CN110608939A - Ceramic electronic component metallographic section and preparation method thereof - Google Patents
Ceramic electronic component metallographic section and preparation method thereof Download PDFInfo
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- CN110608939A CN110608939A CN201910800099.6A CN201910800099A CN110608939A CN 110608939 A CN110608939 A CN 110608939A CN 201910800099 A CN201910800099 A CN 201910800099A CN 110608939 A CN110608939 A CN 110608939A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/364—Embedding or analogous mounting of samples using resins, epoxy
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/366—Moulds; Demoulding
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/368—Mounting multiple samples in one block, e.g. TMA [Tissue Microarrays]
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a preparation method of a ceramic electronic component microsection, which comprises the following steps: (1) placing samples to be detected in a mold in parallel, injecting alcohol into the mold to enable the alcohol to surround the samples to be detected and fill gaps among the samples to be detected; (2) injecting resin into the mold, and curing the resin to obtain a resin block; (3) and grinding and polishing the resin block. According to the invention, the sample to be detected is filled with alcohol, air is discharged in advance, and no air bubbles are generated around the sample to be detected after resin is injected, so that the sample to be detected is fully wrapped by the resin, and the sample to be detected is uniformly stressed during grinding and does not crack due to external force. The leveling property of the mixed resin and proper alcohol is good, the non-grinding surface of the resin block is smooth, the pressure applied to the resin block during grinding is uniform, and the grinding surface and the non-grinding surface of the ground resin block are kept parallel, so that when the resin block is observed under an optical microscope, the levelness of the observation surface is good.
Description
Technical Field
The invention relates to the field of component measurement and analysis, in particular to a ceramic electronic component microsection and a preparation method thereof.
Background
When a ceramic electronic component is usually subjected to microsection examination and analysis, a sample to be examined is arranged in a mold and injected with resin to prepare a resin block, then the sample fixed in the resin block is ground and polished, and finally the resin block is placed under a microscope to observe the sample.
Gaps with variable sizes often exist among samples to be detected arranged in the mold, and when resin is injected into the mold, air in the gaps is covered by the resin when the resin is not discharged, so that air bubbles are formed and attached to the sides of the samples to be detected. The bubble makes the sample of examining can not fully be wrapped up by resin, has the inhomogeneous easy fracture of sample atress of examining of fragility in the course of grinding to the grinding piece can get into the cavity formed by the bubble, oppresses or scrapes the sample of examining, treats the sample of examining and causes the damage, and these all bring inconvenience for the inspection analysis.
In addition, the resin with high viscosity has poor leveling property, which causes poor flatness of a non-polished surface (i.e., a surface opposite to the polished surface) of the resin block, uneven pressure applied to the resin block during polishing tends to incline the polished surface, and when the resin block is observed under an optical microscope, the levelness of the observed surface is not good, which is not favorable for quality inspection and analysis.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide a preparation method of a ceramic electronic component microsection. The ceramic electronic component microsection prepared by the method ensures that a sample to be detected is not influenced by air bubbles when a resin block is ground, and the levelness of an observation surface is better when the resin block is observed under an optical microscope, so that the sample preparation quality of the ceramic electronic component microsection is improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a ceramic electronic component microsection comprises the following steps:
(1) placing samples to be detected in a mold in parallel, injecting alcohol into the mold to enable the alcohol to surround the samples to be detected and fill gaps among the samples to be detected;
(2) injecting resin into the mold, and curing the resin to obtain a resin block;
(3) and grinding and polishing the resin block to finish the preparation of the ceramic electronic component microsection.
Preferably, in the step (1), the height of the mold is greater than that of the sample to be detected.
Preferably, in the step (2), the resin is acrylic resin or crystal glue.
Preferably, in the step (2), the volume ratio of the alcohol to the resin is 1: (10-20). The selection of the volume ratio can improve the leveling property of the mixed liquid of the resin and the alcohol and ensure that the resin block has enough strength and enough adhesive force between the resin block and a sample to be detected.
Preferably, an enclosing frame is placed in the mold, and the enclosing frame encloses the sample to be detected; the height of the surrounding frame is less than that of the mould.
Preferably, the material of the enclosure frame is one of plastic, ceramic, glass and metal.
Preferably, when alcohol is injected into the enclosing frame, the alcohol is filled in the sample to be detected and does not overflow the enclosing frame; when resin is injected into the mold, the resin and the alcohol are mixed, and the liquid level of the mixed liquid is higher than that of the surrounding frame. Thus, even if the grinding depth is large and the size of the mold is limited, the injection amount of the alcohol is not so large, the strength of the resin block is ensured and the generation of air bubbles between samples to be inspected is prevented.
Meanwhile, the invention also provides a ceramic electronic component microsection prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the sample to be detected is filled with alcohol, air is discharged in advance, and no air bubbles are generated around the sample to be detected after resin is injected, so that the sample to be detected is fully wrapped by the resin, and the sample to be detected is uniformly stressed during grinding and does not crack due to external force. The leveling property of the mixed resin and proper amount of alcohol is good, the non-grinding surface of the resin block is smooth, the pressure applied to the resin block during grinding is uniform, and the grinding surface and the non-grinding surface of the ground resin block are kept parallel, so that when the resin block is observed under an optical microscope, the levelness of the observation surface is good, and the sample preparation quality of the ceramic electronic component metallographic section is improved.
Drawings
FIG. 1 is a flow chart of a method for preparing a microsection of a ceramic electronic component according to the present invention;
FIG. 2 is a schematic view of a sample to be tested placed in a mold and alcohol injected into the mold;
FIG. 3 is a schematic view of a sample to be tested and an enclosure frame being placed in a mold and alcohol being injected into the enclosure frame;
FIG. 4 is an exemplary illustration of a ground surface of a resin block obtained after curing of the resin of the present invention;
FIG. 5 is an exemplary illustration of a ground surface of a resin block obtained after curing of a resin according to the prior art;
FIG. 6 is an exemplary illustration of a non-abrasive side of a resin block of the present invention;
FIG. 7 is an exemplary illustration of a non-abrasive side of a prior art resin block;
FIG. 8 is an exemplary view of a ground view of a resin block of the present invention;
FIG. 9 is an exemplary view of a prior art resin block after grinding;
wherein, 1, a sample to be detected; 2. a mold; 3. alcohol; 4. and (7) enclosing a frame.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
In an embodiment of the microsection of the ceramic electronic component, referring to fig. 1, the microsection of the ceramic electronic component in the embodiment is prepared by the following method:
step 1, placing samples to be detected in a mold in parallel, injecting alcohol into the mold to enable the alcohol to surround the samples to be detected, and filling gaps among the samples to be detected.
Referring to fig. 2, a sample 1 to be inspected is a ceramic electronic component. The height of the mold 2 is greater than that of the sample 1 to be inspected so that the resin more sufficiently wraps the sample 1 to be inspected. The samples 1 to be tested are placed in parallel in a mold 2, and then alcohol 3 is injected into the mold 2. Preferably, the amount of the alcohol 3 to be injected is controlled according to the desired grinding depth so that the liquid level of the alcohol 3 may be spread over the entire sample 1 to be inspected or may be spread over only a part of the height of the sample 1 to be inspected according to the actually desired grinding depth. The alcohol 3 may be injected using a dropper, preferably a dropper having a volume scale, so that the injection position and the injection amount of the alcohol 3 can be easily controlled.
And 2, injecting resin into the mold, and curing the resin to obtain a resin block.
The resin may be an acrylic resin or a crystal glue.
Because the gap between the samples to be detected is filled with alcohol, air is discharged in advance, and no air bubbles are generated on the periphery of the samples to be detected after resin is injected.
The alcohol and the resin are mixed to form a mixed solution, the viscosity of the mixed solution is smaller than that of the resin, so that the leveling property of the mixed solution is better, and the non-grinding surface of the cured resin block is smoother.
The volume ratio of alcohol to resin is 1: (10-20); by adjusting the proportion of the alcohol to the resin, the viscosity of the mixed liquid is reduced to a proper degree compared with the viscosity of the resin, and the leveling property of the mixed liquid, the strength of the resin block and the bonding effect of the resin block and a sample to be detected are considered. The mold with a proper size can be selected, so that the proportion of alcohol to resin can be adjusted more conveniently by adjusting the volume of the mold.
Referring to fig. 3, in other embodiments, a frame 4 may be placed inside the mold 2 in step 1, and the frame 4 surrounds the sample 1 to be tested. The height of the surrounding frame 4 is set according to the liquid level of the alcohol 3 to be injected, but is smaller than the height of the mold 2. And injecting alcohol 3 into the enclosing frame 4 to fill the sample 1 to be detected without overflowing the enclosing frame 4, and then injecting resin into the mould 2 to mix the resin and the alcohol 3, wherein the liquid level of the mixed liquid is higher than that of the enclosing frame 4. Thus, even in the case where the grinding depth is large and there is a limit to the size of the mold 2, it is possible to prevent the injection amount of the alcohol 3 from being too large, ensure the strength of the resin mass and prevent the generation of bubbles between samples to be inspected. The material of the enclosure frame 4 can be plastic, ceramic, glass, metal, etc.
For comparison of the ground surfaces of the resin blocks obtained after curing of the resins, reference is made to fig. 4 and 5. FIG. 4 shows the effect of the present invention, and FIG. 5 shows the effect of the prior art [ only the step of preparing resin for filling into the mold, and not including the step of injecting alcohol ]. Therefore, in the invention, the grinding surface has no cavity formed by bubbles, and the sample to be detected is fully wrapped by the resin; whereas the prior art abrasive surface has a number of cavities formed by bubbles. For a comparison of the non-ground side of the resin block, see fig. 6 and 7. FIG. 6 shows the effect of the present invention, and FIG. 7 shows the effect of the prior art [ only the step of preparing resin for filling into the mold, and not including the step of injecting alcohol ]. It can be seen that in the present invention, the non-abrasive surface is relatively flat; whereas the non-abrasive side of the prior art is rugged. In order to compare the levelness of the observation surface of the resin block after grinding, the sample in the resin block was magnified 1000 times under an optical microscope and observed, referring to fig. 8 and 9. FIG. 8 shows the effect of the present invention, and FIG. 9 shows the effect of the prior art [ only the step of preparing resin for filling into the mold, and not including the step of injecting alcohol ]. Therefore, in the invention, the whole image is clearer, which shows that the observation surface has good levelness; however, the image in the prior art has a fuzzy area, which indicates that the observation surface has poor levelness.
And 3, grinding and polishing the resin block to finish the preparation of the ceramic electronic component metallographic section.
The resin block can be ground to the required depth by an automatic grinding machine and then polished, thus finishing the preparation of the ceramic electronic component microsection. In the whole grinding process, the sample to be detected is fully wrapped by resin, so that the stress is uniform, the sample to be detected is not cracked due to external force, and the sample to be detected is not damaged by grinding scraps. The non-grinding surface of the resin block is relatively flat, the pressure applied to the resin block during grinding is uniform, and the grinding surface and the non-grinding surface of the ground resin block are kept parallel, so that the levelness of the observation surface is good when the resin block is observed under an optical microscope. After the preparation of the ceramic electronic component metallographic section is finished, an optical microscope or an electron microscope can be adopted for inspection and analysis.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The preparation method of the ceramic electronic component microsection is characterized by comprising the following steps of:
(1) placing samples to be detected in a mold in parallel, injecting alcohol into the mold to enable the alcohol to surround the samples to be detected and fill gaps among the samples to be detected;
(2) injecting resin into the mold, and curing the resin to obtain a resin block;
(3) and grinding and polishing the resin block to finish the preparation of the ceramic electronic component microsection.
2. The method for preparing a microsection of a ceramic electronic component according to claim 1, wherein in the step (1), the height of the die is greater than the height of the sample to be tested.
3. The method for preparing a microsection of a ceramic electronic component according to claim 1, wherein in the step (2), the resin is acrylic resin or crystal glue.
4. The method for preparing a microsection of a ceramic electronic component according to claim 1 or 3, wherein in the step (2), the volume ratio of the alcohol to the resin is 1: (10-20).
5. The method for preparing a microsection of a ceramic electronic component according to claim 1, wherein an enclosure frame is placed in the mold, and the enclosure frame encloses a sample to be detected; the height of the surrounding frame is less than that of the mould.
6. The method for preparing the microsection of the ceramic electronic component according to claim 5, wherein the material of the enclosure frame is one of plastic, ceramic, glass and metal.
7. The method for preparing a microsection of a ceramic electronic component according to claim 5, wherein when alcohol is injected into the surrounding frame, the alcohol fills the sample to be tested and does not overflow the surrounding frame; when resin is injected into the mold, the resin and the alcohol are mixed, and the liquid level of the mixed liquid is higher than that of the surrounding frame.
8. A ceramic electronic component microsection prepared by the preparation method of any one of claims 1 to 7.
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Cited By (3)
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| CN113698731A (en) * | 2021-08-26 | 2021-11-26 | 业成科技（成都）有限公司 | Resin filling method and apparatus |
| CN114323870A (en) * | 2022-01-06 | 2022-04-12 | 中国建筑科学研究院有限公司 | Preparation method of high-viscosity adhesive colloid performance sample |
| CN114486966A (en) * | 2021-12-08 | 2022-05-13 | 东风汽车集团股份有限公司 | Method for manufacturing sheet material scanning electron microscope energy spectrum analysis sample |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113698731A (en) * | 2021-08-26 | 2021-11-26 | 业成科技（成都）有限公司 | Resin filling method and apparatus |
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| CN114486966A (en) * | 2021-12-08 | 2022-05-13 | 东风汽车集团股份有限公司 | Method for manufacturing sheet material scanning electron microscope energy spectrum analysis sample |
| CN114486966B (en) * | 2021-12-08 | 2024-04-16 | 东风汽车集团股份有限公司 | Method for manufacturing thin-sheet material scanning electron microscope energy spectrum analysis sample |
| CN114323870A (en) * | 2022-01-06 | 2022-04-12 | 中国建筑科学研究院有限公司 | Preparation method of high-viscosity adhesive colloid performance sample |
| CN114323870B (en) * | 2022-01-06 | 2023-12-22 | 中国建筑科学研究院有限公司 | Preparation method of high-viscosity adhesive colloid performance sample |
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