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CN110057788B - Nano material absorbance test device, and stabilization phase test method, system and device - Google Patents

Nano material absorbance test device, and stabilization phase test method, system and device Download PDF

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CN110057788B
CN110057788B CN201910434631.7A CN201910434631A CN110057788B CN 110057788 B CN110057788 B CN 110057788B CN 201910434631 A CN201910434631 A CN 201910434631A CN 110057788 B CN110057788 B CN 110057788B
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absorbance
nano dispersion
dispersion liquid
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CN110057788A (en
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段兴汉
武桐
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Shanghai Jingruiyang Industrial Co ltd
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Abstract

The invention discloses a device for testing absorbance of a nano material, a method, a system and a device for testing a stabilization period. The absorbance test device comprises a rotary sample cabin, a slit grating, an avalanche photodiode sensor and a light beam generator. The rotary sample cabin can rotate in a horizontal plane; the light beam generator is arranged above the horizontal plane, and when the rotating sample cabin is positioned right below the light beam generator, the light beam can cover the nano dispersion liquid to be measured in the rotating sample cabin; the slit grating is arranged right below the horizontal plane relative to the light beam generator, and the avalanche photodiode sensor is arranged right below the slit grating. The absorbance test device can quickly measure the absorbance change conditions of the nano dispersion liquid at different moments. The method, the system and the device for testing the stabilization period of the nano dispersion provided by the invention can quickly determine the stability and the stabilization period of the dispersion according to the change of the light transmittance of the nano dispersion in the sample cabin, have high detection efficiency and small error, and are suitable for process production.

Description

Nano material absorbance test device, and stabilization phase test method, system and device
Technical Field
The invention relates to the field of nano dispersion liquid, in particular to a nano material absorbance testing device, a stabilization phase testing method, a system and a device.
Background
The stability of nano materials in a solvent is always a difficult point of material detection, in the field of academic research and research, the stability of suspension is usually indirectly represented by a Zeta potential, generally, an electrophoretic light scattering principle is utilized, charged particles move under the action of an external electric field, the movement of charges enables scattered light to generate frequency drift (Doppler frequency shift), and the electrophoretic mobility and the Zeta potential of the particles can be calculated by adopting a spectrum drift analysis technology. However, this method only shows the relative stability of the current systems and cannot infer the expiration date of the dispersion.
Disclosure of Invention
The invention aims to provide a device, a method, a system and a device for testing absorbance of nano dispersion, which can quickly determine the stability and the stabilization period of the nano dispersion according to the change of the light transmittance of the nano dispersion in a sample cabin, have high detection efficiency and small error and are suitable for process production.
In order to achieve the purpose, the invention provides the following scheme:
a nanodispersion absorbance test device, the absorbance test device comprising: the device comprises a rotary sample cabin, a slit grating, an avalanche photodiode sensor and a light beam generator; wherein,
the rotating sample cabin is used for containing nano dispersion liquid to be detected, and can rotate in a horizontal plane; the light beam generator is arranged above the horizontal plane, and when the rotary sample cabin is positioned right below the light beam generator, the light beam emitted by the light beam generator can cover the nano dispersion liquid to be detected in the rotary sample cabin; the slit grating is arranged below the horizontal plane opposite to the light beam generator, and the avalanche photodiode sensor is arranged right below the slit grating.
Optionally, the absorbance testing device further includes a Zeta potential measuring instrument, and the Zeta potential measuring instrument is used for measuring the Zeta potential of the to-be-tested nano dispersion liquid.
Optionally, the absorbance test device further comprises a centrifugal device, the rotating sample cabin comprises a sample cabin fixing support, a rotating fulcrum and a sample cabin, the sample cabin is fixedly arranged on the sample cabin fixing support, the sample cabin fixing support is fixedly connected with the rotating fulcrum, the centrifugal device is connected with the rotating fulcrum, and the centrifugal device drives the sample cabin fixing support to rotate through the rotating fulcrum so that the nano dispersion liquid to be tested, which is contained in the sample cabin, performs centrifugal motion.
Optionally, the sample chamber is a quartz tube with a diameter range of 1-10 mm.
Optionally, the light source wavelength emitted by the light beam generator is 400-2000 nm.
A nanodispersion stabilization phase test method for use with the absorbance test device, the stabilization phase test method comprising:
obtaining a Zeta potential value of the nano dispersion liquid to be detected;
judging whether the Zeta potential value is larger than +/-40 millivolts or not to obtain a judgment result;
when the judgment result shows that the avalanche photodiode sensor is in the positive state, acquiring transmitted light intensity and incident light intensity measured by the avalanche photodiode sensor at different moments;
determining the absorbance of the nano dispersion liquid to be detected at different moments according to the transmitted light intensity and the incident light intensity;
and determining the stabilization period of the nano dispersion liquid to be detected according to the absorbance at different moments.
Optionally, the determining the stabilization period of the to-be-detected nano dispersion liquid according to the absorbance at different times specifically includes:
drawing absorbance change curves at different moments;
selecting an inflection point of the absorbance change curve at the starting moment as a starting point;
selecting an inflection point of an absorbance change curve at the termination time as a termination point;
determining the moving distance of the nano dispersion particles to be detected according to the starting point and the ending point;
determining the moving speed of the particles relative to the liquid according to the moving distance, the starting time and the ending time;
determining the moving speed of the particles under one time of gravitational acceleration according to the ratio of the moving speed of the particles relative to the liquid to the gravitational acceleration;
and determining the stabilization period according to the moving speed of the particles under the acceleration of one time of gravity and the distance between the highest position of the liquid level in the sample chamber and the bottom of the sample chamber.
A nanodispersion stationary phase testing system for use with the absorbance testing device, the stationary phase testing system comprising:
the potential value acquisition module is used for acquiring a Zeta potential value of the nano dispersion liquid to be detected;
the judgment module is used for judging whether the Zeta potential value is larger than +/-40 millivolts or not and obtaining a judgment result;
the light intensity acquisition module is used for acquiring the transmitted light intensity and the incident light intensity measured by the avalanche photodiode sensor at different moments when the judgment result shows yes;
the absorbance determining module is used for determining the absorbance of the nano dispersion liquid to be detected at different moments according to the transmitted light intensity and the incident light intensity;
and the stabilization phase determining module is used for determining the stabilization phase of the nano dispersion liquid to be detected according to the absorbance at different moments.
A nanodispersion stationary phase testing apparatus, the stationary phase testing apparatus comprising: the absorbance test device and the processor are connected with the Zeta potential measuring instrument and the avalanche photodiode sensor, and the processor is used for executing the steps of the nano dispersion liquid stabilization period test method.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention provides a device for testing absorbance of nano dispersion liquid, which comprises: a rotating sample chamber, a slit grating, an avalanche photodiode sensor, and a light beam generator. The rotating sample cabin is used for containing nano dispersion liquid to be detected and can rotate in a horizontal plane; the light beam generator is arranged above a horizontal plane, and when the rotary sample cabin is positioned right below the light beam generator, the light beam generated by the light beam generator can cover the nano dispersion liquid to be detected in the rotary sample cabin; the slit grating is arranged right below the horizontal plane relative to the light beam generator, and the avalanche photodiode sensor is arranged right below the slit grating. By adopting the absorbance test device provided by the invention, the absorbance change conditions of the nano dispersion liquid at different moments can be rapidly measured.
On the basis, the method, the system and the device for testing the stabilization period of the nano dispersion can quickly determine the stability and the stabilization period of the dispersion according to the change of the light transmittance of the nano dispersion in the sample cabin, have high detection efficiency and small error, and are suitable for process production.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
Fig. 1 is a schematic structural diagram of a nanodispersion absorbance testing apparatus provided in embodiment 1 of the present invention;
FIG. 2 is a flow chart of a method for testing the stationary phase of a nanodispersion according to example 2 of the present invention;
FIG. 3 is a graph showing the variation of absorbance provided in example 2 of the present invention;
fig. 4 is a block diagram of a nanodispersion stability period testing system according to embodiment 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a device, a method, a system and a device for testing absorbance of nano dispersion, which can quickly determine the stability and the stabilization period of the nano dispersion according to the change of the light transmittance of the nano dispersion in a sample cabin, have high detection efficiency and small error and are suitable for process production.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1:
fig. 1 is a schematic structural diagram of a nanodispersion absorbance testing apparatus provided in embodiment 1 of the present invention. As shown in fig. 1, the absorbance test device includes: a rotating sample chamber 1, a slit grating 2, an avalanche photodiode sensor 3 and a light beam generator 4.
The rotating sample cabin 1 is used for containing nano dispersion liquid to be detected, and the rotating sample cabin can rotate in a horizontal plane. The light beam generator 4 is arranged above the horizontal plane, the rotating sample cabin 1 is located under the light beam generator 4, and light beams emitted by the light beam generator 4 can cover the nano dispersion liquid to be measured in the rotating sample cabin. The slit grating 2 is arranged below the horizontal plane opposite to the light beam generator 4, and the avalanche photodiode sensor 3 is arranged right below the slit grating 2.
As a preferable mode, the absorbance testing device further includes a Zeta potential measuring instrument, and the Zeta potential measuring instrument is used for measuring the Zeta potential of the nano dispersion to be tested.
In this embodiment, absorbance test device still includes centrifugal equipment, rotatory sample cabin includes sample cabin fixed bolster 11, rotatory fulcrum 12 and sample cabin 13, sample cabin 13 set firmly in on the sample cabin fixed bolster 11, sample cabin fixed bolster 11 with rotatory fulcrum 12 fixed connection, centrifugal equipment 5 with rotatory fulcrum 12 is connected, centrifugal equipment 5 passes through rotatory fulcrum 12 drives sample cabin fixed bolster 11 is rotatory, so that hold in the sample cabin 13 the nanometer dispersion that awaits measuring carries out centrifugal motion.
In this embodiment, the sample chamber is a high transmittance quartz tube with a diameter range of 1-10 mm. The light beam generator 4 emits light beams with a wavelength of 400-2000 nm. The centrifugation rate of the centrifugal device was 1000-9000 rpm. The Avalanche Photodiode (APD) sensor is parallel to the incident light source, and the detection accuracy can be improved by simultaneously analyzing and comparing multiple groups of data.
Example 2:
fig. 2 is a flowchart of a method for testing a stability period of a nanodispersion provided in embodiment 2 of the present invention. As shown in fig. 2, the stationary phase test method is used in the absorbance test device according to example 1, and includes:
step 201: and obtaining the Zeta potential value of the nano dispersion liquid to be detected.
Step 202: and judging whether the Zeta potential value is larger than +/-40 millivolts or not, and obtaining a judgment result.
Step 203: and when the judgment result shows yes, acquiring the transmitted light intensity and the incident light intensity measured by the avalanche photodiode sensor at different moments.
Step 204: and determining the absorbance of the nano dispersion liquid to be detected at different moments according to the transmitted light intensity and the incident light intensity. The calculation formula of the absorbance is as follows:
Figure BDA0002070132350000061
Etdenotes the absorbance at time t, ItRepresenting the transmitted light intensity at time t, I0tRepresenting the intensity of the incident light at time t. Under the same centrifugal rate, the smaller the change rate of the absorbance of different samples is, the better the stability of the dispersion liquid is; for the same sample, the smaller the rate of change in absorbance, the better the dispersion stability, as the centrifugation rate increased.
Step 205: and determining the stabilization period of the nano dispersion liquid to be detected according to the absorbance at different moments.
Specifically, the step 205: determining the stabilization period of the nano dispersion liquid to be detected according to the absorbance at different moments, which specifically comprises the following steps:
the absorbance change curves were plotted at different times, as shown in fig. 3.
And selecting the inflection point of the absorbance change curve at the starting moment as a starting point. In this embodiment, the starting point is a point a on the curve at time 1.
And selecting the inflection point of the absorbance change curve at the termination time as the termination point. In this embodiment, the termination point is a point B on the curve at time 4.
And determining the moving distance of the nano dispersion particles to be detected, namely the distance between the point A and the point B according to the starting point and the ending point.
And determining the moving speed of the particles relative to the liquid according to the moving distance, the starting time and the ending time, wherein the moving time is the time from the time 1 to the time 4.
And determining the moving speed of the particles under the acceleration of gravity by the ratio of the moving speed of the particles relative to the liquid to the acceleration of gravity.
And determining a stabilization period according to the moving speed of the particles under the acceleration of gravity of one time and the distance between the highest position of the liquid level in the sample chamber and the bottom of the sample chamber.
The expression of stokes law is: f is 6 pi η vR, F is the resistance experienced by the particle, η is the viscosity coefficient, v is the rate of movement of the particle relative to the liquid, and R is the particle radius. The formula for the relative centrifugal force is: RCF 1.118 × 10-5×n2Xrxg, n is the centrifugal rotation speed, r is the rotation radius, g is the gravitational acceleration, RCF is the relative centrifugal force, and is numerically equal to the resistance F to the particles. Let 6 pi η vR be 1.118 × 10-5×n2Xr × g, a binary function v ═ f (n, g) can be obtained, and solving the binary function can calculate the moving speed of the particles under one-time gravity acceleration.
This example first simply judges the stability of the nanodispersion according to the value of Zeta potential. Under a certain PH value, if the Zeta potential value is less than +/-40 millivolts, the nano dispersion liquid can be determined to be an unstable material, if the Zeta potential value is greater than +/-40 millivolts, the stable period of the nano dispersion liquid is calculated through the change of light transmittance on the basis of an accelerated centrifugal test, the detection efficiency is dozens of times of that of the traditional equipment, and the nano dispersion liquid is very suitable for fast detection and fast adjustment of various industrial production line products, and achieves the purposes of cost reduction and efficiency improvement.
Example 3:
fig. 4 is a block diagram of a nanodispersion stability period testing system according to embodiment 3 of the present invention. As shown in fig. 4, the stationary phase test system is used in the absorbance test device according to embodiment 1, and includes:
and the potential value acquisition module 301 is used for acquiring a Zeta potential value of the nano dispersion liquid to be detected.
And the judging module 302 is configured to judge whether the Zeta potential value is greater than ± 40 mv, and obtain a judgment result.
And the light intensity obtaining module 303 is configured to obtain the intensity of the transmitted light and the intensity of the incident light measured by the avalanche photodiode sensor at different times when the determination result indicates yes.
And an absorbance determination module 304, configured to determine absorbance of the nano dispersion to be detected at different times according to the intensity of the transmitted light and the intensity of the incident light.
And a stabilization period determining module 305, configured to determine a stabilization period of the to-be-detected nano dispersion liquid according to the absorbance at different times.
Example 4:
a nanodispersion stationary phase testing apparatus, the stationary phase testing apparatus comprising: the absorbance test device and the processor of embodiment 1, wherein the processor is connected with a Zeta potential measuring instrument and the avalanche photodiode sensor, and the processor is used for executing the steps of the nano dispersion stability period test method of embodiment 2.
The test conditions of the carbon nano tube NMP solution for the stability period test by adopting the nano dispersion liquid stability period test device provided by the invention are as follows:
the carbon nano tube NMP solution concentration is 5%, and the Zeta potential measurement result shows that: the Zeta potential is-43 mv at PH 9. Loading the solution into a 5mm diameter quartz tube, selecting 680nm as incident light source, accelerating and centrifuging at 1500rpm, and moving the particles at 3.5 × 10 under one time of gravitational acceleration-9m/s, the absorbance change rate is 0.9, the test time is 0.5h, and the sample stabilization period is calculated to be about 330 days. Compared with an actual standing experiment, the sample is layered after ten months, and the layering is close to the calculation result of the application.
The test conditions of the conducting silver paste stability period test by adopting the nano dispersion liquid stability period test device provided by the invention are as follows:
the concentration of the conductive silver paste is 90%, and the Zeta potential measurement result shows that: at a pH of 7, the Zeta potential was-63 mV. Loading the solution into a quartz tube with a diameter of 10mm, selecting an incident light source of 1200nm, accelerating and centrifuging at 4500rpm, and moving the particles at a speed of 3.2 x 10 under one-time gravitational acceleration-11m/s, the absorbance change rate is 0.02, the test time is 2.5h, and the calculated sample stabilization period exceeds 10 years. Compared with an actual standing experiment, the stable period of the sample in a normal storage environment exceeds 12 years.
The invention mainly provides a novel dispersion stability testing system, particularly relates to a stable nano material, and rapidly deduces the stability and the stable period of a dispersion according to the change of the light transmittance of the dispersion in a sample cabin by means of a Zeta potential and a centrifugal accelerating device, wherein the testing efficiency of the system exceeds that of all the existing detection technologies, and the system is suitable for process production.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.

Claims (8)

1. A nanodispersion absorbance test device, wherein the absorbance test device comprises: the device comprises a rotary sample cabin, a slit grating, an avalanche photodiode sensor and a light beam generator; wherein,
the rotating sample cabin is used for containing nano dispersion liquid to be detected, and can rotate in a horizontal plane; the light beam generator is arranged above the horizontal plane, and when the rotary sample cabin is positioned right below the light beam generator, the light beam emitted by the light beam generator can cover the nano dispersion liquid to be detected in the rotary sample cabin; the slit grating is arranged below the horizontal plane opposite to the light beam generator, the avalanche photodiode sensor is arranged right below the slit grating, and the avalanche photodiode sensor is parallel to the incident light source;
the absorbance testing device also comprises a Zeta potential measuring instrument, and the Zeta potential measuring instrument is used for measuring the Zeta potential of the nano dispersion liquid to be tested;
judging whether the Zeta potential value is larger than +/-40 millivolts or not to obtain a judgment result;
when the judgment result shows that the avalanche photodiode sensor is in the positive state, acquiring transmitted light intensity and incident light intensity measured by the avalanche photodiode sensor at different moments;
determining the absorbance of the nano dispersion liquid to be detected at different moments according to the transmitted light intensity and the incident light intensity;
and determining the stabilization period of the nano dispersion liquid to be detected according to the absorbance at different moments.
2. The absorbance test device according to claim 1, further comprising a centrifugal device, wherein the rotating sample chamber comprises a sample chamber fixing support, a rotating fulcrum and a sample chamber, the sample chamber is fixedly arranged on the sample chamber fixing support, the sample chamber fixing support is fixedly connected with the rotating fulcrum, the centrifugal device is connected with the rotating fulcrum, and the centrifugal device drives the sample chamber fixing support to rotate through the rotating fulcrum, so that the nano dispersion to be tested contained in the sample chamber performs centrifugal motion.
3. The absorbance test device according to claim 2, wherein the sample chamber is a quartz tube having a diameter in the range of 1-10 mm.
4. The absorbance test device according to claim 2, wherein the light source wavelength emitted from the light beam generator is 400-2000 nm.
5. A method for testing the stationary phase of a nanodispersion, wherein the method for testing the stationary phase is used in the absorbance test device according to any one of claims 1 to 4, and the method for testing the stationary phase comprises:
obtaining a Zeta potential value of the nano dispersion liquid to be detected;
judging whether the Zeta potential value is larger than +/-40 millivolts or not to obtain a judgment result;
when the judgment result shows that the avalanche photodiode sensor is in the positive state, acquiring transmitted light intensity and incident light intensity measured by the avalanche photodiode sensor at different moments;
determining the absorbance of the nano dispersion liquid to be detected at different moments according to the transmitted light intensity and the incident light intensity;
and determining the stabilization period of the nano dispersion liquid to be detected according to the absorbance at different moments.
6. The method for testing the stable phase of the dispersion liquid according to claim 5, wherein the determining the stable phase of the nano dispersion liquid to be tested according to the absorbance at different moments specifically comprises:
drawing absorbance change curves at different moments;
selecting an inflection point of the absorbance change curve at the starting moment as a starting point;
selecting an inflection point of an absorbance change curve at the termination time as a termination point;
determining the moving distance of the nano dispersion particles to be detected according to the starting point and the ending point;
determining the moving speed of the particles relative to the liquid according to the moving distance, the starting time and the ending time;
determining the moving speed of the particles under one time of gravitational acceleration according to the ratio of the moving speed of the particles relative to the liquid to the gravitational acceleration;
and determining the stabilization period according to the moving speed of the particles under the acceleration of one time of gravity and the distance between the highest position of the liquid level in the sample chamber and the bottom of the sample chamber.
7. A nanodispersion stationary phase testing system for use with the absorbance testing device of any one of claims 1-4, the stationary phase testing system comprising:
the potential value acquisition module is used for acquiring a Zeta potential value of the nano dispersion liquid to be detected;
the judgment module is used for judging whether the Zeta potential value is larger than +/-40 millivolts or not and obtaining a judgment result;
the light intensity acquisition module is used for acquiring the transmitted light intensity and the incident light intensity measured by the avalanche photodiode sensor at different moments when the judgment result shows yes;
the absorbance determining module is used for determining the absorbance of the nano dispersion liquid to be detected at different moments according to the transmitted light intensity and the incident light intensity;
and the stabilization phase determining module is used for determining the stabilization phase of the nano dispersion liquid to be detected according to the absorbance at different moments.
8. A nanodispersion stationary phase testing apparatus, comprising: the absorbance test device and processor as claimed in any one of claims 1 to 4, said processor being connected to a Zeta potential meter and said avalanche photodiode sensor, said processor being adapted to perform the steps of the nanodispersion stationary phase test method as claimed in any one of claims 5 to 6.
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CN107349116A (en) * 2017-07-11 2017-11-17 广州大学 One kind cladding sun-screening agent nano-lipid carrier and preparation method and application
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