CN114062399B - Quantitative characterization method for dispersibility of spherical nano powder - Google Patents
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Abstract
The invention discloses a quantitative characterization method of the dispersibility of spherical nano powder. The method comprises the following steps: s1, preparing a spherical nano powder sample; s2, acquiring an electron microscope image of the spherical nano powder by using an electron microscope, and processing to obtain an electron microscope picture; s3, calculating the fractal dimension of the electron microscope picture by adopting a box algorithm. The method realizes the quantitative characterization of the dispersibility of the spherical nano powder, and has the advantages of simple operation, high analysis speed, low subjective degree, high reliability and strong representativeness.
Description
Technical Field
The invention relates to a quantitative characterization method of the dispersibility of spherical nano powder.
Background
Nanomaterial refers to a material having at least one dimension in a three-dimensional space in a nanoscale range or constituted by them as basic units. The nano material has quantum size effect, small size effect, surface effect and macroscopic quantum tunnel effect due to the fact that the particle size enters the nano level, and further shows a plurality of special properties, and particularly has wide application prospects in the aspects of catalyzing, filtering, light absorbing, medical magnetic media, new materials and the like. The nano material has unique mechanical, optical, thermal, electric, magnetic, adsorption, gas-sensitive and other properties, and the addition of nano powder into the traditional material greatly improves the performance. However, in the practical application process, the nano particles have small particle size and high surface activity, so that the nano particles are easy to agglomerate to form agglomerates with larger size, and the application of nano powder and the preparation of corresponding nano materials are seriously hindered.
The current research on the agglomeration behavior of nano powder is mainly focused on how to alleviate the behavior, and the research on the generation mechanism of the behavior is less. Since one often ignores the fractal aggregation or agglomeration morphology of the nano-powder material, few studies have studied their own aggregation structure from the particles themselves. Therefore, how to explore the geometrical shape of the nano powder material aggregate in the preparation process, analyze the aggregation effect from the microstructure, explore the fractal geometrical factors influencing the aggregate, and is a crucial step for solving the aggregation problem of the nano powder material. The present characterization of the agglomeration behavior (or dispersibility) of the nano powder material is mainly in a qualitative level, mainly described by subjective feeling, and the agglomeration degree of the nano powder is usually determined to be serious or good only by observation. How to quantitatively characterize the agglomeration behavior degree is still relatively blank, and the comparison analysis of different nano powder cannot be performed without a unified quantitative standard.
Disclosure of Invention
The invention provides a quantitative characterization method for the dispersibility of spherical nano powder in order to overcome the defect that the agglomeration behavior degree of the spherical nano powder material is not quantitatively characterized in the prior art. The quantitative characterization method of the dispersibility of the spherical nano powder has the advantages of simple operation, high analysis speed, low subjective degree, high reliability and strong representativeness.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a quantitative characterization method of the dispersibility of spherical nano powder, which comprises the following steps:
s1, preparing a spherical nano powder sample;
s2, acquiring an electron microscope image of the spherical nano powder by using an electron microscope, and processing to obtain an electron microscope picture;
s3, calculating the fractal dimension of the electron microscope picture by adopting a box algorithm.
In the present invention, the spherical nano powder may be spherical nano powder of a conventional material, for example, silica spherical nano powder, titania spherical nano powder, iron oxide spherical nano powder or copper oxide spherical nano powder.
In the present invention, the particle diameter of the spherical nano-powder is preferably 5 to 50nm, for example, 7nm or 25nm.
In step S1, the spherical-shaped nano-powder sample may be a single spherical-shaped nano-powder or a composite material including spherical-shaped nano-powder. And when the spherical nano powder sample is a composite material containing spherical nano powder, quantitatively characterizing the agglomeration condition of the spherical nano powder in the composite material. The composite material containing the spherical nano powder is, for example, silicone rubber containing the spherical nano powder.
In step S1, the spherical nano powder sample may be prepared according to conventional requirements of corresponding electron microscope photographing.
When the electron microscope is a transmission electron microscope, the preparation method of the spherical nano powder sample may be a dispersion method or an ultra-thin section method.
When the spherical nano powder sample is a single spherical nano powder, a dispersion method is preferably used. Wherein the general operation of the dispersion method comprises: dispersing the spherical nano powder in a solvent to obtain spherical nano powder dispersion liquid; and (3) dripping the spherical nano powder dispersion liquid on a copper mesh, and drying to obtain the spherical nano powder sample. The solvent may be selected according to the spherical nano powder, for example, absolute ethanol. The dispersion is preferably an ultrasonic dispersion. The dripping is preferably performed using a pipette. The drying is preferably by irradiation with an ultraviolet lamp.
For example, when the spherical nano-powder is a silica spherical nano-powder, the preparation method of the silica spherical nano-powder sample comprises the following steps: 1mg of silicon dioxide spherical nano powder is weighed, placed into a centrifuge tube, added with 1mL of absolute ethyl alcohol, dispersed for 10min by ultrasonic, absorbed by a liquid-transferring gun, dripped on a copper net, 1-2 drops of the dispersed liquid are dripped, and the silicon dioxide spherical nano powder sample is obtained by irradiation and drying for 15min by an ultraviolet lamp.
When the spherical nano-powder sample is a composite material comprising spherical nano-powder, a slicing method is preferably used. Wherein the general operation of the slicing method comprises: slicing the composite material containing the spherical nano powder by adopting a frozen ultrathin slicer, putting the cut slice on a knife edge, and then fishing the slice by clamping a copper mesh dipped with ethanol by using forceps, or fishing the slice by using a sample fishing ring dipped with saturated concentration sucrose and leaning on the copper mesh.
In step S2, the electron microscope may be a conventional electron microscope in the art, for example, a Transmission Electron Microscope (TEM) or a Scanning Electron Microscope (SEM).
In step S2, preferably, the specific operation of acquiring the electron microscope image of the spherical nano powder by using the electron microscope is as follows: after global observation and analysis are carried out on the morphology of the spherical nano powder sample, an area with the aggregate morphology which can most reflect the morphology features of the sample is selected for shooting, and an electron microscope image of the spherical nano powder is obtained.
In step S2, the magnification of the electron microscope image is preferably 10000 to 100000 times, for example 100000 times. The magnification of the images for comparison analysis was the same for the same batch.
In step S2, the scale of the electron microscope image is preferably 50 to 500nm.
In step S2, the processing is preferably such that the electron microscope picture meets the following requirements: contrast 100%, brightness-5%, definition-5%, saturation 100%.
In step S2, preferably, the electron microscope image is in TIFF format.
In step S3, the specific operation of calculating the fractal dimension of the electron microscope picture by using a box algorithm includes:
(1) Importing the electron microscope picture into software, and inputting the box size r i Is defined by the range of (2);
(2) Counting the number N of pixel points respectively contained in each box size within the box size range by adopting an iteration method i ；
(3) By logr i On the abscissa, log N i Fitting to obtain an empirical curve with the ordinate, wherein the fitting formula of the empirical curve is log N i ＝Dlogr i The slope D of the empirical curve is the fractal dimension.
Preferably, the box dimension r i Is in the range r min ≤r i ≤r max Wherein, the r min The diameter of the individual particles of the spherical nano powder is the diameter of the r max The size of the largest aggregate in the electron microscope picture.
In the invention, after the fractal dimension of the electron microscope picture is obtained, the fractal dimension is compared with the aggregation degree of the spherical nano powder in the electron microscope picture, and the relationship between the fractal dimension and the aggregation condition of the spherical nano powder is obtained through analysis, so that the quantitative representation of the dispersibility of the spherical nano powder is realized.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred examples of the invention.
The reagents and materials used in the present invention are commercially available.
The invention has the positive progress effects that:
1. according to the quantitative characterization method for the dispersibility of the spherical nano powder, the aggregation effect of the spherical nano powder is analyzed from a microstructure, the fractal geometric factors influencing the aggregate are explored, the structure and fractal properties of the aggregate are represented in an electron microscope image, the important three-dimensional geometric properties are obtained directly from the image or from the geometric properties measured by standard image characterization software, and the aggregation condition of the spherical nano powder is quantified by using the value of the fractal dimension, so that the reliability is high and the representativeness is strong.
2. The invention uses computer to assist in image analysis, has simple and easily obtained operation, can easily evaluate a large number of particles and clusters, has higher analysis speed and lower subjective degree than the single analysis, can directly convert picture information into data for quantitative comparison, converts agglomeration and dispersion conditions of spherical nano powder which cannot be qualitatively analyzed into data, and can perform longitudinal and transverse comparison.
Drawings
FIG. 1 is a transmission electron microscope image (A-1 and B-1) of the silica sphere nano powder of example 1 of the present invention and an electron microscope image (A-2 and B-2) obtained after the treatment.
FIG. 2 is a transmission electron microscope image (A-1 and B-1) of the spherical nano-powder of titanium dioxide of example 2 of the present invention and an electron microscope image (A-2 and B-2) obtained after the treatment.
Fig. 3 is a transmission electron microscope image of an ultrathin section of a silicone rubber composite containing different mass fractions of spherical silica nano-powder in example 3 of the present invention.
Fig. 4 is the fractal dimension of ultrathin sections of silicone rubber composite containing different mass fractions of spherical silica nanopowder in example 3 of the invention.
Detailed Description
The present invention will be described in detail with reference to the following examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It is noted herein that the following examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as will be apparent to those skilled in the art upon examination of the following, certain essential modifications and adaptations of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
Example 1
Quantitatively characterizing the dispersibility of the silica spherical nano powder:
s1, weighing 1mg of AEROSIL 380 silica spherical nano powder (particle size is 7 nm) of German winning brand, weighing 1mL of absolute ethyl alcohol, placing into a 3mL centrifuge tube, performing ultrasonic dispersion for 10min, taking a small amount of dispersion liquid by a liquid-transferring gun, dripping 1-2 drops on a copper net, and performing irradiation drying for 15min by an ultraviolet lamp to obtain a silica spherical nano powder sample.
S2, under a transmission electron microscope, after overall observation and analysis are carried out on the appearance of the whole sample, two areas A and B are selected for shooting, so that an electron microscope image (shown in figure 1) is obtained, the magnification is 100000 times, and the scale is 50nm; then, the shot image is processed to obtain an electron microscope picture which meets the following requirements: contrast 100%, brightness 5%, definition 5%, saturation 100%; the format is TIFF.
S3, calculating the fractal dimension of the electron microscope picture by adopting a box algorithm:
(1) The electron microscope picture is imported into software, and the box size r is input i Range r of (2) min ≤r i ≤r max Wherein r is min Diameter r of individual particles of spherical nano-powder max The size of the largest aggregate in the electron microscope picture;
(2) Counting each box size r in the box size range by adopting an iterative method i The number of pixel points N contained in each i ；
(3) By logr i On the abscissa, log N i The empirical curve is obtained by fitting with the ordinate, and the fitting formula is logN i ＝Dlogr i The slope D of the empirical curve is the fractal dimension.
Comparing the fractal dimension with the aggregation degree of the spherical nano powder in the electron microscope picture, and obtaining the relationship between the fractal dimension and the aggregation condition of the spherical nano powder through analysis to realize the quantitative characterization of the dispersibility of the spherical nano powder.
Calculated as described above, the fractal dimension corresponding to a-1 and a-2 in fig. 1 is 1.52, the fractal dimension corresponding to B-1 and B-2 in fig. 1 is 1.64, and the fractal dimension corresponding to region a is lower than the fractal dimension corresponding to region B. As can be seen from fig. 1, the silica dispersion degree in the region a is higher than that in the region B. That means that the higher the fractal dimension, the more severe the agglomeration thereof, and the worse the dispersibility.
Example 2
Quantitatively characterizing the dispersibility of the titanium dioxide spherical nano powder:
s1, weighing 1mg of titanium dioxide spherical nano powder (with the particle size of 25 nm), weighing 1mL of absolute ethyl alcohol, placing into a 3mL centrifuge tube, performing ultrasonic dispersion for 10min, taking a small amount of dispersion by a liquid-transferring gun, dripping 1-2 drops of dispersion liquid onto a copper mesh, and performing irradiation drying for 15min by an ultraviolet lamp to obtain a titanium dioxide spherical nano powder sample.
S2, under a transmission electron microscope, after overall observation and analysis are carried out on the appearance of the whole sample, two areas A and B are selected for shooting, so that an electron microscope image (shown in FIG. 2) is obtained, the magnification is 100000 times, and the scale is 50nm; then, the shot image is processed to obtain an electron microscope picture which meets the following requirements: contrast 100%, brightness 5%, definition 5%, saturation 100%; the format is TIFF.
S3, calculating the fractal dimension of the electron microscope picture by adopting a box algorithm:
(1) The electron microscope picture is imported into software, and the box size r is input i Range r of (2) min ≤r i ≤r max Wherein r is min Diameter r of individual particles of spherical nano-powder max The size of the largest aggregate in the electron microscope picture;
(2) Counting each box size r in the box size range by adopting an iterative method i The number of pixel points N contained in each i ；
(3) By logr i On the abscissa, log N i The empirical curve is obtained by fitting with the ordinate, and the fitting formula is logN i ＝Dlogr i The slope D of the empirical curve is the fractal dimension.
Comparing the fractal dimension with the aggregation degree of the spherical nano powder in the electron microscope picture, and obtaining the relationship between the fractal dimension and the aggregation condition of the spherical nano powder through analysis to realize the quantitative characterization of the dispersibility of the spherical nano powder.
Calculated according to the above method, the fractal dimension corresponding to the A-1 and the A-2 in FIG. 2 is 1.56, the fractal dimension corresponding to the B-1 and the B-2 in FIG. 2 is 1.45, and the fractal dimension of the area A is higher than that of the area B. As can be seen from fig. 2, the degree of dispersion of titanium dioxide in zone a is less than that in zone B. Again, the fractal dimension was shown to be inversely related to the degree of dispersion of the spherical nano-powder material and positively related to its degree of aggregation. This is consistent with the regularity of the spherical silica nanopowder in example 1, the lower the fractal dimension, the better the silica dispersibility, the negative correlation between the fractal dimension and the silica dispersibility.
Example 3
Quantitatively characterizing the agglomeration condition of the silicon dioxide spherical nano powder in the silicon rubber:
s1, preparing a silicon rubber sample containing silicon dioxide spherical nano powder:
(1) The silicon rubber composite material is prepared by mixing the silicon dioxide spherical nano powder in the example 1 with silicon rubber, wherein the addition amount of the silicon dioxide spherical nano powder is 5%,10%,15% and 20% respectively; specifically:
(1) respectively treating the silicon dioxide spherical nano powder and raw rubber at 120 ℃ for 2 hours;
(2) mixing raw rubber (100 parts), hydroxyl silicone oil (1.5 parts) and silicon dioxide spherical nano powder (30 parts) uniformly on a double-roller mill according to different formula proportions, wherein the temperature of a roller cannot exceed 50 ℃, cutting for several times in the mixing process, and performing operations such as triangular packaging and the like to accelerate the uniform dispersion of filler in sizing materials; mixing for 2-10 min for each additive is added, wherein the mixing time mainly depends on the amounts of sizing material and filler; finally, thinning out the sheet, and carrying out heat treatment on the mixed rubber in a baking oven at 170 ℃ for 2 hours;
(3) the vulcanizing agent is added in a back refining way, namely double-double (1.0 percent) is calculated according to the raw rubber amount, and the sheet is formed; after the rubber is mixed, the next day of plate vulcanization, compression molding and forming are carried out, the vulcanization temperature is set to 175 ℃, the time is set to 5min, and the pressure is generally selected from 3-10 MPa (the pressure is related to the plasticity of the silicon rubber, the mold structure and the thickness of vulcanized rubber); and after demoulding, placing the vulcanized rubber sheet on a flat table top, cooling to room temperature, and standing for more than 12 hours to obtain the silicon rubber composite material.
(2) The silicon rubber composite material is subjected to low-temperature frozen slicing treatment to prepare ultrathin slices, and specifically: firstly, cutting a silicon rubber composite material into blocks with the length of 1cm, the width of 0.5cm and the height of 0.3cm, roughly repairing the blocks at room temperature, and then placing the blocks into a frozen ultrathin slicing machine with the temperature set in advance for block repairing and slicing; and (3) taking out the cut slice on a knife edge, and then fishing out the slice by using forceps through a copper mesh dipped with ethanol, or fishing out the slice by using a sample fishing ring dipped with sucrose with saturated concentration, and leaning against the copper mesh, thus obtaining the silicon rubber sample containing the silicon dioxide spherical nano powder.
S2, under a transmission electron microscope, after overall observation and analysis are carried out on the appearance of the whole sample, an area of which the aggregate form can most reflect the appearance characteristics of the sample is selected for shooting, the magnification is 100000 times, and the scale is 500nm; then, the shot image is processed to enable the electron microscope picture to be in a TIFF format, and the following requirements are met: contrast 100%, brightness-5%, definition-5%, saturation 100%.
S3, calculating the fractal dimension of the electron microscope picture by adopting a box algorithm:
(1) The electron microscope picture is imported into software, and the box size r is input i Range r of (2) min ≤r i ≤r max Wherein r is min Diameter r of individual particles of spherical nano-powder max The size of the largest aggregate in the electron microscope picture;
(2) Counting each box size r in the box size range by adopting an iterative method i The number of pixel points N contained in each i ；
(3) By logr i On the abscissa, log N i The ordinate is fitted to obtain an empirical curve, and the fitting formula is thatlogN i ＝Dlogr i The slope D of the empirical curve is the fractal dimension.
Comparing the fractal dimension with the aggregation degree of the spherical nano powder in the electron microscope picture, and obtaining the relationship between the fractal dimension and the aggregation condition of the spherical nano powder through analysis to realize the quantitative characterization of the dispersibility of the spherical nano powder.
Fig. 3 is a transmission electron microscope image of an ultrathin section of a silicon rubber composite material with mass fractions of 5%,10%,15% and 20% of the silicon dioxide spherical nano powder respectively. Wherein, fig. 3A, 3B, and 3C are 5% of the silica spherical nano powder by mass, fig. 3D, 3E, and 3F are 10% of the silica spherical nano powder by mass, fig. 3G, 3H, and 3I are 15% of the silica spherical nano powder by mass, and fig. 3J, 3K, and 3L are 20% of the silica spherical nano powder by mass.
According to the calculation method, in the range that the mass fraction of the silicon dioxide spherical nano powder is lower than 20%, the mass fraction of the silicon dioxide spherical nano powder is 5%,10%,15% and the average value of the fractal dimension values of the 20% silicon rubber composite material is 1.34, 1.45, 1.66 and 1.67 respectively, and the fractal dimension of the silicon dioxide spherical nano powder is increased along with the increase of the mass fraction of the silicon dioxide spherical nano powder, as shown in fig. 4. As can be seen from fig. 3, as the mass fraction of the silica spherical nano powder increases, the degree of agglomeration of the silica spherical nano powder in the silicone rubber increases. Therefore, in the silicon rubber composite material, the agglomeration degree of the silicon dioxide spherical nano powder is positively correlated with the fractal dimension, and the dispersion degree of the silicon dioxide spherical nano powder is negatively correlated with the fractal dimension.
From the above evidence, it is shown that the fractal dimension of spherical nano-powder is positively correlated with the degree of agglomeration and negatively correlated with the degree of dispersion. Therefore, the fractal dimension can be used as a quantitative index to characterize the dispersibility of the spherical nano powder, so that the problem that the dispersibility and the agglomeration degree of the spherical nano powder cannot be described by one number in the prior art is solved.
Claims (8)
1. The quantitative characterization method of the dispersibility of the spherical nano powder is characterized by comprising the following steps of:
s1, preparing a spherical nano powder sample;
s2, acquiring an electron microscope image of the spherical nano powder by using an electron microscope, and processing to obtain an electron microscope picture;
s3, calculating the fractal dimension of the electron microscope picture by adopting a box algorithm, wherein the specific operation comprises the following steps:
(1) Importing the electron microscope picture into software, and inputting the range of the box size ri;
(2) Counting the number Ni of the pixel points contained in each box size within the box size range by adopting an iteration method;
(3) Taking logNi as an abscissa and logNi as an ordinate, and fitting to obtain an empirical curve, wherein a fitting formula of the empirical curve is logni=dlogri, and a slope D of the empirical curve is a fractal dimension;
the box size ri is in the range of rmin r rmax, wherein rmin is the diameter of the single particle of the spherical nano powder, and rmax is the size of the largest aggregate in the electron microscope picture.
2. The quantitative characterization method of the dispersibility of spherical nano powder according to claim 1, wherein the spherical nano powder is silica spherical nano powder, titania spherical nano powder, iron oxide spherical nano powder or copper oxide spherical nano powder;
and/or the particle size of the spherical nano powder is 5-50 nm.
3. The method for quantitatively characterizing the dispersibility of spherical nano-powder according to claim 1, wherein in step S1, the spherical nano-powder sample is spherical nano-powder alone or a composite material containing spherical nano-powder.
4. A method for quantitatively characterizing the dispersibility of spherical nano-powder according to claim 3, wherein the composite material containing spherical nano-powder is a silicone rubber containing spherical nano-powder.
5. The method for quantitatively characterizing the dispersibility of spherical nano-powder according to claim 1, wherein in step S2, the electron microscope is a transmission electron microscope or a scanning electron microscope.
6. The quantitative characterization method of the dispersibility of the spherical nano powder according to claim 1, wherein when the electron microscope is a transmission electron microscope, the preparation method of the spherical nano powder sample is a dispersion method or an ultra-thin slice method.
7. The quantitative characterization method of the dispersibility of the spherical nano powder according to claim 1, wherein in the step S2, the magnification of the electron microscope image is 10000-100000 times;
and/or in the step S2, the scale of the electron microscope image is 50-500 nm.
8. The method for quantitatively characterizing the dispersibility of spherical nano-powder according to claim 1, characterized in that in step S2, the treatment is such that the electron microscope picture satisfies the following requirements: contrast 100%, brightness 5%, definition 5%, saturation 100%;
and/or, in step S2, the electron microscope image is in TIFF format.
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