CN108444840A - A kind of three stage thixotropy test methods of characterization thixotropic fluid rheology - Google Patents
A kind of three stage thixotropy test methods of characterization thixotropic fluid rheology Download PDFInfo
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Abstract
The invention discloses a kind of three stage thixotropy test methods of characterization thixotropic fluid rheology.The characterizing method that this method passes through three rank thixotropic fluids of improvement, realize the viscoelastic spectra for obtaining structure destruction and Restoration stage in situ while traditional 3ITT is tested, obtain the differentiation of viscoelastic spectra at any time, complete characterization thixotropic fluid material destroys and the structure change in recovery process in structure, it is hereby achieved that the information of microstructure real-time change of the material under shearing field, the guidance being worth with important references is provided for the production and processing and application of high thixotropic fluent material.
Description
Technical field
The present invention relates to the Rheological Characterization fields of thixotropic fluid, and in particular to a kind of characterization thixotropic fluid rheology
Three stage thixotropy test（3 interval thixotropy test, 3ITT）Method.
Background technology
Thixotropy（thixotropy）Fluid is a kind of common time-dependent fluid, and commercial Application is very extensive, example
Such as：Paint, conductive silver paste, ink, Emulsion ointment etc..Thixotropic fluid becomes another value from a value suddenly in shear rate
When, viscosity reaches new steady-state value from old steady-state value and needs a period of time, and the length of this period depends on temperature, shearing
The factors such as the amplitude of variation of rate and absolute value.Thixotropic fluid needs to adapt to painting, stream according to the difference in concrete application field
The conditions such as saliva, spraying, inkjet printing and the different technological process of quality requirement, therefore thixotropic characterization is related work to regulation and control
The technology emphasis of industry.
Since the time that thixotropic fluid reaches stable state is often very long, the instantaneous rheological equationm of state will strongly depend on shearing and go through
History, therefore its characterization and regulation and control are also technological difficulties.In common thixotropic fluid measurement method, the test of three stage thixotropy
（3 interval thixotropy test, 3ITT）It is that more rigorous thixotropy is tested.The specific implementation method of 3ITT has
Several mutation, but its common basic step is：1）Sample is stood in measuring examination tool until temperature reaches balance；2）To sample
It carries out high speed shear to viscosity and reaches stable state（Structure is destroyed）;3）Small strain measurement is carried out to sample and tracks its structure recovery process
Until reaching stable state.The measurement target of 3ITT is the characteristic time parameter for obtaining sample structure and destroying and restoring, and is touched as sample
The quantitatively characterizing of denaturation.However, the structural information that the test method obtains sample is limited, and structural damage and recovery are thixotropings
The essential reason of the property rheological equationm of state.
The means that sample structure information is characterized in rheology are to carry out but small oscillations frequency sweep, obtain the viscoelastic spectra of sample.It is logical
It crosses and traditional 3ITT is improved, realize the viscoelastic for obtaining structure destruction and Restoration stage in situ while traditional 3ITT is tested
Spectrum, used technology is time resolution orthogonal superposition rheometer test technology.X-y direction, that is, horizontal direction of the technology in sample
Apply continuous shear stress, while applying but small oscillations in the directions the x-z of sample, that is, vertical direction, to may be implemented in different shearing speed
The viscoelastic spectra of sample is obtained under rate.Binding time resolution techniques, can get the differentiation of viscoelastic spectra at any time, and complete characterization sample exists
Structure is destroyed and the structure change in recovery process.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide it is a kind of characterization thixotropic fluid rheology three
Stage thixotropy test method.This method is realized and is surveyed in traditional 3ITT by the characterizing method of three rank thixotropic fluids of improvement
The viscoelastic spectra of structure destruction and Restoration stage is obtained while examination in situ, obtains the differentiation of viscoelastic spectra at any time, complete characterization touches
Fluid is denaturalized in structure destruction and the thixotropic nature of recovery process material and the change of internal microstructure, is cut to obtain difference
The thixotroping information of material under tangent condition.
The purpose of the present invention is achieved through the following technical solutions.
A kind of three stage thixotropy test methods of characterization thixotropic fluid rheology, skill is tested in conjunction with three stage thixotropy
Art and time resolution orthogonal superposition rheometer test technology carry out characterization test；
Specifically comprise the following steps：
（1）After thixotropic fluid after aging is completed loading on rheometer, pre- shear parameters, balance are set on rheometer
The shear rate of circumferencial direction, time resolution orthogonal superposition shake when time of repose, time resolution orthogonal superposition oscillation rheometer test
The small amplitude oscillatory shear parameter and multiple scanning number of vertical direction when swinging rheometer test；
（2）Start rheometer, proceed by test, and carries out all needing before time resolution orthogonal superposition oscillation rheometer test every time
Re-start step（1）The pre- shearing peace weighing apparatus being arranged；Test data is obtained, and is handled using interpolation method, show that difference is cut
The time viscoelastic modal data of sample under cutting speed rate different moments.
Preferably, step（1）In, the aging is stood in the constant-temperature constant-humidity environment of 80 % of 25 DEG C of temperature and humidity
Natural aging 1 ~ 4 day.
Preferably, step（1）In, the pre- shear parameters include pre-shear rate and pre- shear time, and pre- shearing is arranged
Rate is 200 ~ 1500 s-1, preferably 500 s-1；It is 20 ~ 600 s that pre- shear time, which is arranged,.
Preferably, step（1）In, setting balance time of repose is 500 ~ 1000 s.
Preferably, step（1）In, the shear rate of circumferencial direction when setting time resolution orthogonal superposition vibrates rheometer test
For 0.001 ~ 100 s-1。
Preferably, step（1）In, the but small oscillations of vertical direction when the time resolution orthogonal superposition vibrates rheometer test
Shearing（SAOS）Parameter includes orthogonal strain, and ranging from 0.5 % ~ 5 %, preferably 1 % of orthogonal strain is arranged.
Preferably, step（1）In, setting multiple scanning number is 8 times, and 8 sweep times totally 1000 s.
It is furthermore preferred that the frequency scanned every time is arranged with 1,2.15,4.57,10,21.38 and 45.71 rad/s as one
Group of frequencies, and according to frequency, scanning is complete single pass successively from low to high under every group of frequencies, obtains sweeping under every group of frequencies
The 6 groups of data retouched immediately enter scan round next time after the completion of scanning every time, until 8 scanning is completed, 48 groups of numbers are obtained
According to.
Preferably, step（2）In, in the test process, is handled and directly obtained under different shear rate using interpolation method
Multiple scanning total time（1000 s）Interior time resolution viscoelastic spectra.
The time resolution viscoelastic spectra directly obtained under each shear rate under each stand-by period, table are handled using interpolation method
It is now under the same stand-by period, shear rate is bigger, and sample more shows as class I liquid I behavior, when shear rate is closer to zero,
The class solid behavior of sample is more apparent；Under same shear rate, the stand-by period is shorter, and sample more shows as class I liquid I behavior, when
Between it is longer, the class solid behavior of sample is more apparent；Again by when the superposition of m- shear rate method obtain the relaxation behavior of material
Contacting between shear rate.
Preferably, the environment temperature of entire test process is 20 ~ 60 DEG C, preferably 25 DEG C, and specifically used advanced Peltier
System APS carries out accurate temperature control to entirely testing, and temperature-controlled precision is ± 0.1 DEG C；Humidity is strict controlled in 60 % hereinafter, compression
Air pressure reaches 0.5 MPa.
Compared with existing measuring technology, the present invention has the advantage that and technique effect：
（1）By time resolution orthogonal superposition rheometer test technology, high thixotropic fluent material can be obtained with simple and quick original position
The real-time condition of variation and comprehensive viscoplasticity information are destroyed and rebuild to sample interior structure under different shear rate, right
It is of great significance in the production and processing practice and application of actual thixotropic fluid material；
（2）With strain rate frequency scanning method（Strain-Rate Frequency Sweep, SRFS）Difference, the reality of SRFS
Material has been set to enter inelastic region when being more than 100% including strain in the test process of border, the analysis of data at this time cannot directly make
With traditional rheological analyzing method, it is related to the structure of the constitutive equation of inelastic region material, analysis calculation method and process are multiple
It is miscellaneous；And for time resolution orthogonal superposition rheometer test technology, entire orthogonal SAOS is in the range of strain of very little（It should become smaller
In 5 %）, it is in the linear viscoelastic region of material；Therefore, the result reflection that time resolution orthogonal superposition rheometer test technology obtains is
It is the actual change of real material internal microstructure under shear；
（3）Parallel stacking method has prodigious the disadvantage is that, the flow field of one-way flow and the flow fields SAOS of reciprocating vibration can be sent out
Raw strong coupling, that is, the immediate data for testing acquisition are interacted to obtain by two flow fields, the micro- knot of material internal
The variation of structure and be not merely as caused by shear flow, this for it is actual analysis cause very big difficulty；And time resolution
Orthogonal superposition rheometer test technology one-way flow field and oscillating field are independent from each other, testing the result is that real by shearing
Caused by internal structure variation, therefore time resolution orthogonal superposition rheometer test technology can be more intuitive and directly be probed into
Shear the influence for material.
Specific implementation mode
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment, but the protection model of the present invention
It encloses and embodiment is without being limited thereto.
Artificial hectorite is a kind of sheet silicate of synthesis, be not dissolved in water but can be hydrated in water expansion formed it is colourless
Transparent colloid, even if at very low concentrations, artificial hectorite also has splendid thixotropy and yield value.Due to artificial water
Pyroxene generates high viscosity at low shear rates, assigns product splendid anti-deposit；Meanwhile it being generated under high-rate of shear low viscous
Degree has impayable shear shinning, and consistency replys the various unique characteristics such as rapid and controllability after shearing, makes
It becomes most widely used thickener and rheological property conditioning agent, is a kind of material with typical thixotropy effect, wide
It is general to be applied to include the fields such as medicine, agricultural products, coating, household care, personal care articles and tooth paste product.
In specific embodiment, tested using artificial hectorite gel as thixotropic fluid sample.
In specific embodiment, the process tested using artificial hectorite gel as thixotropic fluid sample specifically includes
Following steps：
（1）The preparation of artificial hectorite gel：
Artificial hectorite powder is placed in and is placed with drier（One or more of anhydrous magnesium sulfate and anhydrous calcium chloride）Vacuum
In drying box, fully dry 24 h of 30 DEG C of constant temperature to constant weight；Artificial hectorite after drying is slow（3~5 min）It is added to dress
Have in ultra-pure water of the conductivity equal to 18.2 M Ω cm and the wide mouth glass bottle with cover added with magnetic stir bar, fully acutely stirs
It mixes（400 ~ 800 rpm, 20 ~ 30 min）Ice-bath ultrasonic is carried out later（Ultrasonic power is 100 W, and supersonic frequency is 40 kHz, is surpassed
The sound time is 10 ~ 30 min）, so that dispersion liquid is become clear from turbid whitish, bottleneck be sealed with parafilm, and revolves
Tight bottle cap obtains the primary liquid of artificial hectorite；The primary liquid of artificial hectorite is placed on constant temperature and humidity（25 DEG C, 80 %）Training
It supports in case, stands natural aging 1 ~ 4 day, obtain the artificial hectorite gel sample of homogeneous transparent, wherein the matter of artificial hectorite
Amount score is the wt% of 2.5 wt% ~ 5；
（2）Microstructure and viscoelastic characterization in a shear condition are carried out to the artificial water brightness gel sample of preparation, that is, improved
Three stage thixotropy test（3 interval thixotropy test, 3ITT）--- time resolution orthogonal superposition oscillatory flow
Become test：
Artificial hectorite dispersion liquid sample after aging is fitted under double aperture slit coaxial cylinders in fixture, jiggle fixture so that
Sample distribution is uniform and removes air entrapment, lower fixture is mounted on rheometer, starter motor makes rotating speed reach 1 ~ 5 rad/
S drives lower fixture rotation, manual slowly to decline upper fixture, until upper fixture is automatic after immersing sample most to decline upper fixture, closes
Close motor, completion of the sample；
Experimental arrangement and parameter are set：Pre- shear parameters are set（Including pre-shear rate and pre- shear time, preshearing cutting speed is set
Rate ranging from 200 ~ 1500 s-1, it is 20 ~ 600 s that pre- shear time, which is arranged,）, equilibration time（It is set as 500 ~ 1000 s）, the time
The shear rate of circumferencial direction when differentiating orthogonal superposition oscillation rheometer test（Setting shear rate is 0.001 ~ 100 s-1）, the time
The but small oscillations scanning of vertical direction when differentiating orthogonal superposition oscillation rheometer test（SAOS）Design parameter（It is answered including orthogonal
Become, orthogonal strain 1%）And scan cycle number（The number of multiple scanning is 8 times, and 8 sweep times totally 1000 s；If
The frequency scanned every time is set with 1,2.15,4.57,10,21.38 and 45.71 rad/s for a group of frequencies, and under every group of frequencies
According to frequency, scanning is complete single pass successively from low to high, obtains scanned under every group of frequencies 6 groups of data, scans every time
Scan round next time is immediately entered after the completion, until 8 scanning is completed, 48 groups of data are obtained）；
The temperature of entire test system is 25 DEG C, and accurate temperature control, temperature control are carried out to entirely testing using advanced Peltier system APS
Precision is ± 0.1 DEG C, and humidity is strict controlled in 60 % hereinafter, compressed air air pressure reaches 0.5 MPa；
It is required for re-starting sample before carrying out time resolution orthogonal superposition oscillation rheometer test every time and step（1）'s
Consistent pre- shearing peace weighing apparatus is set, to obtain the sample of original state；Test is obtained test data to handle using interpolation method,
Directly obtain the time viscoelastic spectra in the multiple scanning total time under different shear rate.
Embodiment 1
The three stage thixotropy test methods for characterizing artificial hectorite gel rheology, are as follows：
（1）It takes artificial hectorite to be placed in and is placed with 24 h in 30 DEG C of vacuum drying chambers of anhydrous calcium chloride, precisely quickly weigh 1.2490
The artificial hectorite of g dryings is slowly added in the wide-mouth bottle equipped with stirrer and 48.75 mL ultra-pure waters, one at 100 rpm
Side charging is stirred on one side, is fed and is completed after 3 min, screws bottle cap, is increased mixing speed to 400 rpm, is stirred 25 min and all move
Remove 15 min of ice-bath ultrasonic（Ultrasonic power is 100 W, and supersonic frequency is 40 kHz）, transparent clear dispersion liquid is obtained, stone is used
Paraffin paper seals, and covers tightly bottle cap, is placed in 25 DEG C, and aging 4 days in the climatic chamber of 80 % obtains the people that mass fraction is 2.5 %
Make hectorite gel sample；
（2）Time resolution orthogonal superposition rheometer test is carried out to the sample after aging, time resolution orthogonal superposition rheometer test is pre-
Shearing condition is：Pre-shear rate is 500 s-1, pre- shear time is 200 s, balances 800 s；It is finally 100 in shear rate
s-1Under conditions of carry out it is orthogonal（Orthogonal strain is 1%）Frequency sweep is repeated, the number of multiple scanning is 8 times, and 8 sweep times are total
The frequency scanned every time is arranged with 1,2.15,4.57,10,21.38 and 45.71 rad/s as a group of frequencies in 1000 s, and every
According to frequency, scanning is complete single pass successively from low to high under group of frequencies, obtains scanned under every group of frequencies 6 groups of data,
Scan round next time is immediately entered after the completion of scanning every time, until 8 scanning is completed, 48 groups of data are obtained；Integrated testability
Environmental system temperature is 25 DEG C, and accurate temperature control is carried out to entirely testing using advanced Peltier system APS, temperature-controlled precision is ±
0.1 DEG C, humidity is strict controlled in 60%, and compressed air air pressure reaches 0.5 MPa；
Test data is handled using interpolation method to obtain this shear rate（100 s-1）Under time viscoelastic spectra, and every time into
It needs to re-start sample the pre- shearing consistent with initial pre- shearing before row time resolution orthogonal superposition oscillation rheometer test
（500 s-1, 200 s）And balance（800 s）, to obtain the sample of original state；
When sweep time is 10 s, at 0.1 rad/s, complex viscosity is 18.25 Pas, and storage modulus is 0.14 Pa, damage
Consumption modulus is 2.62 Pa；When sweep time is 10 s, at 0.1 rad/s, complex viscosity is 0.72 Pas, storage modulus
For 21.14 Pa, loss modulus is 20.65 Pa；
Compared to the method that general steady state shearing has to shear viscosity, this tests while obtaining viscosity and modulus information, has
Solid-liquid transformation phenomenon generates, and the time is in short-term class I liquid I behavior, is class solid behavior when the time is long.
Embodiment 2
The three stage thixotropy test methods for characterizing artificial hectorite dispersion liquid rheology, are as follows：
（1）It takes artificial hectorite to be placed in and is placed with 24 h in 30 DEG C of vacuum drying chambers of anhydrous calcium chloride, precisely quickly weigh 1.4978g
Dry artificial hectorite is slowly added in the wide-mouth bottle equipped with stirrer and 48.5 mL ultra-pure waters, at 150 rpm on one side
Charging is stirred on one side, is fed and is completed after 4 min, screws bottle cap, is increased mixing speed to 500 rpm, is stirred 20 min and all remove
10 min of ice-bath ultrasonic（Ultrasonic power is 100 W, and supersonic frequency is 40 kHz）, transparent clear dispersion liquid is obtained, paraffin is used
Paper seals, and covers tightly bottle cap, is placed in 25 DEG C, and aging 2 days in the climatic chamber of 80 % obtains the artificial water that mass fraction is 3 %
Pyroxene gel sample；
（2）Time resolution orthogonal superposition rheometer test is carried out to the sample after aging, time resolution orthogonal superposition rheometer test is pre-
Shearing condition is：Pre-shear rate is 500 s-1, pre- shear time is 200 s, balances 800 s；It is finally 100 in shear rate
s-1Under conditions of carry out it is orthogonal（Orthogonal strain is 0.5%）Frequency sweep is repeated, the number of multiple scanning is 8 times, and 8 sweep times
The frequency scanned every time is arranged with 1,2.15,4.57,10,21.38 and 45.71 rad/s as a group of frequencies in totally 1000 s, and
According to frequency, scanning is complete single pass successively from low to high under per group of frequencies, obtains scanned under every group of frequencies 6 groups of numbers
According to scanning every time immediately enters scan round next time after the completion, until 8 scanning is completed, 48 groups of data are obtained；It is whole to survey
Test ring border system temperature is 25 DEG C, carries out accurate temperature control to entirely testing using advanced Peltier system APS, temperature-controlled precision is
± 0.1 DEG C, humidity is strict controlled in 40%, and compressed air air pressure reaches 0.5 MPa；
Test data is handled using interpolation method to obtain this shear rate（100 s-1）Under time viscoelastic spectra, and every time into
It needs to re-start sample the pre- shearing consistent with initial pre- shearing before row time resolution orthogonal superposition oscillation rheometer test
（500 s-1, 200 s）And balance（800 s）, to obtain the sample of original state；
When sweep time is 10 s, at 0.1 rad/s, complex viscosity is 25.46 Pas, and storage modulus is 1.92 Pa, damage
Consumption modulus is 5.83 Pa；When sweep time is 1000 s, at 0.1 rad/s, complex viscosity is 3.89 Pas, energy storage mould
Amount is 50.22 Pa, and loss modulus is 47.89 Pa；
Compared to the method that general steady state shearing has to shear viscosity, this tests while obtaining viscosity and modulus information, has
Solid-liquid transformation phenomenon generates, and the time is in short-term class I liquid I behavior, is class solid behavior when the time is long.
Embodiment 3
The three stage thixotropy test methods for characterizing artificial hectorite dispersion liquid rheology, are as follows：
（1）It takes artificial hectorite to be placed in and is placed with 24 h in 30 DEG C of vacuum drying chambers of anhydrous calcium chloride, precisely quickly weigh 2.5012g
Dry artificial hectorite is slowly added in the wide-mouth bottle equipped with stirrer and 47.5 mL ultra-pure waters, at 200 rpm on one side
Charging is stirred on one side, is fed and is completed after 5 min, screws bottle cap, is increased mixing speed to 800 rpm, is stirred 30 min and all remove
20 min of ice-bath ultrasonic（Ultrasonic power is 100 W, and supersonic frequency is 40 kHz）, transparent clear dispersion liquid is obtained, paraffin is used
Paper seals, and covers tightly bottle cap, is placed in 25 DEG C, and aging 1 day in the climatic chamber of 90 % obtains the artificial water that mass fraction is 5 %
Pyroxene gel sample；
（2）Time resolution orthogonal superposition rheometer test is carried out to the sample after aging, time resolution orthogonal superposition rheometer test is pre-
Shearing condition is：Pre-shear rate is 500 s-1, pre- shear time is 200 s, balances 800 s；It is finally 100 in shear rate
s-1Under conditions of carry out it is orthogonal（Orthogonal strain is 1%）Frequency sweep is repeated, the number of multiple scanning is 8 times, and 8 sweep times are total
The frequency scanned every time is arranged with 1,2.15,4.57,10,21.38 and 45.71 rad/s as a group of frequencies in 1000 s, and every
According to frequency, scanning is complete single pass successively from low to high under group of frequencies, obtains scanned under every group of frequencies 6 groups of data,
Scan round next time is immediately entered after the completion of scanning every time, until 8 scanning is completed, 48 groups of data are obtained；Integrated testability
Environmental system temperature is 25 DEG C, and accurate temperature control is carried out to entirely testing using advanced Peltier system APS, temperature-controlled precision is ±
0.1 DEG C, humidity is strict controlled in 40%, and compressed air air pressure reaches 0.5 MPa；
Test data is obtained into this shear rate using interpolation method（100 s-1）Under time viscoelastic spectra, and in each carry out
Between differentiate orthogonal superposition oscillation rheometer test before need to re-start sample the pre- shearing consistent with initial pre- shearing（500
s-1, 200 s）And balance（800 s）, to obtain the sample of original state；
When sweep time is 10 s, at 0.1 rad/s, complex viscosity is 80.53 Pas, and storage modulus is 10.25 Pa,
Loss modulus is 20.73 Pa；When sweep time is 1000 s, at 0.1 rad/s, complex viscosity is 12.39 Pas, storage
Energy modulus is 200.55 Pa, and loss modulus is 170.91 Pa；
Compared to the method that general steady state shearing has to shear viscosity, this tests while obtaining viscosity and modulus information, has
Solid-liquid transformation phenomenon generates, and the time is in short-term class I liquid I behavior, is class solid behavior when the time is long.
Embodiment 4
The three stage thixotropy test methods for characterizing artificial hectorite dispersion liquid rheology, are as follows：
（1）It takes artificial hectorite to be placed in and is placed with 24 h in 30 DEG C of vacuum drying chambers of anhydrous calcium chloride, precisely quickly weigh 1.5008g
Dry artificial hectorite is slowly added in the wide-mouth bottle equipped with stirrer and 48.5 mL ultra-pure waters, at 150 rpm on one side
Charging is stirred on one side, is fed and is completed after 4 min, screws bottle cap, is increased mixing speed to 500 rpm, is stirred 20 min and all remove
10 min of ice-bath ultrasonic（Ultrasonic power is 100 W, and supersonic frequency is 40 kHz）, transparent clear dispersion liquid is obtained, paraffin is used
Paper seals, and covers tightly bottle cap, is placed in 25 DEG C, and aging 2 days in the climatic chamber of 80 % obtains the artificial water that mass fraction is 3 %
Pyroxene gel sample；
（2）Steady state shearing and time resolution orthogonal superposition rheometer test, time resolution orthogonal superposition are carried out to the sample after aging
The pre- shearing condition of rheometer test is：Pre-shear rate is 500 s-1, pre- shear time is 200 s, balances 800 s；Finally cutting
Cutting speed rate is 10 s-1Under conditions of carry out it is orthogonal（Orthogonal strain is 5%）Frequency sweep is repeated, the number of multiple scanning is 8 times, and 8 times
The frequency scanned every time is arranged with 1,2.15,4.57,10,21.38 and 45.71 rad/s as one in sweep time totally 1000 s
Group of frequencies, and according to frequency, scanning is complete single pass successively from low to high under every group of frequencies, obtains sweeping under every group of frequencies
The 6 groups of data retouched immediately enter scan round next time after the completion of scanning every time, until 8 scanning is completed, 48 groups of numbers are obtained
According to；Integrated testability environmental system temperature is 25 DEG C, carries out accurate temperature control to entirely testing using advanced Peltier system APS, control
Warm precision is ± 0.1 DEG C, and humidity is strict controlled in 40%, and compressed air air pressure reaches 0.5 MPa；
Test data is obtained into this shear rate using interpolation method（10 s-1）Under time viscoelastic spectra, and every time carry out the time
It needs to re-start sample the pre- shearing consistent with initial pre- shearing before differentiating orthogonal superposition oscillation rheometer test（500 s-1, 200 s）And balance（800 s）, to obtain the sample of original state；
When sweep time is 10 s, at 0.1rad/s, complex viscosity is 50.88 Pas, and storage modulus is 10.78 Pa, damage
Consumption modulus is 9.01 Pa；When sweep time is 1000 s, at 0.1 rad/s, complex viscosity is 12.67 Pas, energy storage mould
Amount is 154.54 Pa, and loss modulus is 124.83 Pa；
Compared to the method that general steady state shearing has to shear viscosity, this tests while obtaining viscosity and modulus information, whole
Storage modulus is more than loss modulus in range in a sweep time, shows as class solid behavior.
Embodiment 5
The three stage thixotropy test methods for characterizing artificial hectorite dispersion liquid rheology, are as follows：
（1）It takes artificial hectorite to be placed in and is placed with 24 h in 30 DEG C of vacuum drying chambers of anhydrous calcium chloride, precisely quickly weigh 1.5010g
Dry artificial hectorite is slowly added in the wide-mouth bottle equipped with stirrer and 48.5 mL ultra-pure waters, at 150 rpm on one side
Charging is stirred on one side, is fed and is completed after 4 min, screws bottle cap, is increased mixing speed to 500 rpm, is stirred 20 min and all remove
10 min of ice-bath ultrasonic（Ultrasonic power is 100 W, and supersonic frequency is 40 kHz）, transparent clear dispersion liquid is obtained, paraffin is used
Paper seals, and covers tightly bottle cap, is placed in 25 DEG C, and aging 2 days in the climatic chamber of 80 % obtains the artificial water that mass fraction is 3 %
Pyroxene gel sample；
（2）Steady state shearing and time resolution orthogonal superposition rheometer test, time resolution orthogonal superposition are carried out to the sample after aging
The pre- shearing condition of rheometer test is：Pre-shear rate is 500 s-1, pre- shear time is 200 s, balances 800 s；Finally cutting
Cutting speed rate is 0.1 s-1Under conditions of carry out it is orthogonal（Orthogonal strain is 1%）Frequency sweep is repeated, the number of multiple scanning is 8 times, and 8
Secondary sweep time, totally 1000 s, the frequency that setting scans every time were with 1,2.15,4.57,10,21.38 and 45.71 rad/s
One group of frequencies, and according to frequency, scanning is complete single pass successively from low to high under every group of frequencies, is obtained under every group of frequencies
6 groups of data of scanning immediately enter scan round next time after the completion of scanning every time, until 8 scanning is completed, are obtained 48 groups
Data；Integrated testability environmental system temperature is 25 DEG C, and accurate temperature control is carried out to entirely testing using advanced Peltier system APS,
Temperature-controlled precision is ± 0.1 DEG C, and humidity is strict controlled in 40%, and compressed air air pressure reaches 0.5 MPa；
Test data is obtained into this shear rate using interpolation method（0.1 s-1）Under time viscoelastic spectra, and in each carry out
Between differentiate orthogonal superposition oscillation rheometer test before need to re-start sample the pre- shearing consistent with initial pre- shearing（500
s-1, 200 s）And balance（800 s）, to obtain the sample of original state；
When sweep time is 10 s, at 0.1 rad/s, complex viscosity is 100.43 Pas, and storage modulus is 50.85 Pa,
Loss modulus is 43.22 Pa；When sweep time is 1000 s, at 0.1 rad/s, complex viscosity is 30.87 Pas, storage
Energy modulus is 249.72 Pa, and loss modulus is 154.85 Pa；
Compared to the method that general steady state shearing has to shear viscosity, this tests while obtaining viscosity and modulus information, whole
Storage modulus is more than loss modulus in range in a sweep time, shows as class solid behavior.
Embodiment 6
The three stage thixotropy test methods for characterizing artificial hectorite dispersion liquid rheology, are as follows：
（1）It takes artificial hectorite to be placed in and is placed with 24 h in 30 DEG C of vacuum drying chambers of anhydrous calcium chloride, precisely quickly weigh 1.5004
The artificial hectorite of g dryings is slowly added in the wide-mouth bottle equipped with stirrer and 48.5 mL ultra-pure waters, at 150 rpm on one side
Charging is stirred on one side, is fed and is completed after 4 min, screws bottle cap, is increased mixing speed to 500 rpm, is stirred 30 min and all remove
15 min of ice-bath ultrasonic（Ultrasonic power is 100 W, and supersonic frequency is 40 kHz）, transparent clear dispersion liquid is obtained, paraffin is used
Paper seals, and covers tightly bottle cap, is placed in 25 DEG C, and aging 2 days in the climatic chamber of 80 % obtains the artificial water that mass fraction is 3 %
Pyroxene gel sample；
（2）Steady state shearing and time resolution orthogonal superposition rheometer test, time resolution orthogonal superposition are carried out to the sample after aging
The pre- shearing condition of rheometer test is：Pre-shear rate is 1500 s-1, pre- shear time is 20 s, balances 1000 s；Finally cutting
Cutting speed rate is 0.01 s-1Under conditions of carry out it is orthogonal（Orthogonal strain is 1%）Frequency sweep is repeated, the number of multiple scanning is 8 times, and 8
Secondary sweep time, totally 1000 s, the frequency that setting scans every time were with 1,2.15,4.57,10,21.38 and 45.71 rad/s
One group of frequencies, and according to frequency, scanning is complete single pass successively from low to high under every group of frequencies, is obtained under every group of frequencies
6 groups of data of scanning immediately enter scan round next time after the completion of scanning every time, until 8 scanning is completed, are obtained 48 groups
Data；Integrated testability environmental system temperature is 25 DEG C, and accurate temperature control is carried out to entirely testing using advanced Peltier system APS,
Temperature-controlled precision is ± 0.1 DEG C, and humidity is strict controlled in 40%, and compressed air air pressure reaches 0.5 MPa；
Test data is obtained into this shear rate using interpolation method（0.01 s-1）Under time viscoelastic spectra, and in each carry out
Between differentiate orthogonal superposition oscillation rheometer test before need to re-start sample the pre- shearing consistent with initial pre- shearing（1500
s-1, 20 s）And balance（1000 s）, to obtain the sample of original state；
Sweep time is 10 s, and at 0.1 rad/s, complex viscosity is 300.24 Pas, and storage modulus is 180.51 Pa,
Loss modulus is 151.77 Pa；When sweep time is 1000 s, at 0.1 rad/s, complex viscosity is 50.83 Pas, storage
Energy modulus is 503.73 Pa, and loss modulus is 265.17 Pa；
Compared to the method that general steady state shearing has to shear viscosity, this tests while obtaining viscosity and modulus information, whole
Storage modulus is more than loss modulus in range in a sweep time, shows as class solid behavior.
Embodiment 7
The three stage thixotropy test methods for characterizing artificial hectorite dispersion liquid rheology, are as follows：
（1）It takes artificial hectorite to be placed in and is placed with 24 h in 30 DEG C of vacuum drying chambers of anhydrous calcium chloride, precisely quickly weigh 1.5012
The artificial hectorite of g dryings is slowly added in the wide-mouth bottle equipped with stirrer and 48.5 mL ultra-pure waters, at 100 rpm on one side
Charging is stirred on one side, is fed and is completed after 3 min, screws bottle cap, is increased mixing speed to 500 rpm, is stirred 30 min and all remove
15 min of ice-bath ultrasonic（Ultrasonic power is 100 W, and supersonic frequency is 40 kHz）, transparent clear dispersion liquid is obtained, paraffin is used
Paper seals, and covers tightly bottle cap, is placed in 25 DEG C, and aging 2 days in the climatic chamber of 80 % obtains the artificial water that mass fraction is 3 %
Pyroxene gel sample；
（2）Steady state shearing and time resolution orthogonal superposition rheometer test, time resolution orthogonal superposition are carried out to the sample after aging
The pre- shearing condition of rheometer test is：Pre-shear rate is 800 s-1, pre- shear time is 150 s, balances 900 s；Finally cutting
Cutting speed rate is 0.01 s-1Under conditions of carry out it is orthogonal（Orthogonal strain is 1%）Frequency sweep is repeated, the number of multiple scanning is 8 times, and 8
Secondary sweep time, totally 1000 s, the frequency that setting scans every time were with 1,2.15,4.57,10,21.38 and 45.71 rad/s
One group of frequencies, and according to frequency, scanning is complete single pass successively from low to high under every group of frequencies, is obtained under every group of frequencies
6 groups of data of scanning immediately enter scan round next time after the completion of scanning every time, until 8 scanning is completed, are obtained 48 groups
Data；Integrated testability environmental system temperature is 25 DEG C, and accurate temperature control is carried out to entirely testing using advanced Peltier system APS,
Temperature-controlled precision is ± 0.1 DEG C, and humidity is strict controlled in 40%, and compressed air air pressure reaches 0.5 MPa；
Test data is obtained into this shear rate using interpolation method（0.01 s-1）Under time viscoelastic spectra, and in each carry out
Between differentiate orthogonal superposition oscillation rheometer test before need to re-start sample the pre- shearing consistent with initial pre- shearing（800
s-1, 150 s）And balance（900 s）, to obtain the sample of original state；
Sweep time is 10 s, and at 0.1rad/s, complex viscosity is 257.42 Pas, and storage modulus is 145.97 Pa, damage
Consumption modulus is 128.14 Pa；When sweep time is 1000 s, at 0.1 rad/s, complex viscosity is 30.84 Pas, energy storage
Modulus is 452.94 Pa, and loss modulus is 223.52 Pa；
Compared to the method that general steady state shearing has to shear viscosity, this tests while obtaining viscosity and modulus information, whole
Storage modulus is more than loss modulus in range in a sweep time, shows as class solid behavior.
Embodiment 8
The three stage thixotropy test methods for characterizing artificial hectorite dispersion liquid rheology, are as follows：
（1）It takes artificial hectorite to be placed in and is placed with 24 h in 30 DEG C of vacuum drying chambers of anhydrous calcium chloride, precisely quickly weigh 1.5052
The artificial hectorite of g dryings is slowly added in the wide-mouth bottle equipped with stirrer and 48.5 mL ultra-pure waters, at 100 rpm on one side
Charging is stirred on one side, is fed and is completed after 3 min, screws bottle cap, is increased mixing speed to 500 rpm, is stirred 30 min and all remove
15 min of ice-bath ultrasonic（Ultrasonic power is 100 W, and supersonic frequency is 40 kHz）, transparent clear dispersion liquid is obtained, paraffin is used
Paper seals, and covers tightly bottle cap, is placed in 25 DEG C, and aging 2 days in the climatic chamber of 80 % obtains the artificial water that mass fraction is 3 %
Pyroxene gel sample；
（2）Steady state shearing and time resolution orthogonal superposition rheometer test, time resolution orthogonal superposition are carried out to the sample after aging
The pre- shearing condition of rheometer test is：Pre-shear rate is 1200 s-1, pre- shear time is 150 s, balances 1000 s；Finally exist
Shear rate is 0.01 s-1Under conditions of carry out it is orthogonal（Orthogonal strain is 1%）Frequency sweep is repeated, the number for repeating frequency sweep is 8 times,
And 8 sweep times totally 1000 s, it is one that each 1,2.15,4.57,10,21.38,45.71 rad/s of scan frequency, which is arranged,
Group scans sample successively from low to high under this class frequency according to frequency, this is complete single pass, obtains said frequencies
6 groups of data of lower scanning immediately enter scan round next time after scanning through every time, until 8 scanning is completed, are obtained 48
Group data；Integrated testability environmental system temperature is 25 DEG C, is precisely controlled using advanced Peltier system APS to entirely testing
Temperature, temperature-controlled precision are ± 0.1 DEG C, and humidity is strict controlled in 40%, and compressed air air pressure reaches 0.5 MPa；
Test data is obtained into this shear rate using interpolation method（0.01 s-1）Under time viscoelastic spectra, and in each carry out
Between differentiate orthogonal superposition oscillation rheometer test before need to re-start sample the pre- shearing consistent with initial pre- shearing（1200
s-1, 150 s）And balance（1000 s）, to obtain the sample of original state；
Sweep time is 10 s, and at 0.1 rad/s, complex viscosity is 201.53 Pas, and storage modulus is 126.95 Pa,
Loss modulus is 109.62 Pa；When sweep time is 1000 s, at 0.1 rad/s, complex viscosity is 26.26 Pas, storage
Energy modulus is 437.31 Pa, and loss modulus is 211.92 Pa；
Compared to the method that general steady state shearing has to shear viscosity, this tests while obtaining viscosity and modulus information, whole
Storage modulus is more than loss modulus in range in a sweep time, shows as class solid behavior.
Embodiment 9
The three stage thixotropy test methods for characterizing artificial hectorite dispersion liquid rheology, are as follows：
（1）It takes artificial hectorite to be placed in and is placed with 24 h in 30 DEG C of vacuum drying chambers of anhydrous calcium chloride, precisely quickly weigh 1.4987
The artificial hectorite of g dryings is slowly added in the wide-mouth bottle equipped with stirrer and 48.5 mL ultra-pure waters, at 100 rpm on one side
Charging is stirred on one side, is fed and is completed after 3 min, screws bottle cap, is increased mixing speed to 500 rpm, is stirred 30 min and all remove
15 min of ice-bath ultrasonic（Ultrasonic power is 100 W, and supersonic frequency is 40 kHz）, transparent clear dispersion liquid is obtained, paraffin is used
Paper seals, and covers tightly bottle cap, is placed in 25 DEG C, and aging 2 days in the climatic chamber of 80 % obtains the artificial water that mass fraction is 3 %
Pyroxene gel sample；
（2）Steady state shearing and time resolution orthogonal superposition rheometer test, time resolution orthogonal superposition are carried out to the sample after aging
The pre- shearing condition of rheometer test is：Pre-shear rate is 1500 s-1, pre- shear time is 20 s, balances 500 s；Finally cutting
Cutting speed rate is 0.01 s-1Under conditions of carry out it is orthogonal（Orthogonal strain is 1%）Frequency sweep is repeated, the number of multiple scanning is 8 times, and 8
Secondary sweep time, totally 1000 s, the frequency that setting scans every time were with 1,2.15,4.57,10,21.38 and 45.71 rad/s
One group of frequencies, and according to frequency, scanning is complete single pass successively from low to high under every group of frequencies, is obtained under every group of frequencies
6 groups of data of scanning immediately enter scan round next time after the completion of scanning every time, until 8 scanning is completed, are obtained 48 groups
Data；Integrated testability environmental system temperature is 25 DEG C, and accurate temperature control is carried out to entirely testing using advanced Peltier system APS,
Temperature-controlled precision is ± 0.1 DEG C, and humidity is strict controlled in 40%, and compressed air air pressure reaches 0.5 MPa；
Test data is obtained into this shear rate using interpolation method（0.01 s-1）Under time viscoelastic spectra, and in each carry out
Between differentiate orthogonal superposition oscillation rheometer test before need to re-start sample the pre- shearing consistent with initial pre- shearing（1500
s-1, 20 s）And balance（500 s）, to obtain the sample of original state；
When sweep time is 10 s, at 0.1 rad/s, complex viscosity is 150.34 Pas, and storage modulus is 88.62 Pa,
Loss modulus is 52.64 Pa；When sweep time is 1000 s, at 0.1 rad/s, complex viscosity is 14.76 Pas, storage
Energy modulus is 325.89 Pa, and loss modulus is 183.73 Pa；
Compared to the method that general steady state shearing has to shear viscosity, this tests while obtaining viscosity and modulus information, whole
Storage modulus is more than loss modulus in range in a sweep time, shows as class solid behavior.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitute, combination, should be
Equivalent substitute mode, is included within the scope of the present invention.
Claims (10)
1. a kind of three stage thixotropy test methods of characterization thixotropic fluid rheology, which is characterized in that touched in conjunction with three stages
It is denaturalized measuring technology and time resolution orthogonal superposition rheometer test technology carries out characterization test；
Specifically comprise the following steps：
（1）After thixotropic fluid after aging is completed loading on rheometer, pre- shear parameters, balance are set on rheometer
The shear rate of circumferencial direction, time resolution orthogonal superposition shake when time of repose, time resolution orthogonal superposition oscillation rheometer test
The small amplitude oscillatory shear parameter and multiple scanning number of vertical direction when swinging rheometer test；
（2）Start rheometer, proceed by test, and carries out all needing before time resolution orthogonal superposition oscillation rheometer test every time
Re-start step（1）The pre- shearing peace weighing apparatus being arranged；Test data is obtained, and is handled using interpolation method, show that difference is cut
The time viscoelastic modal data of sample under cutting speed rate different moments.
2. according to the method described in claim 1, it is characterized in that, step（1）In, the aging is in 25 DEG C of temperature and humidity
In the environment of 80% constant temperature and humidity, natural aging 1 ~ 4 day is stood.
3. according to the method described in claim 1, it is characterized in that, step（1）In, the pre- shear parameters include preshearing cutting speed
Rate and pre- shear time, setting pre-shear rate are 200 ~ 1500 s-1, it is 20 ~ 600 s that pre- shear time, which is arranged,.
4. according to the method described in claim 1, it is characterized in that, step（1）In, setting balance time of repose is 500 ~ 1000
s。
5. according to the method described in claim 1, it is characterized in that, step（1）In, time resolution orthogonal superposition oscillatory flow is set
The shear rate of circumferencial direction is 0.001 ~ 100 s when becoming test-1。
6. according to the method described in claim 1, it is characterized in that, step（1）In, the time resolution orthogonal superposition oscillatory flow
The small amplitude oscillatory shear parameter of vertical direction includes orthogonal strain when becoming test, and setting orthogonal strain is 1 %.
7. according to the method described in claim 1, it is characterized in that, step（1）In, setting multiple scanning number is 8 times, and 8
Totally 1000 s of secondary sweep time.
8. the method according to the description of claim 7 is characterized in that the frequency that scans every time of setting is with 1,2.15,4.57,10,
21.38 and 45.71 rad/s are a group of frequencies, and according to frequency, scanning is complete one successively from low to high under every group of frequencies
Secondary scanning obtains scanned under every group of frequencies 6 groups of data, scan round next time is immediately entered after the completion of scanning every time, until 8
Secondary scanning is completed, and 48 groups of data are obtained.
9. according to the method described in claim 1, it is characterized in that, step（2）In, in the test process, utilize interpolation method
Processing directly obtains the time resolution viscoelastic spectra in the multiple scanning total time under different shear rate.
10. according to the method described in claim 1, it is characterized in that, the environment temperature of entire test process is 25 DEG C, humidity is tight
Lattice control is in 60 % hereinafter, compressed air air pressure reaches 0.5 MPa.
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