CN106707033A - Variable-temperature dielectric constant measurement pool for liquid and solid-liquid phase change - Google Patents
Variable-temperature dielectric constant measurement pool for liquid and solid-liquid phase change Download PDFInfo
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- CN106707033A CN106707033A CN201611125859.0A CN201611125859A CN106707033A CN 106707033 A CN106707033 A CN 106707033A CN 201611125859 A CN201611125859 A CN 201611125859A CN 106707033 A CN106707033 A CN 106707033A
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- dielectric constant
- inner bag
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- 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
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- 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
Abstract
The invention relates to a variable-temperature dielectric constant measurement pool for liquid and solid-liquid phase change. The dielectric constant measurement pool comprises a top electrode, a bottom electrode, a protective electrode, an upper cover, an inner liner, a shell, a water inlet/outlet hole connector, a thermocouple, a BNC adapter, and the like. All the parts coordinate with each other, so that the variable-temperature dielectric constant measurement pool which is stable in structure and good in sealing property, and can regulate the temperature of a sample in real time is formed. The variable-temperature dielectric constant measurement pool for liquid and solid-liquid phase change is connected with a circulating constant-temperature water bath machine and an impedance analyzer, so that the temperature of the sample can be accurately controlled, and the dielectric constant change of the liquid can be accurately measured at the different temperature and when the solid-liquid phase change occurs; the measurement pool is stable in structure, high in vibration resistance and electromagnetic interference resistance, and high in repeatability in measured data; when the liquid has temperature change and solid-liquid phase change, the measurement pool can enable the sample to be closely contacted with an electrode, so that the reliability of the measured data is guaranteed; the cost and maintenance difficulty of dielectric variable-temperature measurement are reduced.
Description
Technical field
The present invention relates to the measurement of dielectric constant, more particularly to when there is solid-liquid phase change in a kind of liquid alternating temperature and liquid
Dielectric constant measurement pond.
Background technology：
When fluid temperature changes and solid-liquid phase change liquid itself occurs, for its dielectric constant, currently with
Electric impedance analyzer is measured to it.In conventional method, structure is carried out to measuring cell based on two electrode runs parallel plate capacitor methods
Design.Its structure is to separate power-on and power-off pole piece using quartz fibre；By measuring the electric capacity of air and sample, final utilization is surveyed
The ratio between sample electric capacity and air electric capacity for obtaining, obtain the relative dielectric constant size of sample.When sample is added, it is necessary to according to sample
The characteristic of product and select measuring cell, if sample is non-volatile in the range of measured temperature, and non-toxic, non-corrosiveness can be by sample
Product are directly added dropwise between two electrode slices；If there is volatility in the range of measured temperature in sample, or with toxicity, corrosivity,
Then need using the liquid measure pond with sealing characteristics.Sealing liquid measure pond, is that Teflon is added between upper/lower electrode
Imperial liner, and add O-ring seal between Teflon liner and power-on and power-off pole plate.Under the compressing of external force, between electrode slice
To form the space of closing, to prevent sample from volatilizing and leakage；Separate still with quartz fibre between electrode slice.In order that sample
Product occurrence temperature changes, and temperature control is carried out to sample frequently with liquid nitrogen alternating temperature stove and temperature control digital display circuit.But this routine side
There is following some shortcoming in method：
1. when isolating power-on and power-off pole piece using quartz fibre, because the putting position of quartz fibre has randomness；And
When electrode slice is installed, electrode slice easily drives liquid in pond, and then changes the putting position of quartz fibre.Both of which
Easily making cannot keeping parallelism between two electrode slices.This non-parallel state increases the randomness of electrode spacing, and cannot
Ensure to be consistent before and after electrode spacing after changing sample.The change of this electrode spacing can be to same sample in different measurements
The capacitance of resulting sample causes a deviation in number of times.Again because quartz fibre diameter is minimum, according toIn electrode
When spacing is minimum, the change of very little can produce strong influence to surveyed electric capacity, and then cause the dielectric constant of gained sample
There is larger deviation and nonrepeatability.
2. when there is solid-liquid phase change for sample, because sealing liquid sample pool inner space does not reserve surplus；And liquid
When body undergoes phase transition, the contraction or expansion of sample volume often occurs.Thus when sample volume changes, this kind of measurement
Pond cannot ensure there is good contact between sample and electrode slice, and then measured dielectric constant is produced deviation.
3. liquid nitrogen alternating temperature stove and the temperature control digital display circuit for matching, involve great expense, bulky, and need in the running
Substantial amounts of liquid nitrogen is consumed, thus limits the popularity that sample becomes temperature measurement, improve measurement threshold and maintenance difficulties.
The content of the invention：
The technical problem to be solved in the present invention is to provide a kind of accuracy of measurement high, strong interference immunity, good airproof performance, cost
It is cheap, safeguard it is simple and can accurate measurement fluid temperature change and dielectric constant when solid-liquid phase change liquid occurs
Measuring cell.
In order to solve the above technical problems, the present invention is adopted the following technical scheme that：
It is a kind of for liquid and the alternating temperature dielectric constant measurement pond of solid-liquid phase change, including Top electrode, bottom electrode, protection electricity
Pole, upper lid, inner bag, shell, intake-outlet connector, thermocouple, the first-class part of BNC switchings；Wherein Top electrode, bottom electrode, on
Lid, inner bag, the profile of shell are that axle center is symmetrical.Top electrode and bottom electrode are all made up of disk sheet metal and metallic rod；Disk gold
Category piece incidentally connects step, and step is included with threaded hole；The subsidiary screw thread of metallic rod, can be by the spiral shell subsidiary with disk sheet metal
Pit is connected, as T-shaped electrode.Guard electrode is cylindrical shape, and attaches connection step, axially extending bore, screw thread.Upper lid is T-shaped
Axle center symmetrical structure, subsidiary screw thread, axially extending bore, seal groove, slot electrode.Inner bag is axle center symmetrical structure, subsidiary countersunk head through hole,
Axially extending bore, screw thread, slot electrode and seal groove.Housing profile attaches screwed hole, axially extending bore, axle to go to push up hollow cylindrical
To screwed hole and radial screw bore.
It is of the invention for liquid and the alternating temperature dielectric constant measurement pond of solid-liquid phase change, upper lid, inner bag, shell maximum it is outer
Footpath is consistent；The subsidiary screw thread of the upper lid screw thread subsidiary with inner bag can cooperate；Upper base portion and inner side of liner bottom
After assembling is completed, there is certain spacing；Upper lid axially extending bore can be engaged with the axially extending bore of guard electrode；Protection electricity
Pole internal diameter is consistent with upper lid base diameter, and can form cooperation；Guard electrode external diameter keeps with bottom electrode disk diameter
Unanimously；Top electrode disk diameter is slightly less than guard electrode internal diameter；The subsidiary slot electrode diameter of upper lid is protected with Top electrode disk diameter
Hold consistent, and can be engaged；The subsidiary slot electrode diameter of inner bag is consistent with bottom electrode diameter, and can be engaged；On
Lid axis through-hole diameter is consistent with Top electrode screw diameter, and can keep loose fit；Inner bag axis through-hole diameter is with
Electrode screw diameter is consistent, and can keep loose fit；The straight external diameter in inner bag bottom is slightly less than outer casing through hole diameter；Inner bag
The countersunk head through hole axial threaded hole subsidiary with shell is engaged；With shell after assembling is completed, both bottoms are in same inner bag
One plane.
It is of the invention for liquid and the alternating temperature dielectric constant measurement pond of solid-liquid phase change, upper lid is carried out with inner bag by screw thread
Assembling；Inner bag is assembled with shell by countersunk head screw, and forms sealing using sealing ring；Upper lid, inner bag, shell are in dress
It is coaxial core structure after matching somebody with somebody.Top electrode is fixed on upper lid by the subsidiary screw thread of metallic rod and nut, and at electrode slice back
Matching sealing ring；Bottom electrode is fixed on inner bag by the screw thread in metallic rod and nut, and in the matching of electrode slice back
Sealing ring；Guard electrode is looped around Top electrode surrounding and profit is screwed on lid, and matches sealing ring；Thermocouple passes through
Upper lid axially extending bore is near Top electrode；The radial screw bore of shell is assembled to form entery and delivery port, water inlet position with metal connector
In bottom, delivery port is located at top.
It is of the invention for liquid and the alternating temperature dielectric constant measurement pond of solid-liquid phase change, upper/lower electrode utilizes BNC adapters
It is connected with electric impedance analyzer BNC holding wires；Entery and delivery port using rubber tube respectively with the feed water inlet of circulation constant temperature water-bath machine and enter
The mouth of a river is connected, and insulating tube is surrounded by outside rubber tube；Guard electrode and entery and delivery port are grounded.
Usage right requirement is of the invention for liquid and the alternating temperature dielectric constant measurement pond of solid-liquid phase change, and sample is carried out
During amount, adopt with the following method：
(1) measuring cell inside and electrode slice are cleaned using pure water, ethanol, acetone；
(2) measuring cell is calibrated using the KCl aqueous solution of air, ethanol, pure water and various concentrations, draws measuring cell
Pond constant, the electric capacity that swims, residual inductance (refer to《Chemical Experiment in Modern Times method and technology》, publishing house of Beijing Normal University,
2010.8,160-164 pages)；
(3) fluid sample is added, alternating temperature is carried out to sample using thermostatic circulation bath machine, sample temperature is detected using thermocouple
Degree, and measure the electric capacity of sample, conductance numerical value at each temperature using electric impedance analyzer；
(4) show that the true dielectric constant of sample and alternation electrical conductivity (are referred to using calibration equation《Chemical Experiment in Modern Times side
Method and technology》, publishing house of Beijing Normal University, page 2010.8,160-164)；
(5) sample is taken out, measuring cell is cleaned, measurement process is completed.
Alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change of the invention is relative to the advantage of prior art：
(1) because upper/lower electrode is separately fixed among upper lid and inner bag, and carried out using screw thread between upper lid and inner bag
Assembling, therefore during sample is changed repeatedly, electrode spacing will not occur obvious change, so as to improve dielectric constant
The data repeatability and reliability of measurement；
(2) guard electrode effectively shields outfield interference, it is ensured that the accuracy of dielectric constant measurement；And actually should
The alternating temperature dielectric constant measurement pond of used time, liquid of the invention and solid-liquid phase change shows very strong antivibration kinetic force, anti-electromagnetism
Interference performance, i.e., when sample cell periphery occurs substantially vibration, large scale electronic equipment operation, the dielectric constant measured by sample is not
Have and significantly change, which enhance the accuracy of dielectric constant measurement；
(3) due to providing spatial margin, when liquid occurs volumetric expansion because of temperature or phase transformation, Neng Gouyou in inner bag
The space for expanding enough；And when volume shrinks, the space that liquid can be under gravity to lacking is carried out in time
Supplement, so as to ensure that the good contact of sample and electrode slice, increased reliability and the degree of accuracy of dielectric constant measurement；
(4) the alternating temperature dielectric constant measurement pond of liquid of the invention and solid-liquid phase change only needs to enter with thermostatic circulation bath machine
Row matching.Compared to liquid nitrogen alternating temperature stove and its temperature control digital display circuit, its cheap, maintenance is simple, thus reduces liquid and consolidate
The threshold of the alternating temperature dielectric constant measurement that liquid phase becomes.
Brief description of the drawings：
Fig. 1 is the side view of guard electrode；
Fig. 2 is the top view of guard electrode
Fig. 3 is the side view of power-on and power-off pole piece and connecting rod；
Fig. 4 is the side view of inner bag
Fig. 5 is the top view of inner bag
Fig. 6 is the side view of upper lid
Fig. 7 is the top view of upper lid
Fig. 8 side view of shell
Fig. 9 is the top view of shell
Figure 10 is the present invention for liquid and the main view half-sectional view in the alternating temperature dielectric constant measurement pond of solid-liquid phase change
Specific embodiment：
1. add O-ring seal in seal groove 8 as shown in Figure 4, Figure 5, in inner bag, seal groove 11, and be pressed into as
In shell shown in Fig. 8, and inner bag is fixed with shell with screwed hole 21 by through hole 6 using counterbore screw, make the interior of inclusion
Portion space forms sealing；At water inlet 22, delivery port 23 in shell both sides, metal connector is screwed in using unsintered tape,
Seal it；Metal connector is connected using rubber tube with thermostatic circulation bath machine；Start thermostatic circulation bath machine and open
Outer circulation, makes thermostatic circulation bath machine that the circulating system of closing is formed with measuring cell；Regulation circulator bath machine outer circulation flux, sees
Examine whether measuring cell shell has water (or other alternating temperature media) to flow with inner bag junction and water inlet 22, the junction of delivery port 23
Go out；If still there are flowing out, by disassembling shell, and sealing ring and unsintered tape should be readjusted, and sealed；Retest, makes
Final anhydrous (or other alternating temperature media) outflow.
2. after Fig. 4 inner bags and the assembling of Fig. 8 shells are finished, inner surface, figure using pure water, ethanol, acetone to Fig. 4 inner bags
Lid, Fig. 3 power-on and power-off pole piece, Fig. 1 guard electrodes are cleaned repeatedly on 6；Cleaning finish after, on Fig. 6 cover seal groove 16 with
O-ring seal is loaded onto in the seal groove 10 of Fig. 4 inner bags, and the upper and lower electrodes of Fig. 3 are assembled by screw thread 3 and screw thread 4, then
Slot electrode 9 and slot electrode 17 are inserted by through hole 12 and through hole 14 respectively；In the through hole end, matched somebody with somebody using nut, pad and screw thread 5
Close, fix upper and lower electrode slice；O-ring seal is added in the seal groove 18 covered on Fig. 6, figure 1 above guard electrode, and profit is covered
It is fixed with through hole 6 by through hole 1 with screw, nut；The upper lid that will be assembled is matched with screw thread 7 by screw thread 15 and merges rotation
Enter in inner bag, form the alternating temperature dielectric constant measurement pond of liquid of the invention and solid-liquid phase change.
3. the water inlet 22 of the measuring cell that will be assembled and delivery port 23, re-use rubber tube and access thermostatic circulation bath
Machine, wraps insulating tube outside rubber tube；Thermostatic circulation bath machine is set to target temperature, outer circulation is opened, certain stream is set
Amount, makes to be full of water (or other alternating temperature media) between measuring cell Fig. 4 inner bags and Fig. 8 shells；By the screw thread 5 of the upper and lower electrode slices of Fig. 3
It is utilized respectively the BNC data wires that BNC adapters access electric impedance analyzer；By Fig. 1 guard electrodes, water inlet 22 and delivery port 23
Metal connector is grounded；The through hole 20 of the disalignment by being covered on Fig. 6, adds thermocouple, the temperature checked in measuring cell.
4. the method for addition sample is：To be covered on Fig. 6 and screwed out from Fig. 4 inner bags, after adding a certain amount of sample, revolved again
Tightly；The addition of sample should be higher than that the height of Fig. 3 Top electrode disks.When the temperature that the thermocouple on measuring cell is detected reaches mesh
During mark temperature, measure.
5. air, ethanol, the electric capacity of pure water and electricity in sample cell when measuring 20 degrees Celsius respectively using electric impedance analyzer
Lead；Air, the electric capacity of ethanol pure water are extracted, and consults the standard dielectric constant of three；By the use of standard dielectric constant as horizontal seat
Mark, by the use of the electric capacity surveyed as total coordinate, and proceeds linear fit, and the slope of gained is pond constant, and intercept is to swim
Electric capacity；The KCL solution of various concentrations is measured, its electric capacity and electric conductivity value is obtained；By the use of conductance square as abscissa, using electricity
Hold as ordinate, and carry out linear fit, gained slope is negative residual inductance.(refer to《Chemical Experiment in Modern Times method and skill
Art》, publishing house of Beijing Normal University, page 2010.8,160-164)
6. measuring cell is cleaned, and adds testing sample, adjust sample temperature using thermostatic circulation bath machine, and utilize impedance
Analyzer measures the electric capacity and electric conductivity value of the sample at a temperature of each；The actual capacitance and electricity of sample are obtained using calibration equation
Lead；The true dielectric constant and electrical conductivity of sample are obtained using correlation formula.(refer to《Chemical Experiment in Modern Times method and technology》,
Publishing house of Beijing Normal University, page 2010.8,160-164)
7. sample is taken out, measuring cell is cleaned, measurement terminates.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to model of the invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, those of ordinary skill in the art are to technical side of the invention
Various modifications and improvement that case is made, all should fall into the protection domain of claims of the present invention determination.
Claims (5)
1. a kind of for liquid and the alternating temperature dielectric constant measurement pond of solid-liquid phase change, it is characterised in that：Including Top electrode, lower electricity
Pole, guard electrode, upper lid, inner bag, shell, intake-outlet connector, thermocouple, the first-class part of BNC switchings；Wherein Top electrode,
Bottom electrode, upper lid, inner bag, the profile of shell are that axle center is symmetrical.Top electrode and bottom electrode are all by disk sheet metal and metallic rod group
Into；Disk sheet metal incidentally connects step, and step is included with threaded hole；The subsidiary screw thread of metallic rod, can by with disk metal
The subsidiary screwed hole connection of piece, as T-shaped electrode.Guard electrode is cylindrical shape, and attaches connection step, axially extending bore, screw thread.
Upper lid is T-shaped axle center symmetrical structure, subsidiary screw thread, axially extending bore, seal groove, slot electrode.Inner bag is axle center symmetrical structure, subsidiary
Countersunk head through hole, axially extending bore, screw thread, slot electrode and seal groove.Housing profile attaches screwed hole, axle to go to push up hollow cylindrical
To through hole, axial threaded hole and radial screw bore.
2. according to claim 1 for liquid and the alternating temperature dielectric constant measurement pond of solid-liquid phase change, it is characterised in that：On
Lid, inner bag, the maximum outside diameter of shell are consistent；The subsidiary screw thread of the upper lid screw thread subsidiary with inner bag can cooperate；On
After assembling is completed, there is certain spacing with inner side of liner bottom in base portion；The axial direction of upper lid axially extending bore and guard electrode
Through hole can be engaged；Guard electrode internal diameter is consistent with upper lid base diameter, and can form cooperation；Guard electrode external diameter
It is consistent with bottom electrode disk diameter；Top electrode disk diameter is slightly less than guard electrode internal diameter；The subsidiary slot electrode of upper lid is straight
Footpath is consistent with Top electrode disk diameter, and can be engaged；The subsidiary slot electrode diameter of inner bag keeps with bottom electrode diameter
Unanimously, and can be engaged；Upper lid axis through-hole diameter is consistent with Top electrode screw diameter, and can keep loose fit；
Inner bag axis through-hole diameter is consistent with bottom electrode screw diameter, and can keep loose fit；The straight external diameter in inner bag bottom is smaller
In outer casing through hole diameter；The axial threaded hole that the countersunk head through hole of inner bag is subsidiary with shell is engaged；Inner bag completes to fill with shell
After matching somebody with somebody, both bottoms are in same plane.
3. according to claim 2 for liquid and the alternating temperature dielectric constant measurement pond of solid-liquid phase change, it is characterised in that：On
Lid is assembled with inner bag by screw thread；Inner bag is assembled with shell by countersunk head screw, and it is close to form axle using sealing ring
Envelope；Upper lid, inner bag, shell are after mounting coaxial core structure.Top electrode is fixed on by the subsidiary screw thread of metallic rod with nut
On upper lid, and sealing ring is matched at electrode slice back；Bottom electrode is fixed on inner bag by the screw thread in metallic rod and nut
On, and match sealing ring at electrode slice back；Guard electrode is looped around Top electrode surrounding and profit is screwed on lid, and
Matching sealing ring；Thermocouple is by upper lid axially extending bore near Top electrode；The radial screw bore of shell is assembled with metal connector
Entery and delivery port is formed, water inlet is located at bottom, and delivery port is located at top.
4. according to claim 2 for liquid and the alternating temperature dielectric constant measurement pond of solid-liquid phase change, it is characterised in that：On
Bottom electrode is connected using BNC adapters with electric impedance analyzer BNC holding wires；Entery and delivery port is permanent with circulation respectively using rubber tube
The feed water inlet of tepidarium machine and water inlet are connected, and insulating tube is surrounded by outside rubber tube；Guard electrode and entery and delivery port are grounded.
5. the alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change described in usage right requirement 1-4 measures liquid alternating temperature
And the method for dielectric constant constant during generation solid-liquid phase change, it is characterised in that：
(1) measuring cell inside and electrode slice are cleaned using pure water, ethanol, acetone；
(2) measuring cell is calibrated using the KCl aqueous solution of air, ethanol, pure water and various concentrations, draws the pond of measuring cell
Constant, the electric capacity that swims, residual inductance (are referred to《Chemical Experiment in Modern Times method and technology》, publishing house of Beijing Normal University,
2010.8,160-164 pages)；
(3) fluid sample is added, alternating temperature is carried out to sample using thermostatic circulation bath machine, sample temperature is detected using thermocouple,
And measure the electric capacity of sample, conductance numerical value at each temperature using electric impedance analyzer；
(4) show that the true dielectric constant of sample and alternation electrical conductivity (are referred to using calibration equation《Chemical Experiment in Modern Times method with
Technology》, publishing house of Beijing Normal University, page 2010.8,160-164)；
(5) sample is taken out, measuring cell is cleaned, measurement process is completed.
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| CN201611125859.0A CN106707033B (en) | 2016-12-08 | 2016-12-08 | A kind of alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change |
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| CN106707033B CN106707033B (en) | 2019-06-21 |
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Cited By (3)
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| CN108195882A (en) * | 2018-02-24 | 2018-06-22 | 青岛允天保温科技有限公司 | A kind of phase transition process monitoring device and its monitoring system |
| CN110749622A (en) * | 2019-09-23 | 2020-02-04 | 杭州电子科技大学 | Solution uniformity detection device and method based on adjustable discontinuous parallel electrode plates |
| CN111157587A (en) * | 2019-12-30 | 2020-05-15 | 中国人民解放军军事科学院国防科技创新研究院 | Conductivity sensor for microgravity environment |
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| CN110749622A (en) * | 2019-09-23 | 2020-02-04 | 杭州电子科技大学 | Solution uniformity detection device and method based on adjustable discontinuous parallel electrode plates |
| CN110749622B (en) * | 2019-09-23 | 2022-04-26 | 杭州电子科技大学 | Solution uniformity detection device and method based on adjustable discontinuous parallel electrode plates |
| CN111157587A (en) * | 2019-12-30 | 2020-05-15 | 中国人民解放军军事科学院国防科技创新研究院 | Conductivity sensor for microgravity environment |
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| CN106707033B (en) | 2019-06-21 |
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