CN110031682A - A kind of dielectric spectra measuring device - Google Patents
A kind of dielectric spectra measuring device Download PDFInfo
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- CN110031682A CN110031682A CN201910258976.1A CN201910258976A CN110031682A CN 110031682 A CN110031682 A CN 110031682A CN 201910258976 A CN201910258976 A CN 201910258976A CN 110031682 A CN110031682 A CN 110031682A
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- coaxial cable
- piston
- cavity
- cable
- low
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- 238000001228 spectrum Methods 0.000 title claims abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052802 copper Inorganic materials 0.000 claims abstract description 45
- 239000010949 copper Substances 0.000 claims abstract description 45
- 229910052738 indium Inorganic materials 0.000 claims abstract description 27
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 27
- 235000002991 Coptis groenlandica Nutrition 0.000 claims abstract description 24
- 239000011324 bead Substances 0.000 claims abstract description 21
- 239000003822 epoxy resin Substances 0.000 claims abstract description 19
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 19
- 229910000679 solder Inorganic materials 0.000 claims abstract description 12
- 239000004020 conductor Substances 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims description 27
- 239000002184 metal Substances 0.000 claims description 27
- 244000247747 Coptis groenlandica Species 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 11
- 229910001275 Niobium-titanium Inorganic materials 0.000 claims description 8
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 claims description 8
- 239000003792 electrolyte Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 239000002887 superconductor Substances 0.000 claims description 5
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 238000011160 research Methods 0.000 abstract description 3
- 230000008054 signal transmission Effects 0.000 abstract description 2
- 241000218202 Coptis Species 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- QYHNIMDZIYANJH-UHFFFAOYSA-N diindium Chemical compound [In]#[In] QYHNIMDZIYANJH-UHFFFAOYSA-N 0.000 description 1
- 238000009429 electrical wiring Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
- G01R27/26—Measuring inductance or capacitance; Measuring quality factor, e.g. by using the resonance method; Measuring loss factor; Measuring dielectric constants ; Measuring impedance or related variables
- G01R27/2617—Measuring dielectric properties, e.g. constants
- G01R27/2623—Measuring-systems or electronic circuits
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Measurement Of Resistance Or Impedance (AREA)
Abstract
The present invention relates to new materials to research and develop field, a kind of dielectric spectra measuring device, including low-temperature (low temperature) vessel, sample cavity, pressure chamber, radio frequency adapter I, four coaxial cable I, copper cable I, switching chamber, controller, impedance analyzer and control stick, the inside of hollow piston is full of epoxy resin, so that fixed between four coaxial cable II and four copper cable II and hollow piston, the lower end of four coaxial cable II and four copper cable II is respectively positioned on outside epoxy resin, the outer conductor layer of the lower end of four coaxial cable II interconnects, four coaxial cable II two are one group, the core wire top of every group two lower ends welds together to form solder joint, and the solder joint is wrapped up to form an indium bead with indium, the corresponding two indium beads of two groups of coaxial cable II pass through two that gold thread I is connected to sample surfaces respectively Different location, the upper end of every coaxial cable II are respectively connected with radio frequency adapter II, can apply high pressure to sample, and electric signal transmission keeps preferable high frequency characteristics.
Description
Technical field
The present invention relates to new materials to research and develop field, especially a kind of to apply pressure to material under cryogenic and be situated between
A kind of dielectric spectra measuring device of electrical property measurement.
Background technique
Extraneous pressure enables to the property such as dielectric property of material to change, by different ambient pressures and temperature
The same sample is measured under the conditions of degree, the state diagram that balances each other of measured and monitored the growth of standing timber material can be obtained, this to structure phase transition,
The research of metal-insulator transition, superconductivity etc. is of great significance.In the single crystal samples smaller and frangible to size
When carrying out the dielectric spectrometry of pressure dependence, need for sample to be connected by electrical wiring on a stitch electrode, in measuring device
Be electrically connected and need to have good high frequency characteristics, to obtain the signal that decaying is small, cutoff frequency is high, a kind of solution is
Coaxial cable is embedded into can be in the feedthrough of pressure resistance, but since cable and feedthrough are tubular structure so that being difficult to seal
And it is easily deformed under stress.Moreover, the experiment carried out at a temperature of being lower than 4.2K needs hyperconductive cable that can effectively transmit
High-frequency signal, and the heat transmission between cable and sample stage is reduced, usual cable is made of niobium titanium alloy, the disadvantage is that more difficult
It directly welds, is had in the prior art in titanium and its alloy surface copper coating using bichromate and the hydrofluoric acid of high concentration
Stronger toxicity, a kind of dielectric spectra measuring device are able to solve problem.
Summary of the invention
To solve the above-mentioned problems, the present invention is using copper-plated niobium titanium coaxial cable and special structure by copper wire and together
Shaft cable is guided in pressure chamber, and pressure chamber keeps good leakproofness under the conditions of low-temperature pressure, and coaxial cable has preferably
High frequency characteristics.
The technical scheme adopted by the invention is that:
A kind of dielectric spectra measuring device include low-temperature (low temperature) vessel, sample cavity, pressure chamber, radio frequency adapter I, four it is coaxial
Cable I, copper cable I, switching chamber, controller, impedance analyzer and control stick, xy z are three-dimensional coordinate system, low-temperature (low temperature) vessel
In there is liquid helium, be vacuum state in sample cavity, sample cavity is located in low-temperature (low temperature) vessel, and pressure chamber is located in sample cavity, switching chamber
It is connected to the upper surface of low-temperature (low temperature) vessel and can be separated with low-temperature (low temperature) vessel, control stick sequentially passes through the bottom of low-temperature (low temperature) vessel and sample cavity
Face, all has air-tightness between control stick and low-temperature (low temperature) vessel and sample cavity, controller and impedance analyzer are respectively positioned on low-temperature (low temperature) vessel
Outside；Pressure chamber include pressure screw bolt, piston screw I, cavity, top anvil, piston, metal o-ring I, rubber seal I, sample,
Hollow piston, rubber seal II, metal o-ring II, piston screw II, gold thread I, indium bead, pressure gauge, gold thread II, epoxy
Resin, four copper cable II, low frequency adapter, four coaxial cable II and radio frequency adapter II；Cavity is cylindrical tube and has
There are upper section, middle section and lower section, all has screw thread on the inside of the upper section and lower section of the cavity and internal diameter is 1 centimetre, the chamber
The middle section internal diameter of body is 0.6 centimetre, and piston screw II and piston screw I are threadedly connected to the upper surface of cavity upper section and lower section respectively
Below, piston screw II and piston screw I are longitudinal hollow, and piston screw I has internal screw thread, and pressure screw bolt is rotatably connected
In in piston screw I, top anvil is located at pressure screw bolt upper end；Between the upper section and middle section of cavity successively have metal o-ring II and
Rubber seal II, successively has rubber seal I and metal o-ring I between the middle section and lower section of cavity, piston is located at top
Between anvil and metal o-ring I, for hollow piston between piston screw II and metal o-ring II, hollow piston is hollow
Class is round table-like, and the upper bottom surface diameter of hollow piston is 0.8 centimetre, bottom surface diameter is 0.6 centimetre, internal diameter is 0.4 centimetre；Sample
In the middle section of cavity, it is filled with the pressure medium of liquid in the middle section of cavity, control stick rotational pressure screw rod can be passed through
And top anvil and piston are moved up, so as to which pressure is applied on sample by pressure medium；Four coaxial cables
From top to bottom through the inside of hollow piston, four coaxial cable II successively have II and four copper cable II from outside to inside
There are external protection, outer conductor layer, electrolyte layer and a core wire, the upper end of every copper cable II is respectively connected with low frequency adapter, wherein
The lower end of two copper cable II is by gold thread II connection pressure gauge, and low frequency adapter is by copper cable I through switching chamber connection control
Device, controller can read the pressure value that manometry obtains；The upper end of four coaxial cable I is separately connected resistance through switching chamber
Analysis resistant instrument, lower end are connected separately with radio frequency adapter I；The inside of hollow piston is full of epoxy resin, so that four coaxial electricals
Fixed between cable II and four copper cable II and hollow piston, the lower end of four coaxial cable II and four copper cable II are respectively positioned on
Outside epoxy resin, the outer conductor layer of the lower end of four coaxial cable II is interconnected, and four coaxial cable II two are one group, often
The core wire top of two lower ends of group welds together to form solder joint, and with indium that solder joint package is small to form an indium
Ball, the corresponding two indium beads of two groups of coaxial cable II pass through two different locations that gold thread I is connected to sample surfaces respectively, often
The upper end of root coaxial cable II is respectively connected with radio frequency adapter II, and radio frequency adapter II can connect radio frequency adapter I, and four same
The core wire of shaft cable II is made of niobium titanium superconductor.
The beneficial effects of the present invention are:
Apparatus of the present invention can apply the pressure of highest 10kPa, sample and impedance analyzer to sample under cryogenic
Between electric signal transmission maintain preferable high frequency characteristics.
Detailed description of the invention
It is further illustrated below with reference to figure of the invention:
Fig. 1 is schematic diagram of the present invention；
Fig. 2 is pressure chamber sectional view；
Fig. 3 is sample and hollow piston partial enlargement diagram.
In figure, 1. low-temperature (low temperature) vessels, 2. sample cavities, 3. pressure chambers, 3-1. pressure screw bolt, 3-2. piston screw I, 3-3. chamber
Body, 3-4. push up anvil, 3-5. piston, 3-6. metal o-ring I, 3-7. rubber seal I, 3-8. sample, 3-9. hollow piston, 3-
10. rubber seal II, 3-11. metal o-ring II, 3-12. piston screw II, 3-13. gold thread I, 3-14. indium bead, 3-
15. pressure gauge, 3-16. gold thread II, 3-17. epoxy resin, tetra- copper cable II, 3-19. low frequency adapters of 3-18., 3-20. tetra-
Root coaxial cable II, 3-21. radio frequency adapter II, 4. radio frequency adapter I, 5. 4 coaxial cable I, 6. copper cable I, 7. transfer
Chamber, 8. controllers, 9. impedance analyzers, 10. control sticks.
Specific embodiment
If Fig. 1 is schematic diagram of the present invention, including low-temperature (low temperature) vessel (1), sample cavity (2), pressure chamber (3), radio frequency adapter I
(4), four coaxial cable I (5), copper cable I (6), switching chamber (7), controller (8), impedance analyzer (9) and control stick
(10), xy z is three-dimensional coordinate system, has liquid helium in low-temperature (low temperature) vessel (1), is vacuum state, sample cavity in sample cavity (2)
(2) it is located in low-temperature (low temperature) vessel (1), pressure chamber (3) is located in sample cavity (2), and switching chamber (7) is connected to the upper of low-temperature (low temperature) vessel (1)
It face and can be separated with low-temperature (low temperature) vessel (1), control stick (10) sequentially passes through the bottom surface of low-temperature (low temperature) vessel (1) and sample cavity (2), manipulation
Air-tightness is all had between bar (10) and low-temperature (low temperature) vessel (1) and sample cavity (2), controller (8) and impedance analyzer (9) are respectively positioned on
Low-temperature (low temperature) vessel (1) is outside.
If Fig. 2 is pressure chamber sectional view, if Fig. 3 is sample and hollow piston partial enlargement diagram, pressure chamber (3) includes
Pressure screw bolt (3-1), piston screw I (3-2), cavity (3-3), top anvil (3-4), piston (3-5), metal o-ring I (3-6),
Rubber seal I (3-7), sample (3-8), hollow piston (3-9), rubber seal II (3-10), metal o-ring II (3-
11), piston screw II (3-12), gold thread I (3-13), indium bead (3-14), pressure gauge (3-15), gold thread II (3-16), epoxy
Resin (3-17), four copper cable II (3-18), low frequency adapter (3-19), four coaxial cable II (3-20) and RF repeating
Head II (3-21)；Cavity (3-3) is cylindrical tube and has upper section, middle section and lower section, the upper section and lower section of the cavity (3-3)
Inside all have screw thread and internal diameter is 1 centimetre, the middle section internal diameter of the cavity (3-3) is 0.6 centimetre, piston screw II
(3-12) and piston screw I (3-2) are threadedly connected to respectively below the upper surface of cavity (3-3) upper section and lower section, piston screw
II (3-12) and piston screw I (3-2) is longitudinal hollow, and piston screw I (3-2) has internal screw thread, and pressure screw bolt (3-1) can revolve
Turn to be connected in piston screw I (3-2), top anvil (3-4) is located at the upper end pressure screw bolt (3-1)；The upper section of cavity (3-3) and middle section
Between successively have metal o-ring II (3-11) and rubber seal II (3-10), between the middle section and lower section of cavity (3-3)
Successively there is rubber seal I (3-7) and metal o-ring I (3-6), piston (3-5) is located at top anvil (3-4) and metal o-ring
Between I (3-6), hollow piston (3-9) is located between piston screw II (3-12) and metal o-ring II (3-11), hollow piston
(3-9) is that hollow class is round table-like, the upper bottom surface diameter of hollow piston (3-9) is 0.8 centimetre, bottom surface diameter is 0.6 centimetre,
Internal diameter is 0.4 centimetre；Sample (3-8) is located in the middle section of cavity (3-3), and the pressure of liquid is filled in the middle section of cavity (3-3)
Power medium can pass through control stick (10) rotational pressure screw rod (3-1) and top anvil (3-4) and piston (3-5) are moved up,
So as to which pressure is applied on sample (3-8) by pressure medium；Four coaxial cable II (3-20) Ji Sigen copper cables
II (3-18) from top to bottom through the inside of hollow piston (3-9), four coaxial cable II (3-20) from outside to inside according to
Secondary to have external protection, outer conductor layer, electrolyte layer and core wire, the core wire is made of niobium titanium superconductor, and every coaxial
The upper end of cable II (3-20) is respectively connected with radio frequency adapter II (3-21), and the upper end of every copper cable II (3-18) is respectively connected with
The lower end of low frequency adapter (3-19), wherein two copper cable II (3-18) connects pressure gauge (3- by gold thread II (3-16)
15), by copper cable I (6) through switching chamber (7) connection controller (8), controller (8) can be read low frequency adapter (3-19)
Pressure gauge (3-15) measures obtained pressure value；The inside of hollow piston (3-9) is full of epoxy resin (3-17), such as the void of Fig. 3
Line range is epoxy resin (3-17), so that four coaxial cable II (3-20) Ji Sigen copper cable II (3-18) and hollow piston
Fixed between (3-9), the lower end of four coaxial cable II (3-20) Ji Sigen copper cable II (3-18) is respectively positioned on epoxy resin (3-
17) outside, the outer conductor layer of the lower end of four coaxial cable II (3-20) interconnects, and four coaxial cable II (3-20) two are
One group, the top of the core wire of every group of two lower ends welds together to form solder joint, and is wrapped up the solder joint to be formed with indium
One indium bead (3-14), the corresponding two indium beads (3-14) of two groups of coaxial cable II (3-20) pass through gold thread I (3- respectively
13) two different locations on the surface sample (3-8) are connected to；The upper end of four coaxial cable I (5) connects respectively through switching chamber (7)
Connect impedance analyzer (9), lower end is connected separately with radio frequency adapter I (4), radio frequency adapter II (3-21) can connect radio frequency turn
Connector I (4).
A kind of dielectric spectra measuring device includes low-temperature (low temperature) vessel (1), sample cavity (2), pressure chamber (3), radio frequency adapter I
(4), four coaxial cable I (5), copper cable I (6), switching chamber (7), controller (8), impedance analyzer (9) and control stick
(10), xy z is three-dimensional coordinate system, has liquid helium in low-temperature (low temperature) vessel (1), is vacuum state, sample cavity in sample cavity (2)
(2) it is located in low-temperature (low temperature) vessel (1), pressure chamber (3) is located in sample cavity (2), and switching chamber (7) is connected to the upper of low-temperature (low temperature) vessel (1)
It face and can be separated with low-temperature (low temperature) vessel (1), control stick (10) sequentially passes through the bottom surface of low-temperature (low temperature) vessel (1) and sample cavity (2), manipulation
Air-tightness is all had between bar (10) and low-temperature (low temperature) vessel (1) and sample cavity (2), controller (8) and impedance analyzer (9) are respectively positioned on
Low-temperature (low temperature) vessel (1) is outside；Pressure chamber (3) include pressure screw bolt (3-1), piston screw I (3-2), cavity (3-3), top anvil (3-4),
Piston (3-5), metal o-ring I (3-6), rubber seal I (3-7), sample (3-8), hollow piston (3-9), rubber seal
Enclose II (3-10), metal o-ring II (3-11), piston screw II (3-12), gold thread I (3-13), indium bead (3-14), pressure
Count (3-15), gold thread II (3-16), epoxy resin (3-17), four copper cable II (3-18), low frequency adapter (3-19), four
Coaxial cable II (3-20) and radio frequency adapter II (3-21)；Cavity (3-3) be cylindrical tube and have upper section, middle section and under
Section, screw thread is all had on the inside of the upper section and lower section of the cavity (3-3) and internal diameter is 1 centimetre, in the cavity (3-3)
Section internal diameter is 0.6 centimetre, and piston screw II (3-12) and piston screw I (3-2) are threadedly connected to cavity (3-3) upper section respectively
Above and below lower section, piston screw II (3-12) and piston screw I (3-2) are longitudinal hollow, piston screw I (3-2) tool
There is internal screw thread, pressure screw bolt (3-1) is rotatably connected in piston screw I (3-2), and top anvil (3-4) is located at pressure screw bolt (3-1)
Upper end；Successively there is metal o-ring II (3-11) and rubber seal II (3-10) between the upper section and middle section of cavity (3-3),
Successively there is rubber seal I (3-7) and metal o-ring I (3-6), piston (3-5) between the middle section and lower section of cavity (3-3)
Between top anvil (3-4) and metal o-ring I (3-6), hollow piston (3-9) is located at piston screw II (3-12) and metal is close
Between seal II (3-11), hollow piston (3-9) is that hollow class is round table-like, and the upper bottom surface diameter of hollow piston (3-9) is 0.8
Centimetre, bottom surface diameter be 0.6 centimetre, internal diameter is 0.4 centimetre；Sample (3-8) is located in the middle section of cavity (3-3), cavity (3-
3) it is filled with the pressure medium of liquid in middle section, control stick (10) rotational pressure screw rod (3-1) can be passed through and to push up anvil
(3-4) and piston (3-5) move up, so as to which pressure to be applied on sample (3-8) by pressure medium；Four coaxial
For cable II (3-20) Ji Sigen copper cable II (3-18) from top to bottom through the inside of hollow piston (3-9), four coaxial
Cable II (3-20) successively has external protection, outer conductor layer, electrolyte layer and core wire, every copper cable II from outside to inside
The upper end of (3-18) be respectively connected with low frequency adapter (3-19), wherein two copper cable II (3-18) lower end by gold thread II
(3-16) connects pressure gauge (3-15), and low frequency adapter (3-19) connects controller through switching chamber (7) by copper cable I (6)
(8), controller (8) can read pressure gauge (3-15) and measure obtained pressure value；The upper end of four coaxial cable I (5) is through turning
Connect that chamber (7) is separately connected impedance analyzer (9), lower end is connected separately with radio frequency adapter I (4)；The inside of hollow piston (3-9)
Full of epoxy resin (3-17), so that four coaxial cable II (3-20) Ji Sigen copper cable II (3-18) and hollow piston 3-9)
Between it is fixed, the lower end of four coaxial cable II (3-20) Ji Sigen copper cable II (3-18) is respectively positioned on epoxy resin (3-17)
Outside, the outer conductor layer of the lower end of four coaxial cable II (3-20) interconnects, and four coaxial cable II (3-20) two are one
Group, the core wire top of every group of two lower ends weld together to form solder joint, and are wrapped up the solder joint to form one with indium
Indium bead (3-14), the corresponding two indium beads (3-14) of two groups of coaxial cable II (3-20) are connected by gold thread I (3-13) respectively
Two different locations on the surface sample (3-8) are connected to, the upper end of every coaxial cable II (3-20) is respectively connected with radio frequency adapter
II (3-21), radio frequency adapter II (3-21) can be connected radio frequency adapter I (4), the core wire of four coaxial cable II (3-20)
It is made of niobium titanium superconductor.
The electroplating process of the core wire of superconductor coaxial cable and the step of connect the method for radio-frequency joint are as follows:
Two electrolytic cells are used to the electroplating process of the core wire of coaxial cable II (3-20), each electrolytic cell all has anode
And cathode has acid copper sulphate molten wherein having basic oxidation solution in first electrolytic cell in second electrolytic cell
Liquid,
Step 1, so that the both ends coaxial cable II (3-20) respectively have the core wire exposing of 1 centimetre length to lead in external protection, outside
Except body layer and electrolyte layer, cleaning and degreasing are carried out to the core wire surface at the both ends coaxial cable II (3-20)；
Step 2, the core wire being electroplated will be needed to be placed in the sodium hydrate aqueous solution of 110 grams per liters in first electrolytic cell
In first electrolytic cell, core wire is connected to anode, and using a copper sheet as cathode, distance is 5 lis between copper sheet and core wire
Rice, applies voltage 5.5V, and the duration 20 seconds, then apply voltage 11V, the duration 40 seconds, so that 30 nano-oxide layer of thickness
It is deposited on core wire surface, in the process, the color on core wire surface made of niobium titanium material is changed into dark yellow from grey；
Step 3, the core wire for the coaxial cable II (3-20) that deposited oxide layer is rinsed in deionized water, and quickly turned
It moves on in second electrolytic cell；
It step 4, is the copper-bath of 250 grams per liters with concentration in second electrolytic cell, coaxial cable II's (3-20)
Core wire connects cathode, applies voltage 6V, continues 200 seconds, so that copper deposition is to the core wire surface of coaxial cable II (3-20)；
Step 5, the core wire of the upper end coaxial cable II (3-20) is welded on radio frequency adapter II (3-21).
The step of method that cable is drawn on sample (3-8) in pressure chamber (3) are as follows:
Four coaxial cable II (3-20) Ji Sigen copper cable II (3-18) are penetrated hollow piston by step 1 from top to bottom
In (3-9)；
The epoxy resin (3-17) of pressure resistance is filled into hollow piston (3-9) with fixed copper cable II (3- by step 2
And coaxial cable II (3-20) 18)；
The outer conductor layer of the lower end of four coaxial cable II (3-20) is mutually connected by step 3 using a silver-coated copper wire
It connects；
Step 4, four coaxial cable II (3-20) are divided into two groups, two coaxial cable II (3-20) lower ends in every group
The top of core wire weld together to form solder joint, and the solder joint is wrapped up to form an indium bead (3-14) with indium,
I.e. two groups of coaxial cable II (3-20) form two indium beads (3-14) altogether；
Step 5 further wraps up the lower end coaxial cable II (3-20) using epoxy resin (3-17), it is ensured that coaxial cable
The outer conductor layer and electrolyte layer of II (3-20) is wrapped up, and two indium beads (3-14) are not wrapped up, so that coaxial cable
The sealing of the lower end II (3-20) is able to bear biggish pressure, and reduces the size of the lower end coaxial cable II (3-20), this is to same
Measuring signal in shaft cable II (3-20) has good shielding, to promote high frequency characteristics；
Step 6 deposits indium on two indium beads (3-14) again after epoxy resin (3-17) is fully cured, so that
The diameter of indium bead (3-14) is 1 millimeter；
Step 7, two indium beads (3-14) are connected to two of the surface sample (3-8) not by gold thread I (3-13) respectively
Same position is used as adhesive, indium bead (3-14) and gold thread I (3-13) by carbon paste between gold thread I (3-13) and sample (3-8)
Between by elargol as adhesive.
Use a kind of method and step of dielectric spectra measuring device progress dielectric material spectrometry are as follows:
One, sample (3-8) is passed sequentially through using above-mentioned " method that cable is drawn on sample (3-8) in pressure chamber (3) "
Gold thread I (3-13), indium bead (3-14) and coaxial cable II (3-20) are connected to radio frequency adapter II (3-21), by pressure gauge
(3-15) passes sequentially through gold thread II (3-16), copper cable II (3-18), low frequency adapter (3-19) and copper cable I (6) connection control
Device (8) processed；
Two, sample (3-8) is placed in the middle section of cavity (3-3), the pressure medium of liquid is added simultaneously in cavity (3-3)
So that it is full of the middle section of cavity (3-3), and hollow piston (3-9) is fixed on piston screw II (3-12) and metal o-ring II
Between (3-11)；
Three, pressure chamber (3) is placed in sample cavity (2), radio frequency adapter II (3-21) is connected to radio frequency adapter I
(4), switching chamber (7) is connected to the upper surface of low-temperature (low temperature) vessel (1)；
Four, liquid helium is added into low-temperature (low temperature) vessel (1) to cool down to sample cavity (2)；
Five, pass through control stick (10) rotational pressure screw rod (3-1) and top anvil (3-4) and piston (3-5) are moved up,
To which pressure to be applied on sample (3-8) by pressure medium, born by pressure gauge (3-15) measurement sample (3-8)
Pressure；
Six, pass through the dielectric spectra of impedance analyzer (9) measurement sample (3-8):
Seven, the position on top anvil (3-4) and piston (3-5) is finely tuned by control stick (10) rotational pressure screw rod (3-1), is changed
Become the pressure being applied on sample (3-8), and passes through Jie of impedance analyzer (9) measurement sample (3-8) under the pressure condition
Electricity spectrum, and the duplicate measurements under multiple pressure conditions；
Eight, the dielectric spectra that impedance analyzer (9) measures under different sample (3-8) pressure conditions is analyzed, sample is finally obtained
The relationship between pressure that the dielectric spectra and sample (3-8) of (3-8) are born.
There is apparatus of the present invention special structure to guide to copper wire and niobium titanium coaxial cable in pressure chamber, so that pressure chamber
There is good leakproofness under low temperature and condition of high voltage, and coaxial cable has preferable high frequency characteristics.
Claims (2)
1. a kind of dielectric spectra measuring device, including low-temperature (low temperature) vessel (1), sample cavity (2), pressure chamber (3), radio frequency adapter I (4),
Four coaxial cable I (5), copper cable I (6), switching chamber (7), controller (8), impedance analyzer (9) and control stick (10), xyz
For three-dimensional coordinate system, there is liquid helium in low-temperature (low temperature) vessel (1), be vacuum state in sample cavity (2), sample cavity (2) is located at low
In warm container (1), pressure chamber (3) is located in sample cavity (2), transfer chamber (7) be connected to the upper surface of low-temperature (low temperature) vessel (1) and can be with
Low-temperature (low temperature) vessel (1) separation, control stick (10) sequentially pass through the bottom surface of low-temperature (low temperature) vessel (1) and sample cavity (2), control stick (10) with it is low
Air-tightness is all had between warm container (1) and sample cavity (2), controller (8) and impedance analyzer (9) are respectively positioned on low-temperature (low temperature) vessel
(1) outside；Pressure chamber (3) includes pressure screw bolt (3-1), piston screw I (3-2), cavity (3-3), top anvil (3-4), piston (3-
5), metal o-ring I (3-6), rubber seal I (3-7), sample (3-8), hollow piston (3-9), rubber seal II (3-
10), metal o-ring II (3-11), piston screw II (3-12), gold thread I (3-13), indium bead (3-14), pressure gauge (3-
15), gold thread II (3-16), epoxy resin (3-17), four copper cable II (3-18), low frequency adapter (3-19), four it is coaxial
Cable II (3-20) and radio frequency adapter II (3-21)；Cavity (3-3) is cylindrical tube and has upper section, middle section and lower section, institute
It states and all has screw thread on the inside of the upper section and lower section of cavity (3-3) and internal diameter is 1 centimetre, in the middle section of the cavity (3-3)
Diameter is 0.6 centimetre, and piston screw II (3-12) and piston screw I (3-2) are threadedly connected to the upper surface of cavity (3-3) upper section respectively
Below lower section, piston screw II (3-12) and piston screw I (3-2) are longitudinal hollow, and piston screw I (3-2) has interior
Screw thread, pressure screw bolt (3-1) are rotatably connected in piston screw I (3-2), and top anvil (3-4) is located on pressure screw bolt (3-1)
End；Successively there is metal o-ring II (3-11) and rubber seal II (3-10), chamber between the upper section and middle section of cavity (3-3)
Successively there is rubber seal I (3-7) and metal o-ring I (3-6), the position piston (3-5) between the middle section and lower section of body (3-3)
Between top anvil (3-4) and metal o-ring I (3-6), hollow piston (3-9) is located at piston screw II (3-12) and metal sealing
It encloses between II (3-11), hollow piston (3-9) is that hollow class is round table-like, and the upper bottom surface diameter of hollow piston (3-9) is 0.8 li
Rice, bottom surface diameter are 0.6 centimetre, internal diameter is 0.4 centimetre；Sample (3-8) is located in the middle section of cavity (3-3), cavity (3-3)
Middle section in be filled with the pressure medium of liquid, control stick (10) rotational pressure screw rod (3-1) can be passed through and to push up anvil (3-
4) and piston (3-5) moves up, so as to which pressure to be applied on sample (3-8) by pressure medium；Four coaxial electricals
Cable II (3-20) Ji Sigen copper cable II (3-18) is from top to bottom through the inside of hollow piston (3-9), four coaxial electricals
Cable II (3-20) successively has external protection, outer conductor layer, electrolyte layer and core wire, every copper cable II (3- from outside to inside
18) upper end be respectively connected with low frequency adapter (3-19), wherein two copper cable II (3-18) lower end by gold thread II (3-
16) pressure gauge (3-15) is connected, low frequency adapter (3-19) is by copper cable I (6) through switching chamber (7) connection controller (8), control
Device (8) processed can read pressure gauge (3-15) and measure obtained pressure value；The upper end of four coaxial cable I (5) is through transferring chamber (7)
Be separately connected impedance analyzer (9), lower end is connected separately with radio frequency adapter I (4),
It is characterized in that: the inside of hollow piston (3-9) be full of epoxy resin (3-17) so that four coaxial cable II (3-20) and
It is fixed between four copper cable II (3-18) and hollow piston (3-9), four coaxial cable II (3-20) Ji Sigen copper cable II
The lower end of (3-18) is respectively positioned on epoxy resin (3-17) outside, and the outer conductor layer of the lower end of four coaxial cable II (3-20) is mutually connected
It connects, four coaxial cable II (3-20) two are one group, and the core wire top of every group of two lower ends welds together to form solder joint,
And wrapped up the solder joint to form an indium bead (3-14) with indium, corresponding two indiums of two groups of coaxial cable II (3-20) are small
Ball (3-14) is connected to two different locations on the surface sample (3-8), every coaxial cable II by gold thread I (3-13) respectively
The upper end of (3-20) is respectively connected with radio frequency adapter II (3-21), and radio frequency adapter II (3-21) can connect radio frequency adapter I
(4)。
2. a kind of dielectric spectra measuring device according to claim 1, it is characterized in that: the core of four coaxial cable II (3-20)
Line is made of niobium titanium superconductor.
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| CN110007153A (en) * | 2019-03-22 | 2019-07-12 | 金华职业技术学院 | A kind of method of dielectric material spectrometry |
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