CN111766127A - Membrane thickness detection method - Google Patents
Membrane thickness detection method Download PDFInfo
- Publication number
- CN111766127A CN111766127A CN202010745550.1A CN202010745550A CN111766127A CN 111766127 A CN111766127 A CN 111766127A CN 202010745550 A CN202010745550 A CN 202010745550A CN 111766127 A CN111766127 A CN 111766127A
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- CN
- China
- Prior art keywords
- sample
- film
- detection method
- film layer
- thickness detection
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Classifications
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
- G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
- G01B11/0616—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating
Abstract
The invention relates to sample preparation for detecting the thickness of a film (plating) layer after surface treatment and oxidation (plating) of a metal part, in particular to a film thickness detection method. Wrapping the cross section of a sample to be ground and polished by a plastic film, loading the wrapped sample into a clamping device, adjusting the position of the sample until the surface to be polished of the sample and the bottom surface of the clamping device are on the same plane, fixing and fastening the clamping device, grinding and polishing until the cross section of the sample is a mirror surface, and observing and measuring the thickness of the film under a microscope. The invention provides a rapid and efficient preparation technology for preventing detection result errors caused by improper sample preparation. The sample prepared by the method effectively avoids the damage of a film (plating) layer caused by the sample manufacturing process, and can accurately detect the thickness.
Description
Technical Field
The invention relates to sample preparation for detecting the thickness of a film (plating) layer after surface treatment and oxidation (plating) of a metal part, in particular to a film thickness detection method.
Background
The processing of the sample for measuring the thickness of the film (plating) layer must ensure the reality, continuity and integrity of the film (plating) layer observed under a microscope, so the manufacture of the sample is the key for accurately measuring the thickness of the film (plating) layer. The samples tested in GB/T6462 film (plating) were generally pretreated before production in the following two ways: cold and hot inlaying, namely, coating a protective coating (such as a gold coating) which is easier to distinguish outside a film (coating) layer, and then carrying out cold (hot) inlaying. The mosaic purpose is to increase the contact surface between the sample polishing surface and the polishing device, ensure the sample polishing surface to be the same horizontal plane to the maximum extent, and simultaneously protect the detected film (plating) layer from being damaged. However, the inlaid material is a high molecular material, the hardness and the wear resistance of the inlaid material are lower than those of metal parts, the inlaid material at the joint part of the inlaid sample and the metallographic sample is easily abraded earlier than the sample in the grinding and polishing processes of the inlaid sample, and meanwhile, the film (plating) layer is also seriously damaged to be a film (plating) free layer, which shows that the sample protrudes above the inlaid object (the convex platform feeling is touched), so that the error conclusion that the film (plating) layer is observed and detected to be zero is caused.
Disclosure of Invention
The invention provides a sample preparation method which is simple, rapid and efficient to operate, and aims to solve the problems that the cross section and the edge of a film (plating) layer covered by a sample are not completely flat or the edge is chamfered easily in the polishing process of the existing metal film (plating) layer sample, and the thickness of the complete film (plating) layer is difficult to accurately observe and detect. The sample prepared by the method effectively avoids the damage of a film (plating) layer caused by the sample manufacturing process, and can accurately detect the thickness.
Technical scheme
In order to solve the error condition which is easy to occur in the sample preparation, the invention provides the following technical scheme:
a film thickness detection method comprises the steps of wrapping the cross section of a sample to be ground and polished by a plastic film in a winding mode, loading the wrapped sample into a clamping device, adjusting the position of the sample until the surface to be polished of the sample and the bottom surface of the clamping device are on the same plane, fixing and fastening the clamping device, grinding and polishing until the cross section of the sample is a mirror surface, and observing and measuring the film thickness under a microscope.
When the film layer and the matrix of the cross section can not be identified, the cross section is etched by using the etching agent in GB/T6462.
And observing and measuring the thickness of the film layer under a microscope when a fine and clear boundary is generated on the cross section of the two metals after etching.
The etching agent is a nitric acid alcohol solution.
The sample is a strip processed along with the part in the same groove.
The plastic film is an electrical insulating tape.
The clamping device is made of metal.
And the grinding and polishing processes are carried out according to a sample preparation procedure of the metallographic sample.
The specific details are as follows:
(1) grinding the sample, wherein when the sample is manually and finely ground, regardless of the thickness of the abrasive paper, after the sample is ground, the color of the whole trace left on the abrasive paper is consistent in depth, the width of the trace is the same as the size of the ground surface of the sample, the trace of the arc trace is not required to appear, the flatness of the whole ground surface is ensured, and the chamfering phenomenon of the sample is reduced;
(2) the polishing time of the sample is 3-5 min;
(3) the selection of the erosion time and the erosion time of the sample are related to the material, the processing state and the freshness of the erosion agent.
The cross section of the sample is wound and wrapped on an object to be adhered and fixed, the adhesive tape shaft is rotated while being adhered, the adhesive tape is slowly opened at a small distance, the opened position of the adhesive tape is ensured to be straight and not inclined, and the adhesive tape is cut off after the adhesive tape is rotated and adhered to a required length position.
Technical effects
The invention relates to sample preparation for detecting the thickness of a film (plating) layer after surface treatment and oxidation (plating) of a metal part, and provides a rapid and efficient preparation technology for preventing detection result errors caused by improper sample preparation.
Detailed Description
The technical scheme of the invention is further explained in detail below, the cross section of a strip-shaped sample processed along with a part in the same groove, which needs to be ground and polished, is determined, a layer of electrical insulating tape is tightly wound around the cross section, and a film (plating) layer wrapping the surface of the sample is wrapped; and (3) putting the wrapped sample into a clamping device made of metal, adjusting the position of the sample until the surface to be polished of the sample and the bottom surface of the clamping device are on the same plane, fixing and fastening the clamping device, and then grinding and polishing the sample according to a sample preparation procedure of the metallographic sample until the cross section and the edge of the film (plating) layer are completely flat (no edge chamfer) and the mirror surface with an obvious interface line between the film (plating) layer and the metal matrix can be clearly observed.
For the sample with the part of the plating layer having the same color with the base metal and no obvious interface line after grinding and polishing, the polished cross section of the sample can be etched by using an etchant in GB/T6462, and the measurement is carried out after the etching treatment shows a clear thin line at the boundary surface of the film (plating) layer. Commonly used etchants include nital, picric acid, ammonium persulfate, nitrohydrochloric acid glycerol, aqua regia, ferric chloride ammonia, and the like.
The plastic film needs to have moderate strength and meets the experimental environment. The thickness is generally 0.13mm-0.15mm, the tensile rate at break is about 200%, if the strength of the plastic film is too high, the plastic film can not be guaranteed to completely wrap the cross section of the sample, the sample can be displaced during polishing due to untight wrapping, the polishing effect is greatly influenced, the thickness measurement is indirectly inaccurate, and the test effect cannot be achieved. If the strength of the plastic film is too low, when the device is used for clamping a sample wrapped by the plastic film, the outer surface of the sample is easily damaged by the clamping device. The insulating tape has certain strength and flexibility, can be tightly wrapped at a joint for a long time, is dry-cured and shaped under the influence of time and temperature, cannot fall off, is flame-retardant, and can be dampproof and antirust after being wrapped by the insulating tape.
The sample is a strip processed along with the part in the same groove. The sample shape and the part notch phase-match reduce the relative displacement who takes place among the test process to guarantee the terminal surface roughness.
The plastic film is an electrical insulating tape. The electrical tape is recommended because the detection requirement can be satisfied from the strength of the electrical tape.
The clamping device is made of metal. The clamping device is selected without excessive technical requirements, proper strength is guaranteed, deformation is not prone to occurring, and metal is adopted, so that the clamping device is easy to obtain.
And the grinding and polishing processes are carried out according to a sample preparation procedure of the metallographic sample. The preparation of the metallographic specimen is the prelude to the identification of the microstructure, and the material becomes the process with the requirements of metallographic observation through the steps of sampling, polishing, erosion and the like.
The sample preparation procedure of the metallographic sample comprises the following specific details:
(1) when the sample is ground manually and finely, regardless of the thickness of the abrasive paper, after the sample is ground, the color depth of the whole trace left on the abrasive paper is consistent, the width of the sample is the same as the size of the ground surface of the sample, and the trace of the arc trace is not required to appear.
(2) The polishing time of the sample is preferably 3-5min, scratches left by polishing in too short a time cannot be completely eliminated, the time is too long, pits are generated on the surface of the sample due to the falling of hard particles, and new scratches are likely to be generated on the sample with a softer material, so that the sample needs to be polished again.
(3) The selection of the erosion time, the erosion time of the sample is related to the material, the processing state, the freshness of the erosion agent and the like, the erosion time is too short, the microstructure part can be effectively displayed, the erosion time is too long, the microstructure is unclear, the accurate identification and the accurate evaluation of the microstructure are greatly influenced, the proper sample is eroded, the microstructure is clear at a glance, and a fresh and comfortable feeling is brought to people during observation,
the GB/T6462 etching agent is a national unified standard and belongs to the field of the prior art. The common etching agents are different according to different materials, different tissues have different etching agents, and the common etching agents are generally 3-4% of nitric acid-alcohol solutions.
It should be noted that the plastic film wrapping technique avoids wrinkles affecting the measurement. Firstly, an object to be adhered is fixed, the adhesive tape cannot be cut off and adhered according to the length of the object, the adhesive tape shaft is rotated while being adhered, the adhesive tape is slowly opened at a small distance, the opened position of the adhesive tape is ensured to be straight and not inclined, and the adhesive tape is cut off after being rotated and adhered to the position with the required length, so that the phenomenon of wrinkles can be avoided.
Claims (9)
1. A film layer thickness detection method is characterized in that: wrapping the cross section of a sample to be ground and polished by a plastic film, loading the wrapped sample into a clamping device, adjusting the position of the sample until the surface to be polished of the sample and the bottom surface of the clamping device are on the same plane, fixing and fastening the clamping device, grinding and polishing until the cross section of the sample is a mirror surface, and observing and measuring the thickness of the film under a microscope.
2. The film layer thickness detection method according to claim 1, wherein: when the film layer and the substrate of the cross section can not be identified, the cross section is etched by an etchant.
3. The film layer thickness detection method according to claim 2, wherein: when a fine and clear boundary is formed on the cross section of the two metals after etching, the thickness of the film is observed and measured under a microscope.
4. The film layer thickness detection method according to claim 1, wherein: the etching agent is a nitric acid alcohol solution.
5. The film layer thickness detection method according to claim 1, wherein: the sample is a strip processed along with the part in the same groove.
6. The film layer thickness detection method according to claim 1, wherein: the plastic film is an electrical insulating tape.
7. The film layer thickness detection method according to claim 1, wherein: the clamping device is made of metal.
8. The film layer thickness detection method according to claim 1, wherein: the grinding and polishing processes are carried out according to a sample preparation procedure of a metallographic sample, and the specific details are as follows:
(1) grinding the sample, wherein when the sample is manually and finely ground, regardless of the thickness of the abrasive paper, after the sample is ground, the color of the whole trace left on the abrasive paper is consistent in depth, the width of the trace is the same as the size of the ground surface of the sample, the trace of the arc trace is not required to appear, the flatness of the whole ground surface is ensured, and the chamfering phenomenon of the sample is reduced;
(2) the polishing time of the sample is 3-5 min;
(3) the selection of the erosion time and the erosion time of the sample are related to the material, the processing state and the freshness of the erosion agent.
9. The film layer thickness detection method according to claim 1, wherein: the cross section of the sample is wound and wrapped on an object to be adhered and fixed, the adhesive tape shaft is rotated while being adhered, the adhesive tape is slowly opened at a small distance, the opened position of the adhesive tape is ensured to be straight and not inclined, and the adhesive tape is cut off after the adhesive tape is rotated and adhered to a required length position.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010745550.1A CN111766127A (en) | 2020-07-29 | 2020-07-29 | Membrane thickness detection method |
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| CN202010745550.1A CN111766127A (en) | 2020-07-29 | 2020-07-29 | Membrane thickness detection method |
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| CN111766127A true CN111766127A (en) | 2020-10-13 |
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| CN202010745550.1A Pending CN111766127A (en) | 2020-07-29 | 2020-07-29 | Membrane thickness detection method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113686273A (en) * | 2021-07-28 | 2021-11-23 | 临海市伟星化学科技有限公司 | Thickness measuring method for surface film layer of electroplated part |
| CN114322798A (en) * | 2022-01-28 | 2022-04-12 | 唐山瑞丰钢铁（集团）有限公司 | Hot rolled strip Fe using optical microscope3O4Method for measuring thickness value |
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| CN104266595A (en) * | 2014-09-29 | 2015-01-07 | 宁波金田新材料有限公司 | Microscopic detection method for paint film thickness of enameled wire |
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| CN110596167A (en) * | 2019-09-12 | 2019-12-20 | 北京首钢股份有限公司 | Sample preparation process method |
| CN111024469A (en) * | 2019-12-25 | 2020-04-17 | 珠海格力电工有限公司 | Method for testing eccentricity of enameled wire |
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2020
- 2020-07-29 CN CN202010745550.1A patent/CN111766127A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH11194078A (en) * | 1998-01-07 | 1999-07-21 | Matsushita Electron Corp | Method for preparing sample for transmission electron microscope observation and apparatus for preparing sample |
| CN103196379A (en) * | 2013-03-11 | 2013-07-10 | 江苏常铝铝业股份有限公司 | Measurement method of thickness of aluminium and aluminium alloy sheet material coating layer |
| CN104266595A (en) * | 2014-09-29 | 2015-01-07 | 宁波金田新材料有限公司 | Microscopic detection method for paint film thickness of enameled wire |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113686273A (en) * | 2021-07-28 | 2021-11-23 | 临海市伟星化学科技有限公司 | Thickness measuring method for surface film layer of electroplated part |
| CN114322798A (en) * | 2022-01-28 | 2022-04-12 | 唐山瑞丰钢铁（集团）有限公司 | Hot rolled strip Fe using optical microscope3O4Method for measuring thickness value |
| CN114322798B (en) * | 2022-01-28 | 2024-03-08 | 唐山瑞丰钢铁（集团）有限公司 | Fe of hot rolled strip steel by using optical microscope 3 O 4 Method for measuring thickness value |
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