CN111006921B - Sample preparation method for determining dielectric constant of carbon black material - Google Patents
Sample preparation method for determining dielectric constant of carbon black material Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation, and discloses a sample preparation method for determining the dielectric constant of a carbon black material, which comprises the steps of drying carbon black material powder to be detected for 4 hours at the temperature of 40 +/-2 ℃ for later use; weighing 100.0g +/-0.5 g of the slice paraffin by using an electronic balance with the sensing quantity of 0.1g, adding into a 250ml beaker, rapidly heating and melting by using an electric heating furnace, and weighing a certain proportion of dried carbon black sample by using the electronic balance with the sensing quantity of 0.1 g; dispersing the weighed carbon black sample; placing the dispersed sample into a forming grinding tool for casting and forming; and separating the molded sample from the mold, and finishing and molding. The paraffin wax and the carbon black material in a molten state are mixed, cast and molded, the stability problem of a sample for testing the dielectric constant of the carbon black material at present can be solved, the dispersion uniformity and the compactness of the carbon black material are ensured, the stability of the sample for testing the dielectric constant of the carbon black material is greatly improved, and the stability of a test result is improved.
Description
Technical Field
The invention belongs to the technical field of preparation, and particularly relates to a sample preparation method for determining a dielectric constant of a carbon black material.
Background
Currently, the current state of the art commonly used in the industry is such that:
carbon black is a carbon material with very special microstructure, particle morphology and surface performance, and is a fine granular black powdery substance generated by cracking and incomplete combustion of hydrocarbon substances (hydrocarbons such as oil or natural gas). The carbon black material is a low-loss dielectric material and has the characteristics of fluffy structure, low density, easy stress deformation and the like. The electromagnetic parameters of the carbon black material are generally characterized by dielectric constant and magnetic permeability, wherein the carbon black material has good dielectric loss performance (dielectric constant), but the magnetic performance (magnetic permeability) is very small, the real part of the magnetic permeability is about 1, and the imaginary part of the magnetic permeability is about 0.
The general electromagnetic parameter test method is shown in table 1:
TABLE 1 comparison of the applicability of the commonly used electromagnetic parameter test methods
Referring to the table above, the accuracy of testing the low-loss dielectric material by using the slotline reflection method and the coaxial reflection method is low, and the method is not suitable for testing the electromagnetic parameters of the carbon black material.
The free space method has narrow testing frequency band, the required size of the sample is too large, the carbon black material is inconvenient to prepare a testing sample, the dispersion uniformity is difficult to control, and the method is not suitable for testing the electromagnetic parameters of the carbon black material.
The resonant cavity method is special for testing hardware equipment, the testing frequency band is a single frequency point, only the dielectric constant of a fixed frequency point can be carried out, the broadband test cannot be carried out, and the method is not suitable for testing the electromagnetic parameters of the carbon black material.
A common dielectric constant test method uses coaxial air lines in a coaxial transmission/reflection method. Before testing, paraffin and carbon black are uniformly mixed in a melting state, and are pressed into coaxial samples with the thickness of 2mm, the inner diameter of phi 3mm and the outer diameter of phi 7mm in a special copper mold. The mass ratio of the carbon black material to the paraffin is generally 25:100, and the test frequency range is generally 2-18 GHz. The dielectric constant was determined by a coaxial line-based transmission/reflection method (see standard SJ 20512-1995).
The coaxial air line in the coaxial transmission/reflection method is adopted to test the dielectric constant, is very mature in principle, and is also the method adopted by the existing electromagnetic parameter test.
In summary, the problems of the prior art are as follows: the main method for testing the electromagnetic parameters of the existing carbon black material is that the stability of the test result of the dielectric constant of the carbon black material is poor, and the reason is that the repeatability of the preparation of a test sample of the carbon black material is poor, which is caused by the physical properties of the carbon black material. The carbon black material has a fluffy structure, small density and easy deformation, so that the dispersion uniformity of the carbon black in a test sample is poor, and the stress in the sample preparation process can cause the non-uniform compactness of the sample. Meanwhile, the mass of the test sample is not more than 0.1g, and the requirement on sample preparation repetition is high, so that the difference between samples in the same batch is large.
The existing carbon black material test sample preparation method is poor in repeatability, and the prepared carbon black material is fluffy in structure, small in density, easy to deform and poor in carbon black dispersion uniformity.
The difficulty of solving the technical problems is as follows: the difficulty of the dielectric constant stability test of the carbon black material is that a test sample with uniform dispersion can be prepared in a repeatable manner. The carbon black material has the characteristics of fluffy structure, small density, easy stress deformation and the like, so that the preparation of a uniformly dispersed test sample is a key technology for testing the dielectric constant of the carbon black material.
The significance of solving the technical problems is as follows:
aiming at the preparation of electromagnetic parameter test samples of carbon black type fluffy materials, the preparation of uniformly dispersed test samples is a precondition for the stable dielectric constant test of the carbon black materials.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a sample preparation method for determining the dielectric constant of a carbon black material.
The invention is realized in such a way that the sample preparation method for measuring the dielectric constant of the carbon black material obtains the appropriate sample preparation conditions by researching the sample proportion, the molding temperature and other influencing factors in the preparation process of the electromagnetic parameter test sample of the carbon black material. The preparation method of the sample for measuring the dielectric constant of the carbon black material specifically comprises the following steps:
drying carbon black material powder to be detected for 4 hours at the temperature of 40 +/-2 ℃ for later use;
weighing 100.0g +/-0.5 g of the slice paraffin by using an electronic balance with the sensing quantity of 0.1g, adding the slice paraffin into a 250ml beaker, rapidly heating and melting the slice paraffin by using an electric heating furnace, and weighing a certain proportion of dried carbon black sample by using the electronic balance with the sensing quantity of 0.1 g;
dispersing the weighed carbon black sample;
placing the dispersed sample into a forming grinding tool for casting and forming;
and step five, separating the molded sample from the mold, and finishing and molding.
Further, in the third step, the dispersing of the carbon black sample specifically includes:
firstly, placing a beaker on a heating platform of a magnetic stirrer, placing a temperature sensor and a magneton, setting the temperature to be 70 ℃, stirring at 80-100 RPM, adding weighed carbon black materials into molten paraffin in batches under the conditions of heating and stirring after the temperature is stable, and adding the carbon black materials for 3 times;
then, the magnetic stirrer was kept at 70 ℃ in a beaker and stirred for 15min to completely remove the residual gas.
Further, in the fourth step, the pouring and molding of the carbon black sample specifically includes:
(1) covering the cavity of the waveguide mold with a smooth metal sheet at the bottom of the standard waveguide mold in the same frequency band, namely the surface A, sealing the smooth metal sheet with an aluminum adhesive tape, and adhering an aluminum adhesive tape for protecting the waveguide mold to the other surface, namely the surface B except the cavity part;
(2) coating proper amount of silicone oil on the inner wall of a rectangular square frame with the thickness of 5mm, and respectively adhering the silicone oil to the surfaces B of 3 waveguide molds, wherein the size of the inner frame of the rectangular square frame is slightly larger than that of a cavity of the waveguide mold;
(3) setting the temperature to 70 ℃, placing a standard waveguide mold, and enabling the A surface to be downward;
(4) after the temperature is stable, directly and quickly pouring the uniformly dispersed carbon black and paraffin mixture into a standard waveguide mold, wherein the pouring volume just exceeds the rectangular frame;
(5) and taking the standard waveguide mold off the constant temperature table, and naturally curing and molding at the room temperature of 20-25 ℃ for 30 min.
Further, in the fifth step, the sample separation and molding specifically comprises:
1) slightly pushing the sample after the sample is formed, and taking down the rectangular square frame;
2) after the rectangular square frame is taken down, cutting off an upper layer sample by using a paper cutter, and cutting off redundant samples by using a plastic scraper until the sample and the surface B of the waveguide mold are smooth;
3) and stripping the smooth metal sheet and the aluminum adhesive tape of the waveguide mold, wiping off carbon black sample scraps stuck on the waveguide mold by using gauze or absorbent cotton, and placing the carbon black sample scraps in a clean tray to be detected.
The invention provides a sample for measuring the dielectric constant of a carbon black material, which is prepared by the sample preparation method for measuring the dielectric constant of the carbon black material.
In summary, the advantages and positive effects of the invention are:
the carbon black material has a fluffy structure, small density and easy deformation, so that the dispersion uniformity of the carbon black in a test sample is poor, and the stress in the sample preparation process can cause the non-uniform compactness of the sample. Meanwhile, the mass of a test sample is not more than 0.1g, and the repeated requirement on sample preparation is high, so that the difference among samples in the same batch is large, and the real part fluctuation of the electromagnetic parameter is large and even exceeds 50%. By adopting the sample preparation method, the fluctuation of each frequency band of the real part of the electromagnetic parameter is less than 10%.
According to the physical characteristics of the carbon black material, the dielectric constant of the carbon black material sample is determined by adopting a standard rectangular waveguide transmission line method in a coaxial transmission/reflection method, and a stable test sample is prepared by utilizing a method of mixing, casting and molding the carbon black material and paraffin.
According to the invention, the dielectric constant of a carbon black material sample is determined by adopting a standard rectangular waveguide transmission line method according to the physical characteristics of the carbon black material, paraffin is used as a dispersion carrier of the carbon black material, the mass ratio of the carbon black material to the paraffin is reduced, the carbon black material and the paraffin are dispersed uniformly and fully, and the influence of the dielectric constant test stability of the factors such as the mass ratio of the carbon black to the paraffin, the pouring temperature and the forming time is analyzed after casting forming and trimming. It is determined that: the mass ratio of the carbon black to the paraffin is 5:100 (acetylene black), the pouring temperature is 70 ℃, the forming time is more than 30min, the testing stability of the real part of the dielectric constant is evaluated according to the relative standard deviation of a testing sample, 20 samples are repeatedly prepared and tested, each frequency band of each sample is tested with 201 data points, and the relative standard deviation is calculated for each data point.
The test method is simple to operate and high in test stability, and the sample preparation and test method can be popularized and used for testing the dielectric constant of other types of carbon black materials or fluffy powder materials with low density.
The paraffin wax and the carbon black material in a molten state are mixed, poured and molded, so that the stability problem of a dielectric constant sample of the carbon black material in the current test can be solved, the dispersion uniformity and the compactness of the carbon black material are ensured, the stability of the dielectric constant test sample of the carbon black material is greatly improved, and the stability of a test result is improved;
the casting molding method can effectively eliminate the defects of gas cavities and corners of the sample.
Drawings
FIG. 1 is a flow chart of a sample preparation method for determining the dielectric constant of a carbon black material according to an embodiment of the present invention.
Fig. 2 is a schematic view of a forming mold according to an embodiment of the present invention.
FIG. 3 is a graph showing the dielectric constant real part test result of the acetylene-carbon black X frequency band (8.2 GHz-12.4 GHz).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
The technical scheme of the invention is explained in detail in the following with reference to the attached drawings.
As shown in fig. 1, a sample preparation method for determining a dielectric constant of a carbon black material provided in an embodiment of the present invention specifically includes:
s101, drying the carbon black material powder to be detected for 4 hours at the temperature of 40 +/-2 ℃ for later use.
S102, weighing 100.0g +/-0.5 g of the section paraffin by using an electronic balance with a sensing quantity of 0.1g, adding the section paraffin into a 250ml beaker, rapidly heating and melting the section paraffin by using an electric heating furnace, and weighing a certain proportion of dried carbon black sample by using the electronic balance with a sensing quantity of 0.1 g.
And S103, dispersing the weighed carbon black sample.
And S104, placing the dispersed sample into a forming grinding tool for casting and forming.
And S105, separating the molded sample from the mold, and trimming and molding.
In step S103, the dispersion of the carbon black sample provided in the embodiment of the present invention specifically includes:
firstly, placing a beaker on a heating platform of a magnetic stirrer, placing a temperature sensor and a magneton, setting the temperature at 70 ℃, stirring at 80-100 RPM, adding weighed carbon black materials into molten paraffin in batches under the conditions of heating and stirring after the temperature is stable, and adding the carbon black materials for 3 times.
Then, the magnetic stirrer was kept at 70 ℃ in a beaker and stirred for 15min to completely remove the residual gas.
In step S104, the pouring and forming of the carbon black sample provided in the embodiment of the present invention specifically includes:
(1) and covering the cavity of the waveguide mold with a smooth metal sheet at the bottom of the standard waveguide mold in the same frequency band, namely the surface A, sealing the smooth metal sheet with an aluminum adhesive tape, and adhering an aluminum adhesive tape for protecting the waveguide mold to the other surface, namely the surface B except the cavity part.
(2) And (3) smearing a proper amount of silicone oil on the inner wall of a rectangular square frame with the thickness of 5mm, respectively sticking the silicone oil on the surfaces B of 3 waveguide molds, wherein the size of the inner frame of the rectangular square frame is slightly larger than the cavity of the waveguide mold.
(3) The temperature was set at 70 ℃ and the standard waveguide mold was placed with the a side down.
(4) And after the temperature is stable, directly and quickly pouring the uniformly dispersed carbon black and paraffin mixture into a standard waveguide mold, wherein the pouring volume just exceeds the rectangular frame.
(5) And (3) taking the standard waveguide mold from the constant temperature table, and naturally curing and molding for 30min at the room temperature of 20-25 ℃.
In step S105, the sample separation and molding provided in the embodiment of the present invention specifically includes:
1) slightly pushing the sample after the sample is formed, and taking down the rectangular square frame; .
2) And after the rectangular square frame is taken down, cutting off an upper layer sample by using a paper cutter, and cutting off redundant samples by using a plastic scraper until the sample and the surface B of the waveguide mold are flat.
3) And stripping the smooth metal sheet and the aluminum adhesive tape of the waveguide mold, wiping off carbon black sample scraps stuck on the waveguide mold by using gauze or absorbent cotton, and placing the carbon black sample scraps in a clean tray to be detected.
The technical solution and technical effects of the present invention are further described below with reference to specific embodiments.
Example 1:
the preparation process of the carbon black material dielectric constant test sample mainly comprises the steps of dispersing, forming and trimming the sample, and the specific operation steps are as follows:
1 Dispersion Process
1.1 drying the carbon black material powder to be tested for 4 hours at the temperature of 40 +/-2 ℃ for later use.
1.2 weighing 100.0g +/-0.5 g of the section paraffin by using an electronic balance with a sensing quantity of 0.1g, adding the section paraffin into a 250ml beaker, rapidly heating and melting the section paraffin by using an electric heating furnace, and weighing a certain proportion of dried carbon black samples (such as 5.0g +/-0.1 g of acetylene black) by using an electronic balance with a sensing quantity of 0.1 g.
1.3 placing the beaker on a heating platform of a magnetic stirrer, placing a temperature sensor and a magneton, setting the temperature at 70 ℃, stirring at a speed of 80-100 RPM, adding weighed carbon black materials into molten paraffin in batches under the conditions of heating and stirring after the temperature is stable, and adding the materials for 3 times.
1.4 because air remains in the gaps of the carbon black material, the temperature of the beaker on the magnetic stirrer should be kept at 70 ℃, and the stirring is continued for 15min, so that the residual air is completely removed.
2 Process of Forming
2.1 at the bottom (surface A) of the standard waveguide mold in the same frequency band, as shown in fig. 2, a smooth metal sheet is used for covering the cavity of the waveguide mold, an aluminum adhesive tape is used for sealing the smooth metal sheet, and the aluminum adhesive tape is also pasted on the other surface (surface B) except the cavity part, so that the waveguide mold is protected.
2.2 smearing a small amount of silicone oil on the inner wall of the rectangular square frame with the thickness of 5mm, respectively sticking the silicone oil on the surfaces B of the 3 waveguide molds, wherein the size of the inner frame of the rectangular square frame is slightly larger than the cavity of the waveguide mold.
2.3 opening the thermostatic table, setting the temperature at 70 ℃, placing the standard waveguide mold with the A side facing downwards.
2.4 after the temperature is stable, directly and quickly pouring the uniformly dispersed carbon black and paraffin mixture into a standard waveguide mold, wherein the pouring volume just exceeds the rectangular square frame.
And 2.5, taking down the standard waveguide mold from the constant temperature table, and naturally curing and molding at the room temperature of 20-25 ℃ for 30 min.
3 dressing samples
3.1 after the sample is formed, slightly pushing the sample, and taking down the rectangular square frame.
3.2 after taking down the rectangular square frame, cutting off the upper layer sample by using a paper cutter, and cutting off redundant samples by using a plastic scraper until the sample and the surface B of the waveguide mold are flat.
3.3 stripping the smooth metal sheet and the aluminum adhesive tape of the waveguide mold, wiping off carbon black sample scraps adhered on the waveguide mold by gauze or absorbent cotton, and placing the carbon black sample scraps in a clean tray to be tested.
According to the physical characteristics of the carbon black material, the dielectric constant of a carbon black material sample is measured by adopting a standard rectangular waveguide transmission line method, paraffin is used as a dispersion carrier of the carbon black material, the mass ratio of the carbon black material to the paraffin is reduced, the carbon black material and the paraffin are dispersed uniformly, and the influence of the dielectric constant test stability of factors such as the mass ratio of the carbon black to the paraffin, the pouring temperature and the forming time is researched after casting forming and trimming. It is determined that: the mass ratio of the carbon black to the paraffin is 5:100 (acetylene black), the pouring temperature is 70 ℃, the forming time is more than 30min, the testing stability of the real part of the dielectric constant is evaluated according to the relative standard deviation of a testing sample, 20 samples are repeatedly prepared and tested, each frequency band of each sample is totally tested with 201 data points, and the relative standard deviation is respectively calculated for each data point. The curve of the dielectric constant real part test result of the acetylene-carbon black X frequency band (8.2 GHz-12.4 GHz) is shown in the following figure 3, and the volatility (relative standard deviation) of each data point of the dielectric constant real part is not more than 4.25%. The test method is simple to operate and high in test stability, and the sample preparation and test method can be popularized and used for testing the dielectric constant of other types of carbon black materials or fluffy powder materials with low density.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (3)
1. The sample preparation method for measuring the dielectric constant of the carbon black material is characterized by specifically comprising the following steps of:
drying carbon black material powder to be detected for 4 hours at the temperature of 40 +/-2 ℃ for later use;
weighing 100.0g +/-0.5 g of the slice paraffin by using an electronic balance with the sensing quantity of 0.1g, adding the slice paraffin into a 250ml beaker, rapidly heating and melting the slice paraffin by using an electric heating furnace, and weighing a certain proportion of dried carbon black sample by using the electronic balance with the sensing quantity of 0.1 g;
dispersing the weighed carbon black sample;
placing the dispersed sample into a forming grinding tool for casting and forming;
step five, separating the molded sample from the mold, and finishing and molding;
in step three, the dispersion of the carbon black sample specifically comprises:
firstly, placing a beaker on a heating platform of a magnetic stirrer, placing a temperature sensor and a magneton, setting the temperature to be 70 ℃, stirring at 80-100 RPM, adding weighed carbon black materials into molten paraffin in batches under the conditions of heating and stirring after the temperature is stable, and adding the carbon black materials for 3 times;
then, keeping the temperature of a beaker on a magnetic stirrer at 70 ℃, and continuously stirring for 15min to completely remove residual gas;
in the fourth step, the casting molding of the carbon black sample specifically comprises:
(1) covering the cavity of the waveguide mold with a smooth metal sheet at the bottom of the standard waveguide mold in the same frequency band, namely the surface A, sealing the smooth metal sheet with an aluminum adhesive tape, and adhering an aluminum adhesive tape for protecting the waveguide mold to the other surface, namely the surface B except the cavity part;
(2) coating proper amount of silicone oil on the inner wall of a rectangular square frame with the thickness of 5mm, and respectively adhering the silicone oil to the surfaces B of 3 waveguide molds, wherein the size of the inner frame of the rectangular square frame is slightly larger than that of a cavity of the waveguide mold;
(3) setting the temperature to 70 ℃, placing a standard waveguide mold with the A surface facing downwards;
(4) after the temperature is stable, directly and quickly pouring the uniformly dispersed carbon black and paraffin mixture into a standard waveguide mold, wherein the pouring volume just exceeds the rectangular frame;
(5) and (3) taking the standard waveguide mold from the constant temperature table, and naturally curing and molding for 30min at the room temperature of 20-25 ℃.
2. The method for preparing a sample for determining the dielectric constant of the carbon black material according to claim 1, wherein in the fifth step, the separating and molding of the sample specifically comprises:
1) slightly pushing the sample after the sample is formed, and taking down the rectangular square frame;
2) after the rectangular square frame is taken down, cutting off an upper layer sample by using a paper cutter, and cutting off redundant samples by using a plastic scraper until the sample and the surface B of the waveguide mold are smooth;
3) and stripping the smooth metal sheet and the aluminum adhesive tape of the waveguide mold, wiping off carbon black sample scraps adhered on the waveguide mold by using gauze or absorbent cotton, and placing the carbon black sample scraps in a clean tray to be tested.
3. A sample for measuring the dielectric constant of a carbon black material prepared by the sample preparation method for measuring the dielectric constant of a carbon black material according to claim 1.
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