurement are provided, it includes：The making of step 1, oxygen fugacity buffering ring；Step 2, utilize oxygen fugacity buffering ring making insulated compound pad；Step 3, the deposition in diamond anvil face progress different metal metal oxide, and form electrode configuration；Step 4, by insulated compound pad and in the deposition of diamond anvil face different metal metal oxide form closed sample cavity；When solving prior art the experiment of HTHP electricity is carried out in DAC, due to the particularity of DAC devices, its sample cavity only has hundred micron dimensions, the oxygen fugacity control method of generally use in traditional electrical properties measurement process, it is difficult to reach preferable effect；How solid buffer agents are effectively integrated in the small cavitys of DAC also without technical problems such as accurate implementation methods.
Description
Technical field：
The invention belongs to physical quantity in-situ technique field under condition of high voltage, more particularly to a kind of diamond anvil cell electricity
Learn different oxygen fugacity in-situ control methods in measurement.
Background technology：
Diamond anvil cell (Diamond Anvil Cell, abbreviation DAC) is currently the only can to produce million atmospheric pressure
The science apparatus of static pressure, it is high-pressure science and most important scientific instrument in technical field of research.Utilize DAC, Ren Menneng
The change of the structure and physical property of material under ultra-high voltage environment is enough observed, especially shows the pressure of laboratory simulation Earth
In terms of power and temperature environment.The pressure and temperature environment of laboratory simulation Earth can study each layer related substances of the earth
Static physical and chemical property are explanation of seismic wave number evidences, understand the important channel of earth's internal structure and dynamic process.With
The fast development of high-pressure science technology, each breakthrough of in site measurement means, can all expand and enrich high-pressure science under high pressure
The possibility of research.
Various HTHP electricity experiment in, contain valence variation element in all samples, wherein oxygen fugacity just as temperature, pressure
Power equally turns into one of most basic external key elements for influenceing experiment.The control in place of oxygen fugacity becomes high temperature under HTHP
Particularly important basic problem in High-Voltage Experimentation technology.In existing high-pressure installation, the control of oxygen fugacity is mainly used in
In the equipment such as multiaspect top large cavity press, autoclave.The method of use mainly has：(1) gas buffer agent method, (2) solid buffer
Agent method and (3) comprehensive buffer method.These oxygen fugacity control technologies in large cavity press are very ripe.Yet with
The particularity of DAC devices, its sample cavity only have hundred micron dimensions, the oxygen ease of generally use in traditional electrical properties measurement process
Spend control method, it is difficult to reach preferable effect, cause different oxygen fugacity control problems in DAC never to be solved well
Certainly.It is well known that oxygen fugacity is the monotropic function of temperature and pressure, in various high temperature and pressure experiment, by changing solid oxygen
Contained variable valency metal element type in buffer, to realize any control and regulation of different oxygen fugacities in sample chamber.Such as
Solid buffer agents are effectively integrated in the small cavitys of DAC also without accurate implementation method etc. by what.
The content of the invention：
The technical problem to be solved in the present invention：There is provided different oxygen fugacities in a kind of diamond anvil cell electrical measurement control in situ
Method processed, when carrying out the experiment of HTHP electricity to solve prior art in DAC, due to the particularity of DAC devices, its sample
Chamber only has hundred micron dimensions, the oxygen fugacity control method of generally use in traditional electrical properties measurement process, it is difficult to reach reason
The effect thought；How solid buffer agents are effectively integrated in the small cavitys of DAC also without technologies such as accurate implementation methods
Problem.
Technical solution of the present invention：
Different oxygen fugacity in-situ control methods in a kind of diamond anvil cell electrical measurement, it includes：
The making of step 1, oxygen fugacity buffering ring；
Step 2, utilize oxygen fugacity buffering ring making insulated compound pad；
Step 3, the deposition in diamond anvil face progress different metal-metal oxide, and form electrode configuration；
Step 4, by insulated compound pad and diamond anvil face different metal-metal oxide deposition formed it is closed
Sample cavity.
The preparation method of oxygen fugacity buffering ring described in step 1 includes：
Step 1.1, by metal and its corresponding metal oxide powder according to chemical reaction cushioning balance equation, carry out equal
Even mixing；
Step 1.2, mixture of powders will be obtained, and by means of hot isostatic press high-tension apparatus, carry out Thermocompressed sintering and forming shape
Into cylinder；
Step 1.3, corroded using spark discharge hot-forming metal-metallic oxide cylinder cut into thickness
For 60 μm of thin slice；
Step 1.4, using sand paper by thin slice uniform grinding to thickness be 50 μm；Finally, using laser cutting machine by thin slice
Circlewise, as oxygen fugacity buffering ring, inner ring radius is 80 μm, and outer shroud radius is 120 μm for cutting.
The method that step 2 makes insulated compound pad using oxygen fugacity buffering ring includes：
Step 2.1, selection T301 stainless steel substrates or rhenium piece make gasket material, with diamond anvil cell precompressed, in pad material
Diamond anvil face pressure trace, diamond anvil chamfering impression and diamond anvil incline impression are outwards pressed with by center on material, is utilized
Laser-beam drilling machine punches at diamond anvil face pressure trace concentric, and the diameter in hole is identical with the external diameter of oxygen fugacity buffering ring and is less than
Diamond anvil face impression diameter；
Step 2.2, oxygen fugacity buffering ring is fixed on concentric circle holes center and applying pressure fixes oxygen fugacity buffering ring；
Step 2.3, by bortz powder, cubic boron nitride powder or alumina powder and epoxy resin it is 4 in mass ratio:1 ratio
Example mixing, is inserted in the hole and all impressions of oxygen fugacity buffering ring after grinding uniformly, then is pressurizeed with diamond anvil cell concentric；
Step 2.4, by the use of burrowing at laser diamond anvil face pressure trace concentric in the third step it is used as sample cavity, sample
The diameter of chamber is less than the internal diameter of oxygen fugacity buffering ring.
The deposition of different metal-metal oxide is carried out in diamond anvil face and form electrode configuration method described in step 3
Including：
Step 3.1, diamond surface sputter layer of metal sull；
Step 3.2, layer of metal film is sputtered on metal-oxide film；
Step 3.3, using graphical etching system by metallic film etching be required electrode configuration.
Beneficial effect of the present invention：
Magnetron sputtering technique, film micro-processing technology and diamond anvil cell technology are combined by the present invention, utilize difference
The oxygen fugacity buffering ring that metal and its oxide are mixed, the closed sample cavity of controllable oxygen atmosphere is formd, so as to build
It is a kind of to can be widely applied to oxygen fugacity in-situ control in sample electrical properties measurement process under the extreme condition of HTHP
Experimental provision and measuring method；The integrated metal oxide of diamond anvil face and its metallic film not only can control in sample cavity
Oxygen atmosphere, can be used as electrode pair sample carry out HTHP under electrical properties measurement.This invention overcomes completely
The less shortcoming of DAC cavitys under HTHP, compensate for the blank of uncontrollable oxygen fugacity in DAC devices.It is of the invention simple
It is portable, it is safe and efficient, by slight improvements, upper and lower two diamond anvils can be used for carry out optics, magnetics, calorifics, mechanics,
A variety of tests such as acoustics, it is that the measurement under HTHP to a variety of physical quantitys of material creates advantage；Present invention design
Go out it is a set of can be widely applied in the small cavity of DAC high pressure electrical conductivity measurement experiment devices, it is solid by changing in experimentation
The type of contained metal and metal oxide in state oxygen buffering ring and buffer electrode, and then realize oxygen fugacity in sample chamber
Effectively and accurately control, therefore will greatly lift high pressure minerals physics and the measurement essence of material science original position electrical properties
Degree..
Brief description of the drawings：
Fig. 1 is diamond anvil cell oxygen fugacity control schematic sectional representation；
Fig. 1 a are precompressed pad and punched that Fig. 1 b are the insertion of oxygen fugacity buffering ring, and Fig. 1 c are the pressure of sample cavity insulating powder
Process processed, Fig. 1 d are the preparation of final sample chamber.Wherein, 1 is diamond anvil incline impression, and 2 be pad chamfering impression, and 3 are
Laser ablated holes；4 be oxygen buffering ring, and 5 be cubic boron nitride insulating powder, and 6 be the sample well of the laser ablation on insulating powder；
Fig. 2 is sample overall package profile；
Detailed construction is：7 be oxygen buffering ring, and 8 be insulating barrier, and 7 and 8 be outer layer and internal layer position relationship；9 be steel alloy,
10 be beryllium copper, and 9 with 10 be mutually nested position relationship；11 be mica sheet, and 12 be shaking table, and 13 be diamond anvil, 11,12 and 13
For stacked position relationship；14 be pad, and 15 be spiral heating wire, and 16 be thermocouple, and 17 be Pneumatic quick connector, and 18 be circulation
Water cavity, 19 be mould on press, and 20 be upper mould cylinder inner wall, and 21 be mould under press, and 22 be W metal+NiO electrodes, and 23 be mineral list
Brilliant sample.
Embodiment：
Different oxygen fugacity in-situ control methods in a kind of diamond anvil cell electrical measurement, it includes：
The making of step 1, oxygen fugacity buffering ring；The preparation method of oxygen fugacity buffering ring described in step 1 includes：
Step 1.1, by metal and its corresponding metal oxide powder according to chemical reaction cushioning balance equation, carry out equal
Even mixing；In order to control the oxygen atmosphere condition in sample cavity, need to consider how to form closing using oxygen fugacity padded coaming
Cavity space.What buffer material was selected is various metals and its corresponds to metal oxide, such as Fe+FeO, Fe+Fe3O4、Ni
+NiO、Cu+CuO、Mo+MoO2Deng.
Step 1.2, mixture of powders will be obtained on hot isostatic press, sinter molding forms cylinder；
Step 1.3, corroded using spark discharge hot-forming metal-Metal oxide cylinder cut into thickness
Spend the thin slice for 60 μm；
Step 1.4, using sand paper by thin slice uniform grinding to thickness be 50 μm；Finally, using laser cutting machine by thin slice
It is cut into oxygen fugacity buffering ring.Annulus internal-and external diameter is respectively 150 μm and 200 μm.Fig. 1 a are precompressed pad and punched that Fig. 1 b are
The insertion of oxygen fugacity buffering ring, Fig. 1 c are the pressing process of sample cavity insulating powder, and Fig. 1 d are the preparation of final sample chamber.
Step 2, utilize oxygen fugacity buffering ring making insulated compound pad；
During superhigh-temperature and-pressure diamond anvil electrical measurement, sample insulation the problem of being very important.Traditional gold
It is the metallic gaskets such as T301 stainless steel substrates, rhenium piece, leaf used in hard rock anvil, between pad, sample and metal electrode
Insulation Problems are always the difficult point in high pressure electricity measurement process.For the present invention in order to solve these problems, spy passes through following methods
To realize.
The method that step 2 makes insulated compound pad using oxygen fugacity buffering ring includes：
Step 2.1, selection T301 stainless steel substrates or rhenium piece make gasket material, with diamond anvil cell precompressed, in pad material
Diamond anvil face pressure trace, diamond anvil chamfering impression and diamond anvil incline impression are outwards pressed with by center on material, is utilized
Laser-beam drilling machine punches at diamond anvil face pressure trace concentric, and the diameter in hole is identical with the external diameter of oxygen fugacity buffering ring and is less than
Diamond anvil face impression diameter；
Step 2.2, oxygen fugacity buffering ring is fixed on concentric circle holes center and applying pressure fixes oxygen fugacity buffering ring；
Step 2.3, by bortz powder, cubic boron nitride powder or alumina powder and epoxy resin it is 4 in mass ratio:1 ratio
Example mixing, is inserted in the hole and all impressions of oxygen fugacity buffering ring after grinding uniformly, then is pressurizeed with diamond anvil cell concentric；
Step 2.4, by the use of burrowing at laser diamond anvil face pressure trace concentric in the third step it is used as sample cavity, sample
The diameter of chamber is less than the internal diameter of oxygen fugacity buffering ring.
The deposition of diamond anvil face different metal-metal oxide：For existing diamond anvil mineral electricity both at home and abroad
(deformation of hand layouts electrode, insulating properties are low, temperature calibration error is larger, means of testing for many defects of e measurement technology
It is single etc.), and the airtight cavity of effectively control oxygen atmosphere is formed, the present invention utilizes thin film deposition and micro-processing technology, in Buddha's warrior attendant
Stone anvil face grows the metal-metallic oxide film corresponding with oxygen fugacity buffering ring.
Step 3, the deposition in diamond anvil face progress different metal-metal oxide, and form electrode configuration；
Step 4, by insulated compound pad and diamond anvil face different metal-metal oxide deposition formed it is closed
Sample cavity.
The deposition of different metal-metal oxide is carried out in diamond anvil face and form electrode configuration method described in step 3
Including：
Step 3.1, diamond surface sputter layer of metal sull；
Step 3.2, layer of metal film is sputtered on metal-oxide film；
Step 3.3, using graphical etching system by metallic film etching be required electrode configuration.
According to the difference of test sample, different electrode configurations is needed in actual measurement process.
The present invention remarks additionally with reference to Fig. 2 to technical solution of the present invention：
The diamond anvil cell package assembly of the present invention is composite structure.Main structure is steel alloy-beryllium copper press, is equipped with
Tungsten carbide shaking table is substrate, use anvil face size for 300 μm diamond produce super-pressure, using external resistance heater strip as
The thermal source of DAC heating, outside cooling is carried out to pressure using recirculated water.Detailed construction is：7 be oxygen buffering ring, and 8 be insulating barrier, 7
It is outer layer and internal layer position relationship with 8.9 be steel alloy, and 10 be beryllium copper, and 9 with 10 be mutually nested position relationship.11 be mica
Piece, 12 be shaking table, and 13 be diamond anvil, and 11,12 and 13 be stacked position relationship.14 be pad, and 15 be spiral heating wire,
16 be thermocouple, and 17 be Pneumatic quick connector, and 18 be circulating water cavity, and 19 be mould on press, and 20 be upper mould cylinder inner wall, and 21 be pressure
Mould under machine, 22 be W metal+NiO electrodes, and 23 be mineral single crystal samples.
By the test, the in-situ control of oxygen fugacity in sample chamber can be achieved, the technology can be widely applied to diamond
The measurement of electrical properties, feasible in opposed anvils.
Claims (4)
1. different oxygen fugacity in-situ control methods in a kind of diamond anvil cell electrical measurement, it includes：
The making of step 1, oxygen fugacity buffering ring；
Step 2, utilize oxygen fugacity buffering ring making insulated compound pad；
Step 3, the deposition in diamond anvil face progress different metal-metal oxide, and form electrode configuration；
Step 4, by insulated compound pad and in the deposition of diamond anvil face different metal-metal oxide form closed sample
Chamber.
2. different oxygen fugacity in-situ control methods in a kind of diamond anvil cell electrical measurement according to claim 1, its
It is characterised by：
The preparation method of oxygen fugacity buffering ring described in step 1 includes：
Step 1.1, by metal and its corresponding metal oxide powder according to chemical reaction cushioning balance equation, uniformly mixed
Close；
Step 1.2, mixture of powders will be obtained, and by means of hot isostatic press high-tension apparatus, carry out Thermocompressed sintering and forming, form circle
Cylinder；
Step 1.3, use spark discharge corrosion that hot-forming metal-metallic oxide cylinder is cut into thickness for 60
μm thin slice；
Step 1.4, using sand paper by thin slice uniform grinding to thickness be 50 μm；Finally, thin slice is cut using laser cutting machine
Circlewise, as oxygen fugacity buffering ring, inner ring radius is 80 μm, and outer shroud radius is 120 μm.
3. different oxygen fugacity in-situ control methods in a kind of diamond anvil cell electrical measurement according to claim 1, its
It is characterised by：The method that step 2 makes insulated compound pad using oxygen fugacity buffering ring includes：
Step 2.1, selection T301 stainless steel substrates or rhenium piece make gasket material, with diamond anvil cell precompressed, on gasket material
Diamond anvil face pressure trace, diamond anvil chamfering impression and diamond anvil incline impression are outwards pressed with by center, utilizes laser
Puncher punches at diamond anvil face pressure trace concentric, and the diameter in hole is identical with the external diameter of oxygen fugacity buffering ring and is less than Buddha's warrior attendant
Stone anvil face impression diameter；
Step 2.2, oxygen fugacity buffering ring is fixed on concentric circle holes center and applying pressure fixes oxygen fugacity buffering ring；
Step 2.3, by bortz powder, cubic boron nitride powder or alumina powder and epoxy resin it is 4 in mass ratio:1 ratio is mixed
Close, inserted after grinding uniformly in the hole and all impressions of oxygen fugacity buffering ring, then pressurizeed with diamond anvil cell concentric；
Step 2.4, by the use of burrowing as sample cavity at laser diamond anvil face pressure trace concentric in the third step, sample cavity
Diameter is less than the internal diameter of oxygen fugacity buffering ring.
4. different oxygen fugacity in-situ control methods in a kind of diamond anvil cell electrical measurement according to claim 1, its
It is characterised by：
The deposition of different metal-metal oxide is carried out in diamond anvil face and form electrode configuration method and include described in step 3：
Step 3.1, diamond surface sputter layer of metal sull；
Step 3.2, layer of metal film is sputtered on metal-oxide film；
Step 3.3, using graphical etching system by metallic film etching be required electrode configuration.
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