CN113418949A - Preparation method and test method of standard-size sample for X-ray test of composite material - Google Patents
Preparation method and test method of standard-size sample for X-ray test of composite material Download PDFInfo
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- CN113418949A CN113418949A CN202011491655.5A CN202011491655A CN113418949A CN 113418949 A CN113418949 A CN 113418949A CN 202011491655 A CN202011491655 A CN 202011491655A CN 113418949 A CN113418949 A CN 113418949A
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- 238000012360 testing method Methods 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000010998 test method Methods 0.000 title abstract description 15
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000011521 glass Substances 0.000 claims abstract description 93
- 239000011324 bead Substances 0.000 claims abstract description 85
- 239000003822 epoxy resin Substances 0.000 claims abstract description 26
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 26
- 238000005507 spraying Methods 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 239000002390 adhesive tape Substances 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 238000004544 sputter deposition Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 25
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 15
- 239000010931 gold Substances 0.000 claims description 15
- 229910052737 gold Inorganic materials 0.000 claims description 15
- 238000001878 scanning electron micrograph Methods 0.000 claims description 10
- 238000010894 electron beam technology Methods 0.000 claims description 7
- 230000035515 penetration Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 3
- 238000002834 transmittance Methods 0.000 claims description 3
- 239000011325 microbead Substances 0.000 claims description 2
- 238000005259 measurement Methods 0.000 description 10
- 238000010586 diagram Methods 0.000 description 6
- 239000004005 microsphere Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000004075 alteration Effects 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
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- 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
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- 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 relates to a preparation method of a standard-size sample for X-ray testing of a composite material, which comprises the following steps: selecting glass beads with a set diameter, inlaying the glass beads in a sample groove filled with epoxy resin, and curing the glass beads into a sample with a standard size; glass beads with a set diameter are adhered to a conductive carbon adhesive tape, and the conductive carbon adhesive tape is placed in an ion sputtering instrument for spraying metal for a set time to form an SEM sample and is adhered to a small sample table. The invention also relates to a testing method of the standard-size sample for the X-ray testing of the composite material. The preparation method and the test method of the standard-size sample for the X-ray test of the composite material aim to solve the problem that the size of a microstructure cannot be accurately measured by comparison of the standard-size sample for the X-ray test in the prior art.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a preparation method and a test method of a standard size sample for X-ray test of a composite material.
Background
The X-ray has the characteristics of short wavelength and penetration depth, the high-contrast X-ray three-dimensional microscope utilizes perspective two-dimensional projection imaging of different angles of a sample, combines a computer three-dimensional digital imaging reconstruction technology, constructs a three-dimensional high-resolution perspective structure of an object to be detected, clearly, accurately and visually displays information such as internal structural features of the object to be detected in the form of an image, and measures the internal microscopic size of the sample.
The resolution of a standard size sample of the existing X-ray test is in millimeter level, the microstructure size cannot be accurately measured in a contrast manner, and the micron-level standard sample is lacked.
Therefore, the inventor provides a preparation method and a test method of a standard-size sample for X-ray testing of a composite material.
Disclosure of Invention
(1) Technical problem to be solved
The embodiment of the invention provides a preparation method and a test method of a standard size sample for X-ray testing of a composite material.
(2) Technical scheme
A first aspect of an embodiment of the present invention provides a method of preparing a standard size sample for composite X-ray testing, the method comprising the steps of:
selecting glass beads with a set diameter, inlaying the glass beads in a sample groove filled with epoxy resin, and curing the glass beads into a sample with a standard size;
the glass beads with the set diameter are adhered to a conductive carbon adhesive tape, and the conductive carbon adhesive tape is placed in an ion sputtering instrument for spraying metal for set time to form an SEM sample and adhered to a small sample table.
Further, the particle size of the glass micro-beads with the set diameter is 10-500 μm.
Further, the set time is 1-2 min.
A second aspect of an embodiment of the present invention provides a method of testing a standard size sample for composite X-ray testing, the method comprising the steps of:
measuring the size of the glass beads embedded in the epoxy resin sample by using an X-ray three-dimensional microscope;
measuring the size of the glass beads subjected to gold spraying treatment by using a field emission environment electron microscope;
and determining that the epoxy resin sample is a standard size sample by comparing the sizes of the glass beads and the glass beads after the gold spraying treatment.
Further, the method for measuring the size of the glass bead embedded in the epoxy resin sample by using the X-ray three-dimensional microscope specifically comprises the following steps:
bonding the glass beads embedded in the epoxy resin sample to the top end of a cross-shaped sample table, and placing the sample table into a high-contrast X-ray three-dimensional microscope for fixing;
selecting a set test voltage, a set current, a set exposure time, a set penetration rate and a set image resolution, measuring the diameter of the glass beads, and intercepting and storing the measured image.
Further, the set test voltage is 140KV, the set current is 70 μ a, the set exposure time is 5s, the set transmittance is 50%, and the set image resolution is 0.5 μm.
Further, the method for measuring the size of the glass bead after the gold spraying treatment by using the field emission environment electron microscope specifically comprises the following steps:
placing the glass beads subjected to metal spraying treatment into the field emission environment electron microscope, and selecting a set voltage and a set electron beam current in a high vacuum mode;
and when the definition of the image reaches a set condition, measuring the diameter of the glass bead after the gold spraying treatment, and storing the measured SEM image.
Further, the set voltage is 10KV, and the set electron beam current is 3.5 pA.
Further, the sizes of the glass beads and the glass beads after the gold spraying treatment are measured at least three times.
(3) Advantageous effects
In conclusion, the invention contrasts and measures the size of the glass microsphere and marks the standard size sample for the X-ray test of the composite material by the field emission environment electron microscope and the high-contrast X-ray three-dimensional microscope with higher resolution, thereby solving the problem that the standard size sample for the X-ray test in the prior art can not accurately contrast and measure the size of the microstructure.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic flow chart of a method for preparing a standard-sized sample for X-ray testing of a composite material according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of a method for testing a standard-sized sample for X-ray testing of a composite material according to an embodiment of the present invention;
FIG. 3 is a schematic illustration of an SEM image of a composite X-ray tested standard size sample for measuring the size of 80 μm glass microspheres in a test method provided by an embodiment of the invention;
FIG. 4 is a schematic illustration of an SEM image of a composite X-ray tested standard size sample for measuring the size of 100 μm glass microspheres in a test method provided by an embodiment of the invention;
FIG. 5 is a schematic illustration of an SEM image of a composite X-ray tested standard size sample for measuring the size of glass microspheres of 150 μm size;
FIG. 6 is a schematic illustration of an SEM image of a composite X-ray tested standard size sample measuring the size of glass beads of 200 μm size;
FIG. 7 is a schematic representation of an SEM image of a composite X-ray tested standard size sample measuring the size of 320 μm glass microspheres in a test method provided by an embodiment of the invention;
FIG. 8 is a schematic diagram of a CT image for measuring the size of 80 μm glass beads embedded in epoxy resin in a standard size sample test method for composite material X-ray testing according to an embodiment of the present invention;
FIG. 9 is a schematic diagram of a CT image for measuring the size of 100 μm glass beads embedded in epoxy resin in a standard size sample test method for composite material X-ray testing according to an embodiment of the present invention;
FIG. 10 is a schematic diagram of a CT image for measuring the size of 150 μm glass beads embedded in epoxy resin in a standard size sample test method for composite X-ray testing according to an embodiment of the present invention;
FIG. 11 is a schematic diagram of a CT image for measuring the size of glass beads embedded in epoxy resin in a 200 μm stage in a standard size sample testing method for composite X-ray testing according to an embodiment of the present invention;
fig. 12 is a schematic diagram of a CT image for measuring the size of 320 μm glass beads embedded in epoxy resin in the test method of a standard-sized sample for composite material X-ray testing according to an embodiment of the present invention.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following detailed description of the embodiments and the accompanying drawings are provided to illustrate the principles of the invention and are not intended to limit the scope of the invention, i.e., the invention is not limited to the embodiments described, but covers any modifications, alterations, and improvements in the parts, components, and connections without departing from the spirit of the invention.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
Fig. 1 is a schematic flow chart of a method for preparing a standard-sized sample for X-ray testing of a composite material according to a first aspect of an embodiment of the present invention, as shown in fig. 1, the method includes the following steps:
s101, selecting glass beads with set diameters, embedding the glass beads in a sample groove filled with epoxy resin, and curing the glass beads into a sample with a standard size;
s102, adhering glass beads with a set diameter to a conductive carbon adhesive tape, placing the conductive carbon adhesive tape in an ion sputtering instrument for spraying metal for a set time to form an SEM sample, and adhering the SEM sample to a small sample table.
In the above embodiment, glass beads having diameters of 80 μm, 100 μm, 150 μm, 200 μm, and 320 μm were selected, embedded in a sample cell (length 5mm, width 3mm, and thickness 3mm) filled with epoxy resin, and cured to obtain a standard size sample.
Glass beads with diameters of 80 μm, 100 μm, 150 μm, 200 μm and 320 μm are adhered to a conductive carbon tape, and are placed in an ion sputtering apparatus for gold spraying treatment for 1-2min to form an SEM (Scanning Electron Microscope) sample, and the SEM sample is adhered to a small sample stage.
The standard size sample is composed of epoxy resin and glass beads. The sample size comparison measurement method is adopted, and the equipment and tools used for the test are respectively as follows: a field emission environment electron microscope, a high-contrast X-ray three-dimensional microscope, an ion sputtering instrument, a cross sample table and a small sample table.
In some alternative embodiments, the glass microspheres of a set diameter have a particle size of 10-500 μm.
In some alternative embodiments, the set time is 1-2 min.
Fig. 2 is a schematic flow chart of a testing method of a standard-sized sample for X-ray testing of a composite material according to a second aspect of an embodiment of the present invention, as shown in fig. 2, the method includes the following steps:
s201, measuring the size of glass beads embedded in an epoxy resin sample by using an X-ray three-dimensional microscope;
s202, measuring the size of the glass beads subjected to gold spraying treatment by using a field emission environment electron microscope;
s203, determining that the epoxy resin sample is a standard size sample by comparing the sizes of the glass beads and the glass beads subjected to gold spraying treatment.
In the above embodiment, glass beads having diameters of 80 μm, 100 μm, 150 μm, 200 μm, and 320 μm were selected and used as SEM samples. Putting the glass bead sample subjected to metal spraying treatment into a field emission environment electron microscope in a high vacuum mode, with a voltage of 10KV and an electron beam current of 3.5pA, adjusting the image to be clear, wherein the magnification times are 250X, 500X and 1000X, the image resolution is 0.1 mu m, on an SEM image, selecting any point of a section of the glass bead by using a software measuring caliper, penetrating through the center of a cross of the sample to reach another section point of the glass bead, and the middle distance is the diameter of the glass bead.
Glass beads of 80 μm, 100 μm, 150 μm, 200 μm, and 320 μm in diameter were selected and prepared as samples for X-ray testing. Bonding an epoxy resin cured glass bead sample on the top end of a cross sample table, placing the cross sample table into a high-contrast X-ray three-dimensional microscope sample table, testing the voltage of 140KV, the current of 70 muA, the exposure time of 5s, the penetration rate of 50 percent and the image resolution of 0.5μm, selecting any point of a section of the glass bead on a CT image by using a software measuring caliper, penetrating through the center of the cross of the sample to reach another section point of the glass bead, wherein the middle distance is the diameter of the glass bead.
FIGS. 3-7 are schematic views of SEM images of glass bead size measurement in a standard size sample testing method of composite X-ray testing provided by embodiments of the present invention; among them, as shown in FIGS. 3 to 7, the measurement result of 80 μm-sized glass beads was 80.4 μm, the measurement result of 100 μm-sized glass beads was 102.3 μm, the measurement result of 150 μm-sized glass beads was 148.4 μm, the measurement result of 200 μm-sized glass beads was 203.4 μm, and the measurement result of 320 μm-sized glass beads was 325.9 μm.
FIGS. 8 to 12 are schematic diagrams of CT images for measuring the size of glass beads embedded in epoxy resin in a standard size sample test method for composite material X-ray test according to an embodiment of the present invention; among them, as shown in FIGS. 8 to 12, the measurement result of glass beads in 80 μm-sized resin was 80.8 μm, the measurement result of glass beads in 100 μm-sized resin was 103.2 μm, and the measurement result of glass beads in 150 μm-sized resin was: 150.2 μm, the glass beads in the 200 μm grade resin were measured to be 203.8 μm, and the glass beads in the 320 μm grade resin were measured to be 322.7 μm.
In order to avoid accidental errors of the experiment and improve the accuracy of the result, the number of the samples in each group is not less than 3.
The results of the comparison and calculation of the test data are shown in Table 1
TABLE 1
The sizes of the glass beads are measured by calculating a field emission environment electron microscope and a high-contrast X-ray three-dimensional microscope, and the relative error of the five groups of measurement results is less than 1 percent. The glass bead sample embedded in the epoxy resin can be calibrated to be a standard size sample by using an emission environment electron microscope with higher resolution and precision.
In some optional embodiments, in step S201, the method for measuring the size of the glass bead embedded in the epoxy resin sample by using an X-ray three-dimensional microscope specifically includes the following steps:
s2011, adhering glass beads embedded in an epoxy resin sample to the top end of a cross-shaped sample table, and placing the sample table into a high-contrast X-ray three-dimensional microscope for fixing;
s2012, selecting and setting test voltage, setting current, setting exposure time, setting penetration rate and setting image resolution, measuring the diameter of the glass bead, and intercepting and storing the measured image.
In some optional embodiments, in step S2012, the test voltage is set to 140KV, the current is set to 70 μ a, the exposure time is set to 5S, the transmittance is set to 50%, and the image resolution is set to 0.5 μm.
In some optional embodiments, in step S202, the step of measuring the size of the glass bead after the gold spraying treatment by using a field emission environment electron microscope specifically includes the following steps:
s2021, putting the glass beads subjected to the gold spraying treatment into a field emission environment electron microscope, and selecting a set voltage and a set electron beam current in a high vacuum mode;
and S2022, when the definition of the image reaches the set condition, measuring the diameter of the glass bead after the metal spraying treatment, and storing the measured SEM image.
In some alternative embodiments, in step S2021, the voltage is set to 10KV and the electron beam current is set to 3.5 pA.
In some optional embodiments, in steps S201 and S202, the sizes of the glass beads and the glass beads after the gold spraying treatment are measured at least three times.
It should be clear that the embodiments in this specification are described in a progressive manner, and the same or similar parts in the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. The present invention is not limited to the specific steps and structures described above and shown in the drawings. Also, a detailed description of known process techniques is omitted herein for the sake of brevity.
The above are merely examples of the present application and are not intended to limit the present application. Various modifications and alterations to this application will become apparent to those skilled in the art without departing from the scope of this invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (9)
1. A method for preparing a standard size sample for composite X-ray testing, the method comprising the steps of:
selecting glass beads with a set diameter, inlaying the glass beads in a sample groove filled with epoxy resin, and curing the glass beads into a sample with a standard size;
the glass beads with the set diameter are adhered to a conductive carbon adhesive tape, and the conductive carbon adhesive tape is placed in an ion sputtering instrument for spraying metal for set time to form an SEM sample and adhered to a small sample table.
2. The method for preparing a standard size sample for X-ray testing of composite materials according to claim 1, wherein the glass micro beads with a set diameter have a particle size of 10-500 μm.
3. The method of preparing a standard size sample for composite X-ray testing according to claim 1, wherein the set time is 1-2 min.
4. A method for testing a standard size sample for X-ray testing of a composite material, the method comprising the steps of:
measuring the size of the glass beads embedded in the epoxy resin sample by using an X-ray three-dimensional microscope;
measuring the size of the glass beads subjected to gold spraying treatment by using a field emission environment electron microscope;
and determining that the epoxy resin sample is a standard size sample by comparing the sizes of the glass beads and the glass beads after the gold spraying treatment.
5. The method for testing the standard-sized sample for the X-ray test of the composite material, according to claim 4, is characterized in that the method for measuring the size of the glass beads embedded in the epoxy resin sample by using an X-ray three-dimensional microscope specifically comprises the following steps:
bonding the glass beads embedded in the epoxy resin sample to the top end of a cross-shaped sample table, and placing the sample table into a high-contrast X-ray three-dimensional microscope for fixing;
selecting a set test voltage, a set current, a set exposure time, a set penetration rate and a set image resolution, measuring the diameter of the glass beads, and intercepting and storing the measured image.
6. The method of claim 5, wherein the set test voltage is 140KV, the set current is 70 μ A, the set exposure time is 5s, the set transmittance is 50%, and the set image resolution is 0.5 μm.
7. The method for testing standard-sized samples for X-ray testing of composite materials according to claim 4, wherein the step of measuring the size of the glass beads after the gold spraying treatment by using a field emission environment electron microscope specifically comprises the following steps:
placing the glass beads subjected to metal spraying treatment into the field emission environment electron microscope, and selecting a set voltage and a set electron beam current in a high vacuum mode;
and when the definition of the image reaches a set condition, measuring the diameter of the glass bead after the gold spraying treatment, and storing the measured SEM image.
8. The method of claim 7, wherein the set voltage is 10KV and the set electron beam current is 3.5 pA.
9. The method for testing standard-sized samples for X-ray testing of composite materials according to claim 4, wherein the sizes of the glass beads and the gold-sprayed glass beads are measured at least three times.
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| US4746571A (en) * | 1986-08-01 | 1988-05-24 | Wisconsin Alumni Research Foundation | X-ray detector efficiency standard for electron microscopes |
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| JPH07229860A (en) * | 1994-02-16 | 1995-08-29 | Hihakai Kensa Kk | Method, standard piece and device for evaluating defect height in radiation transmission test |
| JP2001080953A (en) * | 1999-09-08 | 2001-03-27 | Toshiba Tungaloy Co Ltd | Ceramic sintered compact and coated ceramic sintered compact |
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2020
- 2020-12-16 CN CN202011491655.5A patent/CN113418949B/en active Active
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| US4746571A (en) * | 1986-08-01 | 1988-05-24 | Wisconsin Alumni Research Foundation | X-ray detector efficiency standard for electron microscopes |
| US4955974A (en) * | 1988-08-18 | 1990-09-11 | Mcr Technology Corporation | Apparatus for generating x-ray holograms |
| JPH07229860A (en) * | 1994-02-16 | 1995-08-29 | Hihakai Kensa Kk | Method, standard piece and device for evaluating defect height in radiation transmission test |
| JP2001080953A (en) * | 1999-09-08 | 2001-03-27 | Toshiba Tungaloy Co Ltd | Ceramic sintered compact and coated ceramic sintered compact |
| US20100278440A1 (en) * | 2009-04-30 | 2010-11-04 | General Electric Company | Nondestructive inspection method and system |
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| CN108344885A (en) * | 2018-02-07 | 2018-07-31 | 陕西地建土地工程技术研究院有限责任公司 | A method of improving pedotheque scanning electron microscope observation electric conductivity |
| CN108444416A (en) * | 2018-06-13 | 2018-08-24 | 中国计量科学研究院 | A kind of standard group for length measurement calibrations |
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