CN113720868B - Method for measuring content of mesophase pitch of pitch material - Google Patents
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- CN113720868B CN113720868B CN202010453120.2A CN202010453120A CN113720868B CN 113720868 B CN113720868 B CN 113720868B CN 202010453120 A CN202010453120 A CN 202010453120A CN 113720868 B CN113720868 B CN 113720868B
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- 239000011302 mesophase pitch Substances 0.000 title claims abstract description 66
- 239000000463 material Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000011295 pitch Substances 0.000 title description 13
- 239000010426 asphalt Substances 0.000 claims abstract description 48
- 239000002184 metal Substances 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 238000005507 spraying Methods 0.000 claims abstract description 8
- 239000000523 sample Substances 0.000 claims description 65
- 238000005498 polishing Methods 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 2
- 238000000691 measurement method Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000011294 coal tar pitch Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000010894 electron beam technology Methods 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000003384 imaging method Methods 0.000 description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012811 non-conductive material Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011331 needle coke Substances 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention provides a method for acquiring microscopic images of asphalt materials, which is used for measuring the content of mesophase asphalt of the asphalt materials, and comprises the following steps: 1) Collecting microscopic images of a bituminous material sample by using a scanning electron microscope, wherein the bituminous material sample is not subjected to metal spraying treatment; 2) Obtaining the content of the mesophase pitch of the asphalt material according to the proportion of the mesophase pitch in one microscopic image, or obtaining the content of the mesophase pitch of the asphalt material according to the average value of the proportion of the mesophase pitch in a plurality of microscopic images, wherein in the step 1), the working voltage of the scanning electron microscope is 0.1 kV-1.0 kV. By not carrying out metal spraying treatment on the asphalt material sample and adopting 0.1kV to 1.0kV at the same time, a microscopic image of the asphalt material with the resolution reaching 1nm is obtained, so that the structure, the shape and the size of the mesophase asphalt and the distribution condition of the asphalt material can be obtained according to the microscopic image.
Description
Technical Field
The invention relates to a method for measuring the content of mesophase pitch of a bituminous material and application of the method in measuring the content of mesophase pitch.
Background
The mesophase pitch is an aggregate of aromatic hydrocarbon with optical anisotropy, and a liquid crystal substance composed of disc-shaped or rod-shaped polycyclic aromatic hydrocarbon generated in the heat treatment process of heavy aromatic hydrocarbon substances is a precursor of a high-quality carbon material, and can be widely used for high-performance carbon fibers, active carbon with ultrahigh specific surface area, high-quality needle coke, foam carbon and the like. Knowing the proportion of mesophase pitch in the pitch material, as well as the structure, shape, size and distribution of mesophase pitch, is a key factor in providing performance indicators for subsequent high carbon products.
In general, two methods are used to measure the mesophase pitch content of a pitch material, the first being a selective solvent extraction method that utilizes a specific solvent to dissolve out the non-mesophase pitch fraction, the remainder being mesophase pitch. The second is to use quantitative microscope technique, the method can obtain microscopic pictures of asphalt material, thus obtaining the distribution condition of intermediate phase asphalt in asphalt material, and then calculating the proportion of intermediate phase asphalt in asphalt material by software, thus achieving the quantitative effect.
The selective solvent extraction method is simple, but the method is easy to cause quantitative misalignment due to incomplete extraction or partial dissolution of the mesophase pitch, and in addition, after the mesophase pitch is dissolved, the true morphology and distribution of the mesophase pitch are destroyed, and tiny particles (microcrystalline structure) cannot be observed, so that important information of the structure of the mesophase pitch is lost.
The quantitative microscopic technology is to polish a sample to a mirror surface, obtain a polarized light photo through a polarized light microscope, obtain a photo with high contrast by means of the reflectivity difference of the mesophase pitch and other parts for polarized light, calculate the ratio of the mesophase pitch by distinguishing the mesophase pitch, and calculate the average value of the content through a large number of photos. This method is most commonly accepted in the industry as a truly effective method. However, the quantitative microscope technique is simple, but is limited by an optical instrument, and a sample needs a better polishing procedure, because scratches are easily generated on the surface of the unpolished complete sample, so that the quality of a picture image is affected, and even the image cannot be quantified, which is time-consuming and labor-consuming. In addition, the image obtained by the polarizing microscope is influenced by the grain growth direction of the mesophase pitch itself, so that bright and dark interference fringes appear, and the existence of the fringes can increase the difficulty in calibrating the mesophase pitch, thereby influencing the quantitative result. Further, when observing mesophase pitch by an optical microscope, the minimum observation size is about 10 μm due to the limitation of the optical limit, and therefore the microcrystalline structure (smaller than 5 μm) in mesophase pitch cannot be observed, which becomes a blind spot for structural observation.
In view of the foregoing, it is necessary to develop a new method for effectively observing the mesophase pitch, so as to obtain the ratio of the mesophase pitch to the pitch material, and obtain the structure, shape and size of the mesophase pitch and the distribution of the mesophase pitch to the pitch material.
Disclosure of Invention
In view of the above problems in the prior art, it is an object of the present invention to provide a method for measuring the content of mesophase pitch of a pitch material, in which a microscopic image of a pitch material with a resolution of up to 10 nm is obtained by using an operating voltage of 0.2kV to 0.5kV without performing a metal spraying treatment on a sample of the pitch material, so that the structure, shape and size of the mesophase pitch and the distribution of the pitch material can be known from the microscopic image.
The second object of the invention is an application related to one of the objects.
In order to achieve one of the above purposes, the technical scheme adopted by the invention is as follows:
method for measuring the content of mesophase pitch of a bituminous material a method for acquiring microscopic images of a bituminous material comprising:
1) Collecting microscopic images of a bituminous material sample by using a scanning electron microscope, wherein the bituminous material sample is not subjected to metal spraying treatment;
2) Deriving the mesophase pitch content of the asphalt material from the ratio of mesophase pitch in one microscopic image, or deriving the mesophase pitch content of the asphalt material from the average of the ratios of mesophase pitch in a plurality of microscopic images,
in the step 1), the working voltage of the scanning electron microscope is 0.1 kV-1.0 kV.
In the art, mesophase pitch is generally observed by a polarizing microscope, but the effect is poor. The inventors of the present application have found in the study that under certain specific conditions, such as a specific voltage, a scanning electron microscope can be used to observe mesophase pitch and to obtain microscopic images with a resolution of up to 10 nanometers.
In observing the morphology of non-conductive materials using scanning electron microscopy, it is common practice in the art to spray a metal layer onto the surface of the non-conductive material to render the material to be observed conductive. However, the inventor of the application found in experiments that the gold spraying treatment is not carried out on the asphalt material sample, and a clear microscopic image can be obtained by utilizing a scanning electron microscope under the working voltage of 0.1 kV-1.0 kV, especially 0.1 kV-0.5 kV, and the resolution of the obtained microscopic image can reach 10 nanometers, so that the observation size of the asphalt material is greatly improved. Based on the microscopic image obtained by the method, the structure, the shape and the size of the mesophase pitch and the distribution condition of the pitch material can be observed.
The scanning electron microscope uses electron excitation technology, uses electron beam to strike on the sample surface, at this time, the electron on the material surface will generate excitation phenomenon due to the irradiation of electron beam, and the image signal is collected by the sensor; different materials have different element contents and conductivity, so that the yield of excited electrons can be correspondingly increased; mesophase pitch is similar to normal pitch in terms of constituent elements, and because mesophase pitch is good in conductivity and crystallinity, and is different from surrounding normal pitch, the yield of excited electrons is different, and contrast is present on an image, thereby characterizing the distribution of mesophase pitch.
According to the invention, the asphalt material may be a coal asphalt material or a petroleum asphalt material.
According to the invention, the metal spraying treatment refers to spraying a metal coating on the surface of a sample, and is a conventional operation in the field.
In some preferred embodiments of the present invention, the scanning electron microscope has an operating voltage of 0.1kV to 0.5kV.
In some preferred embodiments of the present invention, the scanning electron microscope has an operating voltage of 0.1kV to 0.3kV.
According to the invention, the operating voltage of the scanning electron microscope refers to the operating voltage of the electron beam.
According to the present invention, in actual operation, the working voltage is selected depending on the type of the scanning electron microscope, for example, when the voltage of the scanning electron microscope can be changed only by 0.1KV, the working voltage that can be used in the present invention may be 0.1KV, 0.2KV, 0.3KV, 0.4KV, 0.5KV, 0.6KV, 0.7KV, 0.8KV, 0.9KV or 1.0KV. When the voltage of the scanning electron microscope can be changed at 0.01KV, the working voltage which can be adopted by the invention can be 0.1KV, 0.11KV, 0.12KV or 0.13KV and the like.
In some preferred embodiments of the present invention, the type of the scanning electron microscope is not particularly limited as long as it can achieve the voltage required by the present invention, and it is preferable that the working distance between the sample stage and the objective lens is sufficiently large, for example, at least more than 20mm, to accommodate and observe a large volume of mesophase pitch.
In some preferred embodiments of the invention, the scanning electron microscope is model FEI Nova Nano SEM, 450.
In some preferred embodiments of the invention, the thickness of the sample of asphalt material is 10 μm or more, preferably 20 μm or more.
According to the invention, sufficient secondary electrons are generated if and only if the thickness of the sample of bituminous material is within the above specified range, so that a clear microscopic image is obtained.
According to the invention, the thickness of the asphalt material sample should not exceed the elevation limit of the sample stage. Typically, the limit of elevation of the sample stage is about 20cm.
According to the invention, the thickness of the asphalt material sample is 20 μm to 2cm.
In some preferred embodiments of the invention, the sample of asphalt material is not subjected to a grinding and/or polishing treatment.
According to the method, when the method is adopted, the asphalt material sample does not need fine polishing or polishing, the natural fracture surface can be imaged, and the interference of lines or scratches on the surface of the sample is avoided, so that the nondestructive section characterization can be realized, the sample processing time is saved, the characterization step is simplified, and more accurate quantification is obtained.
In some preferred embodiments of the present invention, in step 1), when acquiring a microscopic image of the asphalt material sample, a linear distance between an electronic probe of the scanning electron microscope and a surface of the asphalt material sample adjacent to the electronic probe is controlled to be 5mm to 10mm, preferably 6mm to 8mm.
According to the invention, in step 1), when acquiring microscopic images of the asphalt material sample, the imaging mode of the scanning electron microscope is controlled to be secondary electron imaging, preferably, the large-range multiplying power is controlled to be 100-1000 times, and the small-range multiplying power is controlled to be 5000-20000 times.
According to the present invention, a large-range magnification means a magnification that is small, and thus a field of view is wide, and a large range can be seen. The small-range magnification means that the magnification is large, and thus the area of the visible region is small.
In some preferred embodiments of the invention, the contrast of the acquired microscopic image is adjusted before step 2) is performed, so that the area where the mesophase pitch is located is prominently strengthened.
In some preferred embodiments of the present invention, the contrast of the microscopic image is adjusted to 90% or more, preferably 90% to 95%. According to the present invention, impurities, such as dust, on the surface of asphalt material can be removed using high-pressure air.
In order to achieve the second purpose, the technical scheme adopted by the invention is as follows:
use of a method according to the above in the field of measurement of the content of mesophase pitch.
The invention has the advantages that:
firstly, the minimum observable size of the method provided by the invention is 10 nanometers, so that the observed size of the mesophase pitch (the limit of an optical microscope is 10 micrometers) is greatly improved, and the method breaks through the microcrystalline observation and research of the mesophase pitch.
Secondly, the method provided by the invention can be used for collecting images of samples which are not polished, and avoids the influence of scratches caused by polishing operation.
Drawings
Fig. 1 is a microscopic image obtained by the measurement method of example 1.
Fig. 2 is a microscopic image obtained by the measurement method of example 2.
Fig. 3 is a microscopic image obtained by the measurement method of example 3.
Fig. 4 is a microscopic image obtained by the measurement method of example 4.
Fig. 5 is a microscopic image (contrast 70%, brightness 40%) obtained by the measurement method of example 5.
Fig. 6 is a microscopic image (contrast 90%, brightness 5%) obtained by the measurement method of example 5.
Fig. 7 is a microscopic image obtained by the measurement method of example 6.
Fig. 8 is a partially enlarged view of a microscopic image obtained by the measurement method of example 6.
Fig. 9 is a microscopic image obtained by the measurement method of comparative example 1.
Fig. 10 is a microscopic image obtained by the measurement method of comparative example 2.
Fig. 11 is a microscopic image obtained by the measurement method of comparative example 3.
Fig. 12 is a microscopic image of the microscopic image obtained by the measuring method of comparative example 3 after the image software adjustment.
Detailed Description
The present invention will be described in detail with reference to examples, but the scope of the present invention is not limited to the following description.
Example 1
Step 1: directly breaking the massive coal tar pitch, and taking a piece of petroleum pitch with a relatively flat fracture surface as a sample to be tested;
step 2: blowing off dust on the surface of the sample by using high-pressure air, then placing the sample on a special sample table, and simply fixing the sample so that the sample cannot move;
step 3: placing the sample into an observation chamber, and vacuumizing to 5E-3Pa;
step 4: setting the working voltage to be 0.2kV, and adjusting the multiplying power to be 100 times by using a secondary electron imaging mode;
step 5: the electron probe of the scanning electron microscope was moved to a position about 5-10mm from the surface of the sample, and a suitable area was selected and photographed with a suitable magnification adjusted to obtain a microscopic image of the sample, as shown in fig. 1. In fig. 1, the sample surface texture can be clearly seen. Non-mesophase pitch (dark grey) and mesophase pitch (white) are clearly visible with clear boundaries.
Step 6: and (3) moving the sample stage, and collecting images in other areas of the sample, wherein more than 5 images are collected in total.
Step 7: and calculating the average content of mesophase pitch in each image by statistics.
Example 2
In this example, coal tar pitch of another area obtained in step 1 of example 1 was used as a sample to be tested, and an image was collected in the manner of example 1, except that the operating voltage was 0.4kV, and the obtained microscopic image was as shown in fig. 2.
As can be seen from comparing fig. 1 and fig. 2, the contrast ratio of fig. 2 is slightly lower than that of fig. 1.
Example 3
In this example, coal tar pitch of another area obtained in step 1 of example 1 was used as a sample to be tested, and an image was collected in the manner of example 1, except that the operating voltage was 1.0kV, and the obtained microscopic image was as shown in fig. 3.
Comparing fig. 1 and 3, the signal in fig. 3 is inverted, that is, the original mesophase asphalt turns black gray, and the non-mesophase asphalt turns white, which indicates that the voltage is too high, which causes deep effect of electron beam and sample, and affects the appearance, which is unfavorable for obtaining clear microscopic image.
Example 4
In this example, another piece of coal tar pitch having a relatively flat fracture surface obtained in step 1 of example 1 was used as a sample to be tested, and an image (not polished) was collected in the same manner as in example 1, and the obtained microscopic image was shown in fig. 4.
In fig. 4, the natural cracking trace of the asphalt surface is seen in a hidden way, but the mesophase asphalt is still clearly distinguishable (white part) due to the large contrast in black and white, indicating that the observation of the mesophase asphalt by an electron microscope is not affected by the surface flatness.
Example 5
In this example, another piece of coal tar pitch with a relatively flat fracture surface obtained in step 1 of example 1 was used as a sample to be tested, and after the sample was simply polished, an image was collected in the manner of example 1, the contrast was 70%, and the brightness was adjusted to 40%, and the obtained microscopic image was shown in fig. 5. To show the effect of contrast and brightness on distinguishing mesophase pitch from non-mesophase pitch, the contrast of fig. 5 was adjusted to 90% and the brightness was adjusted to 5% so that the region where mesophase pitch was located was prominently strengthened as shown in fig. 6.
Example 6
In this example, another petroleum asphalt with a relatively flat fracture surface obtained in step 1 of example 1 was used as a sample to be tested, and an image was acquired in the manner of example 1, and the obtained microscopic image is shown in fig. 7. In fig. 7, an area (block) is selected for enlargement, as shown in fig. 8.
In fig. 8, the secondary particles of mesophase pitch are clearly visible, the minimum size of which is about 50 nm, in this mode, a resolution of up to 10 nm, which is not possible by other observation means, such as optical microscopy.
Comparative example 1
In this comparative example, another petroleum asphalt having a relatively flat fracture surface obtained in step 1 of example 1 was used as a sample to be tested, and an image was collected in the same manner as in example 1 except that the operating voltage was 10kV, which is a voltage commonly used in the art for observing the sample by a scanning electron microscope, and the obtained microscopic image was shown in fig. 9.
As can be seen by comparing fig. 1 and 9, fig. 9 does not clearly distinguish between asphalt and mesophase asphalt. The surface is not observable with mesophase pitch at the voltages typically employed. This is also one of the reasons for the technical prejudice in the art that the mesophase pitch cannot be observed with a scanning electron microscope.
Comparative example 2
In this comparative example, a non-polished asphalt sample was directly observed with a polarizing microscope.
Another piece of petroleum asphalt with a relatively flat fracture surface obtained in step 1 of example 1 was used as a sample to be tested, and the sample was fixed on a glass slide and placed on a polarizing microscope sample stage. And (3) adjusting the light path to be in a reflection mode, adjusting the polaroid to be in an orthogonal polarization mode, and selecting the objective lens of 20 times. Focusing, the clearest picture is obtained, as shown in fig. 10.
In fig. 10, since the sample surface was not polished, no clear mesophase and non-mesophase regions could be observed by the polarization method.
Comparative example 3
In this comparative example, the polished asphalt sample was observed with a polarizing microscope.
Another piece of petroleum asphalt with a relatively flat fracture surface obtained in the step 1 of the example 1 is taken as a sample to be tested, and after the sample is simply polished, the sample is fixed on a glass slide and placed on a sample stage of a polarizing microscope. And (3) adjusting the light path to be in a reflection mode, adjusting the polaroid to be in an orthogonal polarization mode, and selecting the objective lens of 20 times. Focusing, the clearest picture is obtained, as shown in fig. 11.
The duty cycle of the mesophase portions in the image is calculated using calculation software. Due to refractive index and mesophase pitch crystal texture, mesophase portions in a polarization microscope picture have bright-dark interference shadows (or fringes), such as the portions within the circles in fig. 11, which shadows also cause quantitative errors. With fine tuning of the image calculation software, the result will be either higher or lower. Fig. 11 does not calculate the intermediate phase shadow into, and calculates the intermediate phase content to be 35.3%, which is low.
To calculate the intermediate phase shadow part, the calculation range is adjusted by image software, and the result is that the shadow part of the non-intermediate phase is also adjusted to be the intermediate phase part, and the result is higher, as shown in fig. 12. The calculated mesophase content in fig. 12 was 57.9%.
It should be noted that the above-described embodiments are only for explaining the present invention and do not constitute any limitation of the present invention. The invention has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the invention as defined in the appended claims, and the invention may be modified without departing from the scope and spirit of the invention. Although the invention is described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, as the invention extends to all other means and applications which perform the same function.
Claims (7)
1. Use of a method of measuring the content of mesophase pitch of a bituminous material in the field of measurement of the content of mesophase pitch, the method comprising:
1) Collecting microscopic images of a bituminous material sample by using a scanning electron microscope, wherein the bituminous material sample is not subjected to metal spraying treatment;
2) Deriving the mesophase pitch content of the asphalt material from the ratio of mesophase pitch in one microscopic image, or deriving the mesophase pitch content of the asphalt material from the average of the ratios of mesophase pitch in a plurality of microscopic images,
in the step 1), the working voltage of the scanning electron microscope is 0.1 kV-0.3 kV;
the thickness of the asphalt material sample is 20 μm to 2cm;
in the step 1), when a microscopic image of the asphalt material sample is acquired, controlling the linear distance between an electronic probe of the scanning electron microscope and the surface of the asphalt material sample, which is close to the electronic probe, to be 5 mm-10 mm;
the scanning electron microscope is model FEI Nova Nano SEM 450,450.
2. Use according to claim 1, wherein the sample of bituminous material has not been subjected to a grinding and/or polishing treatment.
3. The use according to claim 1, characterized in that the contrast of the acquired microscopic image is adjusted before step 2) is performed, so that the area where the mesophase pitch is located is prominently strengthened.
4. The use according to claim 3, wherein the contrast of the microscopic image is adjusted to be above 90%.
5. The use according to claim 4, wherein the contrast of the microscopic image is adjusted to 90% -95%.
6. The use according to claim 1, wherein in step 2) the ratio refers to the percentage of the area of mesophase pitch in the total area of the microscopic image.
7. The use according to claim 1, wherein in step 2) the duty cycle refers to the percentage of the total pixel value of mesophase pitch in the microscopic image.
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| JPH0714537A (en) * | 1993-06-22 | 1995-01-17 | Hitachi Ltd | Measuring method by scanning electron microscope |
| JP2005121467A (en) * | 2003-10-16 | 2005-05-12 | Jfe Steel Kk | Method for evaluating adhesion property of thin film, and method for manufacturing base having thin film on surface |
| JP2007139633A (en) * | 2005-11-21 | 2007-06-07 | Toppan Printing Co Ltd | Method of preparing sample for scanning electron microscope |
| JP2010025833A (en) * | 2008-07-23 | 2010-02-04 | Jfe Steel Corp | Method of measuring coverage of iron-based powder |
| JP2011158830A (en) * | 2010-02-03 | 2011-08-18 | Canon Inc | Magnetic carrier and two-component developer |
| CN105301026A (en) * | 2015-10-20 | 2016-02-03 | 中国石油天然气股份有限公司 | Method and device for determining asphalt cause in reservoir |
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