CN110031683B - Processing method of pressure cavity for dielectric spectrum measurement under low temperature condition - Google Patents
Processing method of pressure cavity for dielectric spectrum measurement under low temperature condition Download PDFInfo
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- CN110031683B CN110031683B CN201910258977.6A CN201910258977A CN110031683B CN 110031683 B CN110031683 B CN 110031683B CN 201910258977 A CN201910258977 A CN 201910258977A CN 110031683 B CN110031683 B CN 110031683B
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- 238000001453 impedance spectrum Methods 0.000 title claims abstract description 16
- 238000003672 processing method Methods 0.000 title claims abstract description 11
- 238000005259 measurement Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 66
- 229910052802 copper Inorganic materials 0.000 claims description 62
- 239000010949 copper Substances 0.000 claims description 62
- 229910052738 indium Inorganic materials 0.000 claims description 40
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 40
- 238000007789 sealing Methods 0.000 claims description 39
- 239000010410 layer Substances 0.000 claims description 33
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 28
- 229910052751 metal Inorganic materials 0.000 claims description 27
- 239000002184 metal Substances 0.000 claims description 27
- 239000003822 epoxy resin Substances 0.000 claims description 23
- 229920000647 polyepoxide Polymers 0.000 claims description 23
- 238000003466 welding Methods 0.000 claims description 23
- 239000008188 pellet Substances 0.000 claims description 21
- 239000004020 conductor Substances 0.000 claims description 17
- 229910052737 gold Inorganic materials 0.000 claims description 16
- 239000010931 gold Substances 0.000 claims description 16
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 claims description 11
- 229910001275 Niobium-titanium Inorganic materials 0.000 claims description 10
- 239000003792 electrolyte Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000009713 electroplating Methods 0.000 claims description 9
- 239000011241 protective layer Substances 0.000 claims description 7
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000005238 degreasing Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000012827 research and development Methods 0.000 abstract description 2
- 229910000831 Steel Inorganic materials 0.000 description 5
- 238000007747 plating Methods 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 241000218202 Coptis Species 0.000 description 2
- 235000002991 Coptis groenlandica Nutrition 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001419 dependent effect 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
- 238000002474 experimental method Methods 0.000 description 1
- 238000001566 impedance spectroscopy Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000008054 signal transmission Effects 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0607—Wires
-
- 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
- G01R27/2635—Sample holders, electrodes or excitation arrangements, e.g. sensors or measuring cells
- G01R27/2658—Cavities, resonators, free space arrangements, reflexion or interference arrangements
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- 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 invention relates to the field of new material research and development, in particular to a processing method of a pressure cavity for dielectric spectrum measurement under low temperature conditions, which is a processing method of a device for measuring dielectric properties of materials under low temperature and high pressure conditions, and comprises a method for connecting a core wire of a superconducting cable with a radio frequency connector and a method for leading out a cable on a sample in the pressure cavity.
Description
Technical Field
The invention relates to the field of new material research and development, in particular to a processing method of a pressure cavity for dielectric spectrum measurement under low temperature and high pressure conditions, which is a processing method of a device for measuring dielectric properties of materials.
Background
The external pressure can change the properties of the material such as dielectric property, and the phase equilibrium state diagram of the measured material can be obtained by measuring the same sample under different external pressure and temperature conditions, which has important significance in the research of structural phase transformation, metal-insulator transformation, superconductivity and the like. In pressure-dependent dielectric spectroscopy of small and fragile single crystal samples, where the sample is to be connected to a pin electrode by wire, the electrical connection in the measuring device needs to have good high frequency characteristics to obtain a signal with reduced attenuation and high cut-off frequency, one solution is to embed the coaxial cable in a pressure-resistant feedthrough, but because both the cable and the feedthrough are tubular structures that are difficult to seal and are easily deformed under pressure. Moreover, experiments performed at temperatures below 4.2K require that the superconducting cable can effectively transmit high frequency signals and reduce heat transmission between the cable and the sample stage, and the cable is generally made of niobium-titanium alloy, which has the disadvantage of being difficult to directly weld, and the copper plating method on the surface of titanium and the alloy thereof in the prior art adopts dichromate and high-concentration hydrofluoric acid, which has stronger toxicity, and the processing method of the pressure cavity for dielectric spectrum measurement under the low-temperature condition can solve the problems.
Disclosure of Invention
In order to solve the problems, the special copper plating method of the niobium-titanium coaxial cable is adopted to solve the welding problem between the coaxial cable core wire and the radio frequency adapter, the copper plating process is safe and simple, and a special connection mode is adopted to communicate a sample in the pressure cavity with an impedance analyzer outside the pressure cavity, so that the transmission of signals in the cable has good high-frequency characteristics on the basis of ensuring the tightness of the pressure cavity.
The technical scheme adopted by the invention is as follows:
The dielectric spectrum measuring device comprises a low-temperature container, a sample cavity, a pressure cavity, a radio frequency adapter I, four coaxial cables I, a copper cable I, an adapter cavity, a controller, an impedance analyzer and an operating rod, wherein xyz is a three-dimensional space coordinate system, liquid helium is arranged in the low-temperature container, the sample cavity is in a vacuum state, the sample cavity is positioned in the low-temperature container, the pressure cavity is positioned in the sample cavity, the adapter cavity is connected to the upper surface of the low-temperature container and can be separated from the low-temperature container, the operating rod sequentially penetrates through the bottom surfaces of the low-temperature container and the sample cavity, air tightness is arranged between the operating rod and the low-temperature container and between the operating rod and the sample cavity, and the controller and the impedance analyzer are positioned outside the low-temperature container; the pressure cavity comprises a pressure screw, a piston screw I, a cavity body, a top anvil, a piston, a metal sealing ring I, a rubber sealing ring I, a sample, a hollow piston, a rubber sealing ring II, a metal sealing ring II, a piston screw II, a gold thread I, a steel ball, a pressure gauge, a gold thread II, epoxy resin, four copper cables II, a low-frequency adapter, four coaxial cables II and a radio frequency adapter II; The cavity is cylindrical and tubular and is provided with an upper section, a middle section and a lower section, the inner sides of the upper section and the lower section of the cavity are provided with threads, the inner diameter of the middle section of the cavity is 0.6 cm, a piston screw II and a piston screw I are respectively connected below the upper section and the lower section of the cavity in a threaded manner, the piston screw II and the piston screw I are both hollow longitudinally, the piston screw I is provided with internal threads, a pressure screw rod is rotatably connected in the piston screw I, and a top anvil is positioned at the upper end of the pressure screw rod; a metal sealing ring II and a rubber sealing ring II are sequentially arranged between the upper section and the middle section of the cavity, a rubber sealing ring I and a metal sealing ring I are sequentially arranged between the middle section and the lower section of the cavity, a piston is positioned between the top anvil and the metal sealing ring I, a hollow piston is positioned between a piston screw II and the metal sealing ring II, the hollow piston is in a hollow truncated cone-like shape, the diameter of the upper bottom surface of the hollow piston is 0.8 cm, the diameter of the lower bottom surface of the hollow piston is 0.6 cm, and the inner diameter of the hollow piston is 0.4 cm; The sample is positioned in the middle section of the cavity, the middle section of the cavity is filled with liquid pressure medium, the pressure screw rod can be rotated through the control rod, and the anvil and the piston can be moved upwards, so that pressure can be applied to the sample through the pressure medium; the four coaxial cables II and the four copper cables II penetrate through the hollow piston from top to bottom, the four coaxial cables II are sequentially provided with an outer protective layer, an outer conductor layer, an electrolyte layer and a core wire from outside to inside, the upper end of each copper cable II is connected with a low-frequency adapter, the lower ends of the two copper cables II are connected with a pressure gauge through gold wires II, the low-frequency adapter is connected with a controller through a copper cable I through an adapter cavity, and the controller can read a pressure value measured by the pressure gauge; the upper ends of the four coaxial cables I are respectively connected with an impedance analyzer through the switching cavity, and the lower ends of the four coaxial cables I are respectively connected with a radio frequency switching connector I; The inside of the hollow piston is filled with epoxy resin, so that four coaxial cables II and four copper cables II are fixed with the hollow piston, the lower ends of the four coaxial cables II and the four copper cables II are all positioned outside the epoxy resin, the outer conductor layers of the lower ends of the four coaxial cables II are connected with each other, two coaxial cables II are in a group, the core wire top ends of the two lower ends of each group are welded together to form welding spots, the welding spots are wrapped by indium to form an indium small ball, the two indium small balls corresponding to the two groups of coaxial cables II are respectively connected to two different positions on the surface of a sample through gold wires I, the upper end of each coaxial cable II is connected with a radio frequency adapter II, the radio frequency adapter II can be connected with the radio frequency adapter I, and core wires of the four coaxial cables II are all made of niobium-titanium superconducting materials.
The processing method of the pressure cavity for dielectric spectrum measurement under the low temperature condition comprises an electroplating process of a core wire of a superconducting cable, a method for connecting a radio frequency connector and a method for leading out a cable on a sample in the pressure cavity.
The electroplating process of the core wire of the superconducting coaxial cable and the method for connecting the radio frequency connector comprise the following steps:
the electroplating process for the core wire of the coaxial cable II employs two electrolytic cells, each having an anode and a cathode, wherein the first cell has a basic oxidizing solution therein, the second cell has an acidic copper sulfate solution therein,
Step 1, enabling core wires with the length of 1 cm at two ends of a coaxial cable II to be exposed out of an outer protective layer, an outer conductor layer and an electrolyte layer, and cleaning and degreasing the surfaces of the core wires at two ends of the coaxial cable II;
step 2, placing a core wire to be electroplated in a first electrolytic cell, wherein the core wire is provided with a 110 g/L sodium hydroxide aqueous solution, the core wire is connected to an anode, a copper sheet is adopted as a cathode, the distance between the copper sheet and the core wire is 5 cm, a voltage of 5.5V is applied for 20 seconds, a voltage of 11V is applied for 40 seconds, so that a 30-nanometer oxide layer is deposited on the surface of the core wire, and in the process, the color of the surface of the core wire made of a niobium-titanium material is changed from gray to dark yellow;
step 3, flushing the core wire of the coaxial cable II deposited with the oxide layer in deionized water, and rapidly transferring the core wire into a second electrolytic cell;
Step 4, a copper sulfate solution with the concentration of 250 g/L is arranged in the second electrolytic cell, the core wire of the coaxial cable II is connected with the cathode, and the voltage is applied for 200 seconds by 6V, so that copper is deposited on the surface of the core wire of the coaxial cable II;
and 5, welding the core wire at the upper end of the coaxial cable II to the radio frequency adapter II by adopting a common welding method.
The method for leading out the cable on the sample in the pressure cavity comprises the following steps:
Step one, penetrating four coaxial cables II and four copper cables II into a hollow piston from top to bottom;
Filling pressure-resistant epoxy resin into the hollow piston to fix the copper cable II and the coaxial cable II;
step three, adopting a silver-plated copper wire to connect the outer conductor layers at the lower ends of the four coaxial cables II;
dividing four coaxial cables II into two groups, welding the top ends of core wires at the lower ends of the two coaxial cables II in each group together to form welding spots, and wrapping the welding spots by indium to form an indium pellet, namely forming two indium pellets by the two groups of coaxial cables II;
Step five, the lower end of the coaxial cable II is further wrapped by epoxy resin, so that the outer conductor layer and the electrolyte layer of the coaxial cable II are wrapped, and the two indium pellets are not wrapped, so that the sealing of the lower end of the coaxial cable II can bear larger pressure, the size of the lower end of the coaxial cable II is reduced, and the measuring signal in the coaxial cable II has good shielding property, and therefore the high-frequency characteristic is improved;
Step six, after the epoxy resin is completely cured, depositing indium on the two indium pellets again, so that the diameter of the indium pellets is 1 mm;
And seventhly, connecting the two indium pellets to two different positions on the surface of the sample through gold wires I, wherein carbon paste is used as an adhesive between the gold wires I and the sample, and silver paste is used as an adhesive between the indium pellets and the gold wires I.
The beneficial effects of the invention are as follows:
The invention adopts a special copper plating method of the niobium-titanium coaxial cable to improve the connection between the superconducting cable and the radio frequency adapter, the copper plating process is safe and nontoxic, the operation is simple and convenient, and the copper wire and the coaxial cable are led into the pressure cavity by adopting the special method, so that the tightness of the pressure cavity is maintained, and the high-frequency characteristic of the coaxial cable is better.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic illustration of the present invention;
FIG. 2 is a cross-sectional view of a pressure chamber;
fig. 3 is a partially enlarged schematic view of a sample and hollow piston.
In the figure, 1 part of the low-temperature container, 2 parts of the sample cavity, 3 parts of the pressure screw, 3 parts of the piston screw I,3 parts of the cavity, 3 parts of the top anvil, 3 parts of the piston, 3 parts of the metal seal ring I,3 parts of the rubber seal ring I,3 parts of the sample, 3 parts of the hollow piston, 3 parts of the rubber seal ring II,3 parts of the metal seal ring II,3 parts of the piston screw II,3 parts of the gold wire I,3 parts of the steel ball, 3 parts of the pressure gauge, 3 parts of the gold wire II,3 parts of the gold wire 17 parts of the epoxy resin, 3 parts of the copper cable II,3 parts of the copper cable 18 parts of the copper cable II,3 parts of the low-frequency adapter, 3 parts of the copper cable II, 20 parts of the copper cable II,3 parts of the radio-frequency adapter II,4 parts of the radio-frequency adapter I,5 parts of the copper cable I,6 parts of the copper cable I,7 parts of the adapter cavity, 8 parts of the controller, the impedance analyzer and 10 parts of the control rod.
Detailed Description
As shown in fig. 1, the invention is a schematic diagram, which comprises a low-temperature container (1), a sample cavity (2), a pressure cavity (3), a radio frequency adapter I (4), four coaxial cables I (5), a copper cable I (6), an adapter cavity (7), a controller (8), an impedance analyzer (9) and a control rod (10), wherein xyz is a three-dimensional space coordinate system, liquid helium is arranged in the low-temperature container (1), the sample cavity (2) is in a vacuum state, the sample cavity (2) is positioned in the low-temperature container (1), the pressure cavity (3) is positioned in the sample cavity (2), the adapter cavity (7) is connected to the upper surface of the low-temperature container (1) and can be separated from the low-temperature container (1), the control rod (10) sequentially penetrates through the bottom surfaces of the low-temperature container (1) and the sample cavity (2), air tightness is formed between the control rod (10) and the low-temperature container (1) and the sample cavity (2), and the controller (8) and the impedance analyzer (9) are positioned outside the low-temperature container (1).
FIG. 2 is a sectional view of a pressure chamber, as shown in FIG. 3, which is a partially enlarged schematic view of a sample and a hollow piston, wherein the pressure chamber (3) comprises a pressure screw (3-1), a piston screw I (3-2), a chamber body (3-3), a anvil (3-4), a piston (3-5), a metal seal ring I (3-6), a rubber seal ring I (3-7), a sample (3-8), a hollow piston (3-9), a rubber seal ring II (3-10), a metal seal ring II (3-11), a piston screw II (3-12), a gold wire I (3-13), an indium pellet (3-14), a pressure gauge (3-15), a gold wire II (3-16), Epoxy resin (3-17), four copper cables II (3-18), a low-frequency adapter (3-19), four coaxial cables II (3-20) and a radio-frequency adapter II (3-21); The cavity (3-3) is cylindrical and tubular and is provided with an upper section, a middle section and a lower section, threads are formed on the inner sides of the upper section and the lower section of the cavity (3-3) respectively, the inner diameter of the middle section of the cavity (3-3) is 0.6 cm, the piston screw II (3-12) and the piston screw I (3-2) are respectively connected with the upper surface of the upper section and the lower surface of the lower section of the cavity (3-3) in a threaded manner, the piston screw II (3-12) and the piston screw I (3-2) are hollow longitudinally, the piston screw I (3-2) is provided with internal threads, the pressure screw (3-1) is rotatably connected in the piston screw I (3-2), and the top anvil (3-4) is positioned at the upper end of the pressure screw (3-1); A metal sealing ring II (3-11) and a rubber sealing ring II (3-10) are sequentially arranged between the upper section and the middle section of the cavity (3-3), a rubber sealing ring I (3-7) and a metal sealing ring I (3-6) are sequentially arranged between the middle section and the lower section of the cavity (3-3), a piston (3-5) is positioned between a top anvil (3-4) and the metal sealing ring I (3-6), a hollow piston (3-9) is positioned between a piston screw II (3-12) and the metal sealing ring II (3-11), the hollow piston (3-9) is in a hollow round table shape, and the diameter of the upper bottom surface of the hollow piston (3-9) is 0.8 cm, the diameter of the lower bottom surface is 0.6 cm, and the inner diameter is 0.4 cm; The sample (3-8) is positioned in the middle section of the cavity (3-3), the middle section of the cavity (3-3) is filled with liquid pressure medium, the pressure screw (3-1) can be rotated through the control rod (10) and the anvil (3-4) and the piston (3-5) can be moved upwards, so that pressure can be applied to the sample (3-8) through the pressure medium; Four coaxial cables II (3-20) and four copper cables II (3-18) are all penetrated into the hollow piston (3-9) from top to bottom, the four coaxial cables II (3-20) are sequentially provided with an outer protective layer, an outer conductor layer, an electrolyte layer and a core wire from outside to inside, the core wire is made of niobium-titanium superconducting materials, the upper end of each coaxial cable II (3-20) is connected with a radio frequency adapter II (3-21), the upper end of each copper cable II (3-18) is connected with a low frequency adapter (3-19), the lower ends of the two copper cables II (3-18) are connected with a pressure gauge (3-15) through a gold wire II (3-16), The low-frequency adapter (3-19) is connected with the controller (8) through the copper cable I (6) and the adapter cavity (7), and the controller (8) can read the pressure value measured by the pressure gauge (3-15); the hollow piston (3-9) is internally filled with epoxy resin (3-17), as shown in the broken line range of FIG. 3, the epoxy resin (3-17) ensures that four coaxial cables II (3-20) and four copper cables II (3-18) are fixed with the hollow piston (3-9), the lower ends of the four coaxial cables II (3-20) and the four copper cables II (3-18) are all positioned outside the epoxy resin (3-17), the outer conductor layers at the lower ends of the four coaxial cables II (3-20) are connected with each other, two of the four coaxial cables II (3-20) are in a group, the top ends of the core wires at the lower ends of each group are welded together to form welding spots, The welding spots are wrapped by indium to form an indium small ball (3-14), and two indium small balls (3-14) corresponding to two groups of coaxial cables II (3-20) are respectively connected to two different positions on the surface of the sample (3-8) through gold wires I (3-13); the upper ends of the four coaxial cables I (5) are respectively connected with an impedance analyzer (9) through a switching cavity (7), the lower ends of the four coaxial cables I are respectively connected with a radio frequency switching connector I (4), and the radio frequency switching connectors II (3-21) can be connected with the radio frequency switching connector I (4).
The dielectric spectrum measuring device comprises a low-temperature container (1), a sample cavity (2), a pressure cavity (3), a radio frequency adapter I (4), four coaxial cables I (5), a copper cable I (6), an adapter cavity (7), a controller (8), an impedance analyzer (9) and an operating rod (10), xyz is a three-dimensional space coordinate system, liquid helium is arranged in the low-temperature container (1), the sample cavity (2) is in a vacuum state, the sample cavity (2) is positioned in the low-temperature container (1), the pressure cavity (3) is positioned in the sample cavity (2), the adapter cavity (7) is connected on the low-temperature container (1) and can be separated from the low-temperature container (1), the operating rod (10) sequentially penetrates through the low-temperature container (1) and the bottom surface of the sample cavity (2), the control rod (10) is airtight with the low-temperature container (1) and the sample cavity (2), and the controller (8) and the impedance analyzer (9) are positioned outside the low-temperature container (1); The pressure cavity (3) comprises a pressure screw (3-1), a piston screw I (3-2), a cavity (3-3), a top anvil (3-4), a piston (3-5), a metal sealing ring I (3-6), a rubber sealing ring I (3-7), a sample (3-8), a hollow piston (3-9), a rubber sealing ring II (3-10), a metal sealing ring II (3-11), a piston screw II (3-12), a gold wire I (3-13), an indium ball (3-14), a pressure gauge (3-15), a gold wire II (3-16), epoxy resin (3-17), four copper cables II (3-18), the low-frequency adapter (3-19), four coaxial cables II (3-20) and a radio frequency adapter II (3-21); The cavity (3-3) is cylindrical and tubular and is provided with an upper section, a middle section and a lower section, threads are formed on the inner sides of the upper section and the lower section of the cavity (3-3) respectively, the inner diameter of the middle section of the cavity (3-3) is 0.6 cm, the piston screw II (3-12) and the piston screw I (3-2) are respectively connected with the upper surface of the upper section and the lower surface of the lower section of the cavity (3-3) in a threaded manner, the piston screw II (3-12) and the piston screw I (3-2) are hollow longitudinally, the piston screw I (3-2) is provided with internal threads, the pressure screw (3-1) is rotatably connected in the piston screw I (3-2), and the top anvil (3-4) is positioned at the upper end of the pressure screw (3-1); A metal sealing ring II (3-11) and a rubber sealing ring II (3-10) are sequentially arranged between the upper section and the middle section of the cavity (3-3), a rubber sealing ring I (3-7) and a metal sealing ring I (3-6) are sequentially arranged between the middle section and the lower section of the cavity (3-3), a piston (3-5) is positioned between a top anvil (3-4) and the metal sealing ring I (3-6), a hollow piston (3-9) is positioned between a piston screw II (3-12) and the metal sealing ring II (3-11), the hollow piston (3-9) is in a hollow round table shape, and the diameter of the upper bottom surface of the hollow piston (3-9) is 0.8 cm, the diameter of the lower bottom surface is 0.6 cm, and the inner diameter is 0.4 cm; The sample (3-8) is positioned in the middle section of the cavity (3-3), the middle section of the cavity (3-3) is filled with liquid pressure medium, the pressure screw (3-1) can be rotated through the control rod (10) and the anvil (3-4) and the piston (3-5) can be moved upwards, so that pressure can be applied to the sample (3-8) through the pressure medium; the four coaxial cables II (3-20) and the four copper cables II (3-18) penetrate through the hollow piston (3-9) from top to bottom, the four coaxial cables II (3-20) are sequentially provided with an outer protective layer, an outer conductor layer, an electrolyte layer and a core wire from outside to inside, the upper end of each copper cable II (3-18) is connected with a low-frequency adapter (3-19), the lower ends of the two copper cables II (3-18) are connected with a pressure gauge (3-15) through gold wires II (3-16), the low-frequency adapter (3-19) is connected with a controller (8) through a copper cable I (6) through an adapter cavity (7), and the controller (8) can read a pressure value measured by the pressure gauge (3-15); the upper ends of the four coaxial cables I (5) are respectively connected with an impedance analyzer (9) through a switching cavity (7), and the lower ends of the four coaxial cables I are respectively connected with a radio frequency switching connector I (4); The hollow piston (3-9) is internally filled with epoxy resin (3-17) so that four coaxial cables II (3-20) and four copper cables II (3-18) are fixed with the hollow piston (3-9), the lower ends of the four coaxial cables II (3-20) and the four copper cables II (3-18) are all positioned outside the epoxy resin (3-17), the outer conductor layers at the lower ends of the four coaxial cables II (3-20) are connected with each other, two of the four coaxial cables II (3-20) are in a group, the core wire top ends at the lower ends of each group are welded together to form welding spots, the welding spots are wrapped by indium to form a steel ball (3-14), Two indium pellets (3-14) corresponding to two groups of coaxial cables II (3-20) are respectively connected to two different positions on the surface of a sample (3-8) through gold wires I (3-13), the upper end of each coaxial cable II (3-20) is connected with a radio frequency adapter II (3-21), the radio frequency adapter II (3-21) can be connected with a radio frequency adapter I (4), and core wires of the four coaxial cables II (3-20) are made of niobium-titanium superconducting materials.
The processing method of the pressure cavity for dielectric spectrum measurement under the low temperature condition comprises an electroplating process of a core wire of a superconducting cable, a method for connecting a radio frequency connector and a method for leading out a cable on a sample (3-8) in the pressure cavity (3).
The electroplating process of the core wire of the superconducting coaxial cable and the method for connecting the radio frequency connector comprise the following steps:
The electroplating process for the core wire of coaxial cable II (3-20) employs two electrolytic cells, each having an anode and a cathode, wherein the first cell has a basic oxidizing solution therein and the second cell has an acidic copper sulfate solution therein.
Step1, enabling core wires with the length of 1 cm at two ends of a coaxial cable II (3-20) to be exposed out of an outer protective layer, an outer conductor layer and an electrolyte layer, and cleaning and degreasing the surfaces of the core wires at the two ends of the coaxial cable II (3-20);
step 2, placing a core wire to be electroplated in a first electrolytic cell, wherein the core wire is provided with a 110 g/L sodium hydroxide aqueous solution, the core wire is connected to an anode, a copper sheet is adopted as a cathode, the distance between the copper sheet and the core wire is 5 cm, a voltage of 5.5V is applied for 20 seconds, a voltage of 11V is applied for 40 seconds, so that a 30-nanometer oxide layer is deposited on the surface of the core wire, and in the process, the color of the surface of the core wire made of a niobium-titanium material is changed from gray to dark yellow;
step 3, flushing the core wire of the coaxial cable II (3-20) deposited with the oxide layer in deionized water, and rapidly transferring the core wire into a second electrolytic cell;
Step 4, a copper sulfate solution with the concentration of 250 g/L is arranged in the second electrolytic cell, the core wire of the coaxial cable II (3-20) is connected with the cathode, and the voltage is applied for 200 seconds by 6V, so that copper is deposited on the surface of the core wire of the coaxial cable II (3-20);
And 5, welding the core wire at the upper end of the coaxial cable II (3-20) to the radio frequency adapter II (3-21).
The method for leading out the cable on the sample (3-8) in the pressure cavity (3) comprises the following steps:
Step one, penetrating four coaxial cables II (3-20) and four copper cables II (3-18) into a hollow piston (3-9) from top to bottom;
Filling pressure-resistant epoxy resin (3-17) into the hollow piston (3-9) to fix the copper cable II (3-18) and the coaxial cable II (3-20);
Step three, adopting a silver-plated copper wire to connect the outer conductor layers at the lower ends of the four coaxial cables II (3-20) with each other;
Dividing four coaxial cables II (3-20) into two groups, welding the top ends of core wires at the lower ends of the two coaxial cables II (3-20) in each group together to form welding spots, and wrapping the welding spots by indium to form one indium small ball (3-14), namely, forming two indium small balls (3-14) by the two groups of coaxial cables II (3-20);
Step five, the lower end of the coaxial cable II (3-20) is further wrapped by epoxy resin (3-17), so that the outer conductor layer and the electrolyte layer of the coaxial cable II (3-20) are wrapped, and the two indium pellets (3-14) are not wrapped, so that the sealing of the lower end of the coaxial cable II (3-20) can bear larger pressure, the size of the lower end of the coaxial cable II (3-20) is reduced, and the measuring signal in the coaxial cable II (3-20) is well shielded, and the high-frequency characteristic is improved;
step six, after the epoxy resin (3-17) is completely solidified, depositing steel on the two steel pellets (3-14) again so that the diameter of the indium pellets (3-14) is 1 mm;
and seventhly, connecting the two indium pellets (3-14) to two different positions on the surface of the sample (3-8) through gold wires I (3-13), wherein carbon paste is used as an adhesive between the gold wires I (3-13) and the sample (3-8), and silver paste is used as an adhesive between the indium pellets (3-14) and the gold wires I (3-13).
The method for measuring the dielectric spectrum of the material comprises the following steps:
Firstly, connecting the sample (3-8) to a radio frequency adapter II (3-21) through a gold wire I (3-13), an indium ball (3-14) and a coaxial cable II (3-20) in sequence by adopting the method for leading out the cable on the sample (3-8) in the pressure cavity (3), and connecting a pressure gauge (3-15) to a controller (8) through the gold wire II (3-16), a copper cable II (3-18), a low-frequency adapter (3-19) and the copper cable I (6) in sequence;
Secondly, placing a sample (3-8) in the middle section of the cavity (3-3), adding a liquid pressure medium into the cavity (3-3) to fill the middle section of the cavity (3-3), and fixing a hollow piston (3-9) between a piston screw II (3-12) and a metal sealing ring II (3-11);
Thirdly, placing the pressure cavity (3) in the sample cavity (2), connecting the radio frequency adapter II (3-21) to the radio frequency adapter I (4), and connecting the adapter cavity (7) to the upper surface of the low-temperature container (1);
fourthly, adding liquid helium into the low-temperature container (1) to cool the sample cavity (2);
Fifthly, the pressure screw rod (3-1) is rotated through the control rod (10) and the anvil (3-4) and the piston (3-5) are moved upwards, so that pressure is applied to the sample (3-8) through a pressure medium, and the pressure born by the sample (3-8) is measured through the pressure gauge (3-15);
Measuring the dielectric spectrum of the sample (3-8) by an impedance analyzer (9);
Seventhly, rotating the pressure screw (3-1) through the control rod (10) to finely adjust the positions of the anvil (3-4) and the piston (3-5), changing the pressure applied to the sample (3-8), measuring the dielectric spectrum of the sample (3-8) under the pressure condition through the impedance analyzer (9), and repeatedly measuring under a plurality of pressure conditions;
And eight, analyzing the dielectric spectrums measured by the impedance analyzer (9) under the pressure condition of different samples (3-8), and finally obtaining the relation between the dielectric spectrums of the samples (3-8) and the pressure born by the samples (3-8).
The invention adopts a safe and simple method to copper the niobium-titanium core wire of the coaxial cable so as to solve the welding problem between the coaxial cable core wire and the radio frequency adapter, and adopts a special connection mode to introduce the coaxial cable into the pressure cavity, thereby ensuring the tightness of the pressure cavity and the high-frequency characteristic of the coaxial cable.
Claims (1)
1. A processing method of a pressure cavity for dielectric spectrum measurement under a low temperature condition comprises a low temperature container (1), a sample cavity (2), a pressure cavity (3), a radio frequency adapter I (4), four coaxial cables I (5), a copper cable I (6), an adapter cavity (7), a controller (8), an impedance analyzer (9) and an operating lever (10), xyz is a three-dimensional space coordinate system, liquid helium is arranged in the low temperature container (1), the sample cavity (2) is in a vacuum state, the sample cavity (2) is positioned in the low temperature container (1), the pressure cavity (3) is positioned in the sample cavity (2), the adapter cavity (7) is connected on the low temperature container (1) and can be separated from the low temperature container (1), The control rod (10) sequentially penetrates through the bottom surfaces of the low-temperature container (1) and the sample cavity (2), air tightness is formed between the control rod (10) and the low-temperature container (1) and between the control rod and the sample cavity (2), and the controller (8) and the impedance analyzer (9) are both positioned outside the low-temperature container (1); The pressure cavity (3) comprises a pressure screw (3-1), a piston screw I (3-2), a cavity (3-3), a top anvil (3-4), a piston (3-5), a metal sealing ring I (3-6), a rubber sealing ring I (3-7), a sample (3-8), a hollow piston (3-9), a rubber sealing ring II (3-10), a metal sealing ring II (3-11), a piston screw II (3-12), a gold wire I (3-13), an indium ball (3-14), a pressure gauge (3-15), a gold wire II (3-16), epoxy resin (3-17), four copper cables II (3-18), the low-frequency adapter (3-19), four coaxial cables II (3-20) and a radio frequency adapter II (3-21); The cavity (3-3) is cylindrical and tubular and is provided with an upper section, a middle section and a lower section, threads are formed on the inner sides of the upper section and the lower section of the cavity (3-3) respectively, the inner diameter of the middle section of the cavity (3-3) is 0.6 cm, the piston screw II (3-12) and the piston screw I (3-2) are respectively connected with the upper surface of the upper section and the lower surface of the lower section of the cavity (3-3) in a threaded manner, the piston screw II (3-12) and the piston screw I (3-2) are hollow longitudinally, the piston screw I (3-2) is provided with internal threads, the pressure screw (3-1) is rotatably connected in the piston screw I (3-2), and the top anvil (3-4) is positioned at the upper end of the pressure screw (3-1); A metal sealing ring II (3-11) and a rubber sealing ring II (3-10) are sequentially arranged between the upper section and the middle section of the cavity (3-3), a rubber sealing ring I (3-7) and a metal sealing ring I (3-6) are sequentially arranged between the middle section and the lower section of the cavity (3-3), a piston (3-5) is positioned between a top anvil (3-4) and the metal sealing ring I (3-6), a hollow piston (3-9) is positioned between a piston screw II (3-12) and the metal sealing ring II (3-11), the hollow piston (3-9) is in a hollow round table shape, and the diameter of the upper bottom surface of the hollow piston (3-9) is 0.8 cm, the diameter of the lower bottom surface is 0.6 cm, and the inner diameter is 0.4 cm; The sample (3-8) is positioned in the middle section of the cavity (3-3), the middle section of the cavity (3-3) is filled with liquid pressure medium, the pressure screw (3-1) can be rotated through the control rod (10) and the anvil (3-4) and the piston (3-5) can be moved upwards, so that pressure can be applied to the sample (3-8) through the pressure medium; the four coaxial cables II (3-20) and the four copper cables II (3-18) penetrate through the hollow piston (3-9) from top to bottom, the four coaxial cables II (3-20) are sequentially provided with an outer protective layer, an outer conductor layer, an electrolyte layer and a core wire from outside to inside, the upper end of each copper cable II (3-18) is connected with a low-frequency adapter (3-19), the lower ends of the two copper cables II (3-18) are connected with a pressure gauge (3-15) through gold wires II (3-16), the low-frequency adapter (3-19) is connected with a controller (8) through a copper cable I (6) through an adapter cavity (7), and the controller (8) can read a pressure value measured by the pressure gauge (3-15); the upper ends of the four coaxial cables I (5) are respectively connected with an impedance analyzer (9) through a switching cavity (7), and the lower ends of the four coaxial cables I are respectively connected with a radio frequency switching connector I (4); the interior of the hollow piston (3-9) is filled with epoxy resin (3-17) so that four coaxial cables II (3-20) and four copper cables II (3-18) are fixed with the hollow piston (3-9), the lower ends of the four coaxial cables II (3-20) and the four copper cables II (3-18) are all positioned outside the epoxy resin (3-17), the outer conductor layers at the lower ends of the four coaxial cables II (3-20) are connected with each other, two of the four coaxial cables II (3-20) are in a group, the core wire top ends at the two lower ends of each group are welded together to form welding spots, the welding spots are wrapped by indium to form an indium pellet (3-14), Two indium pellets (3-14) corresponding to two groups of coaxial cables II (3-20) are respectively connected to two different positions on the surface of a sample (3-8) through gold wires I (3-13), the upper end of each coaxial cable II (3-20) is connected with a radio frequency adapter II (3-21), the radio frequency adapter II (3-21) can be connected with a radio frequency adapter I (4), the core wires of the four coaxial cables II (3-20) are all made of niobium-titanium superconducting materials,
The method is characterized in that: the processing method of the pressure cavity for dielectric spectrum measurement under the low temperature condition comprises an electroplating process of a core wire of a superconducting cable, a method for connecting a radio frequency connector and a method for leading out a cable on a sample (3-8) in the pressure cavity (3),
The electroplating process of the core wire of the superconducting coaxial cable and the method for connecting the radio frequency connector comprise the following steps:
The electroplating process for the core wire of the coaxial cable II (3-20) employs two electrolytic cells, each having an anode and a cathode, wherein the first cell has a basic oxidizing solution therein, the second cell has an acidic copper sulfate solution therein,
Step1, enabling core wires with the length of 1 cm at two ends of a coaxial cable II (3-20) to be exposed out of an outer protective layer, an outer conductor layer and an electrolyte layer, and cleaning and degreasing the surfaces of the core wires at the two ends of the coaxial cable II (3-20);
step 2, placing a core wire to be electroplated in a first electrolytic cell, wherein the core wire is provided with a 110 g/L sodium hydroxide aqueous solution, the core wire is connected to an anode, a copper sheet is adopted as a cathode, the distance between the copper sheet and the core wire is 5 cm, a voltage of 5.5V is applied for 20 seconds, a voltage of 11V is applied for 40 seconds, so that a 30-nanometer oxide layer is deposited on the surface of the core wire, and in the process, the color of the surface of the core wire made of a niobium-titanium material is changed from gray to dark yellow;
step 3, flushing the core wire of the coaxial cable II (3-20) deposited with the oxide layer in deionized water, and rapidly transferring the core wire into a second electrolytic cell;
Step 4, a copper sulfate solution with the concentration of 250 g/L is arranged in the second electrolytic cell, the core wire of the coaxial cable II (3-20) is connected with the cathode, and the voltage is applied for 200 seconds by 6V, so that copper is deposited on the surface of the core wire of the coaxial cable II (3-20);
step 5, welding a core wire at the upper end of the coaxial cable II (3-20) to the radio frequency adapter II (3-21);
The method for leading out the cable on the sample (3-8) in the pressure cavity (3) comprises the following steps:
Step one, penetrating four coaxial cables II (3-20) and four copper cables II (3-18) into a hollow piston (3-9) from top to bottom;
Filling pressure-resistant epoxy resin (3-17) into the hollow piston (3-9) to fix the copper cable II (3-18) and the coaxial cable II (3-20);
Step three, adopting a silver-plated copper wire to connect the outer conductor layers at the lower ends of the four coaxial cables II (3-20) with each other;
Dividing four coaxial cables II (3-20) into two groups, welding the top ends of core wires at the lower ends of the two coaxial cables II (3-20) in each group together to form welding spots, and wrapping the welding spots by indium to form one indium small ball (3-14), namely, forming two indium small balls (3-14) by the two groups of coaxial cables II (3-20);
Step five, the lower end of the coaxial cable II (3-20) is further wrapped by epoxy resin (3-17), so that the outer conductor layer and the electrolyte layer of the coaxial cable II (3-20) are wrapped, and the two indium pellets (3-14) are not wrapped;
Step six, after the epoxy resin (3-17) is completely solidified, depositing indium on the two indium pellets (3-14) again, so that the diameter of the indium pellets (3-14) is 1 mm;
and seventhly, connecting the two indium pellets (3-14) to two different positions on the surface of the sample (3-8) through gold wires I (3-13), wherein carbon paste is used as an adhesive between the gold wires I (3-13) and the sample (3-8), and silver paste is used as an adhesive between the indium pellets (3-14) and the gold wires I (3-13).
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