CN111982625A - Method for preparing electrochemical test sample of pipe - Google Patents
Method for preparing electrochemical test sample of pipe Download PDFInfo
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- CN111982625A CN111982625A CN202010831768.9A CN202010831768A CN111982625A CN 111982625 A CN111982625 A CN 111982625A CN 202010831768 A CN202010831768 A CN 202010831768A CN 111982625 A CN111982625 A CN 111982625A
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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
- G01N1/34—Purifying; Cleaning
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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
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N2001/2873—Cutting or cleaving
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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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Abstract
The invention provides a method for preparing a tubular product electrochemical test sample, which comprises the following steps: (1) preparation of the test: cutting an arc-shaped test sample for testing; (2) welding a lead: welding a copper wire at the center of the back of the observation surface of the arc-shaped sample; (3) manufacturing an insulating sleeve: cutting an insulating sleeve from an insulating pipe, wherein the height of the insulating sleeve is 10-20 mm longer than that of the test sample; (4) placing a sample: fixing the sample in an insulating sleeve; (5) filling and sealing: fixing the bottom of the insulating sleeve, and filling epoxy resin into the insulating sleeve to seal the sample; (6) drying: drying the sealed sample; (7) polishing; (8) polishing; (9) cleaning; (10) the surface area was calculated. The method for preparing the electrochemical test sample of the pipe solves the problems that the arc-shaped sample of the pipe is difficult to polish, seal and calculate the surface area, and provides a sample preparation method for the electrochemical analysis of the pipe; the invention keeps the original structure and surface of the pipe, and the measured data is more real and reliable.
Description
Technical Field
The invention relates to the technical field of metal corrosion detection and analysis, in particular to a method for preparing a tubular product electrochemical test sample.
Background
The electrochemical corrosion experiment has strict requirements on the corrosion surface treatment of a sample to be measured so as to realize accurate corrosion area measurement, the traditional process of electrochemically analyzing the corrosion resistance of the pipe generally adopts a machining mode to cut a standard plane size sample or flatten or roll a thin-walled pipe and then anneal the flattened or rolled pipe to prepare the standard sample, the integral structure of the pipe along the wall thickness direction has deviation, particularly the outer surface and the inner part of the wall thickness have obvious difference, so that the plane sample is cut along the wall thickness direction, the structure of the sample does not have representativeness, the measurement result has large fluctuation, the thin-walled pipe is flattened or rolled, the original structure of the pipe is seriously damaged by the annealing process, the corrosion resistance of the pipe is not smooth and has a relationship with the structure and is directly related with a special proportion of grain boundary, and the method can cause the distortion of the measurement result.
Patent application No. 201610236020.8 discloses an electrochemical corrosion experimental device and method for realizing measurement of multi-size samples, which provides a precise corrosion area preformed hole, so that the area of each experiment is precisely controlled, the problem that each sample to be measured needs to be measured and sealed before measurement in the prior art is solved, the complicated steps of sample sealing are simplified, experimental errors are reduced, and experimental time is shortened; patent application No. 201210115763.1 discloses an electrochemical corrosion sample preparation device and method, which also aims to solve the problem of troublesome sample sealing. However, the above patents and methods are not suitable for electrochemical evaluation of corrosion resistance of pipes.
Disclosure of Invention
The invention aims to overcome and supplement the defects in the prior art, and provides a method for preparing a pipe electrochemical test sample, which can more truly reflect the corrosion resistance of a pipe by keeping the structure and the grain boundary state of the surface of the pipe. The technical scheme adopted by the invention is as follows:
a method of preparing a pipe electrochemical test specimen, wherein: the method comprises the following steps:
(1) preparation of the test: providing a pipe and measuring the size of the pipe, and cutting an arc-shaped test sample for testing by using linear cutting;
(2) welding a lead: welding a copper wire at the center of the back of the observation surface of the arc-shaped sample;
(3) manufacturing an insulating sleeve: cutting an insulating sleeve from an insulating pipe, wherein the height of the insulating sleeve is 10-20 mm longer than that of the test sample;
(4) placing a sample: fixing a sample in an insulating sleeve, and keeping the distance between the sample and the edge of the insulating sleeve to be 5-10 mm;
(5) filling and sealing: fixing the bottom of the insulating sleeve, and filling epoxy resin into the insulating sleeve to seal the sample;
(6) drying: drying and hardening the sealed sample;
(7) polishing: polishing the hardened sample by a drilling machine until the whole observation surface of the sample can be seen;
(8) polishing: polishing the polished sample by a drilling machine, wherein a polishing tool adopts a louver wheel, the mesh number of the louver wheel is 240 meshes, the polishing tool polishes the surface of an original pipe, then gradually increases the mesh number to 600 meshes and 1000 meshes, and gradually polishes a nylon wheel and a felt wheel, so that the scratches of the previous pass cannot be observed after each pass of polishing;
(9) cleaning: carrying out ultrasonic cleaning on the polished surface;
(10) calculating the surface area: modeling according to the size measured in the step (1) by using three-dimensional software, and measuring and reading the surface area of the sample.
Preferably, the method for preparing the electrochemical test sample of the pipe comprises the following steps: the size of the sample in the step (1) is 5-20 mm long and 5-20 mm wide.
Preferably, the method for preparing the electrochemical test sample of the pipe comprises the following steps: and (3) welding a copper wire at the center of the back of the sample observation surface by using an electric iron in the step (2), wherein the electric iron is used for soldering.
Preferably, the method for preparing the electrochemical test sample of the pipe comprises the following steps: the copper wire in the step (2) is an insulated hard wire, and the section size is 1-3 mm2。
Preferably, the method for preparing the electrochemical test sample of the pipe comprises the following steps: the insulating cover is made of PVC materials, and the inner diameter of the insulating cover is smaller than the outer diameter of the arc-shaped sample.
Preferably, the method for preparing the electrochemical test sample of the pipe comprises the following steps: the drying in the step (6) is room temperature air drying or oven drying, and the oven drying temperature is less than or equal to 60 ℃.
Preferably, the method for preparing the electrochemical test sample of the pipe comprises the following steps: and (5) the rotating speed of the drilling machine in the step (6) and the step (7) is 20-100 r/min.
The invention has the advantages that:
the method for preparing the electrochemical test sample of the pipe solves the problems that the arc-shaped sample of the pipe is difficult to polish, seal and calculate the surface area, and provides a sample preparation method for the electrochemical analysis of the pipe; the invention keeps the original structure and surface of the pipe, and the measured data is more real and reliable.
Drawings
FIG. 1 is a process flow chart of the method for preparing the electrochemical test sample of the pipe material.
Detailed Description
The invention is further illustrated by the following specific figures and examples.
Example 1:
a method of preparing a pipe electrochemical test specimen, wherein: the method comprises the following steps:
(1) preparation of a sample: selecting a test pipe, measuring the outer diameter, the inner diameter, the wall thickness and other dimensions of the pipe, measuring at least 3 points of each dimension of a sample, taking an average value, cutting the test arc-shaped sample by using linear cutting perpendicular to the axis of the pipe, wherein the cutting cooling liquid of the selected linear cutting cannot generate a corrosion reaction with the tested sample, and the cut sample has the length of 5mm, the width of 5mm and the same length and width;
(2) welding a lead: soldering copper wire to the center of the back of the sample observation surface with an electric iron, wherein the electric iron is used for soldering, the wire is an insulated hard wire, and the section size is 1mm2；
(3) Manufacturing an insulating sleeve: cutting an insulating sleeve by adopting an insulating pipe, wherein the height of the insulating sleeve is 10mm longer than that of the test sample, the insulating sleeve is made of PVC (polyvinyl chloride), and the inner diameter of the insulating sleeve in the pipe size is smaller than the outer diameter of the measured metal pipe;
(4) placing a sample: fixing a sample in an insulating sleeve by using an insulating elastic sheet, wherein the sample is centered and 5mm away from the edge of the insulating sleeve, the observation surface of the sample is tightly attached to the inner surface of the pipe, and the insulating sleeve is made by cutting an insulating pipe;
(5) filling and sealing: sealing the bottom of the insulating sleeve by using an adhesive tape, adhering the insulating sleeve on a smooth glass plate, filling prepared epoxy resin, wherein the epoxy resin is transparent and a sample can be observed;
(6) drying: air-drying the sealed sample at room temperature;
(7) polishing: grinding the hardened sample, wherein the grinding equipment adopts a speed-adjustable bench drill, the polishing tool adopts an abrasive paper louver wheel, the number of the louver wheels is 80 meshes, the whole observation surface of the sample can be seen by naked eyes after grinding, and a small amount of epoxy resin is added;
(8) polishing: polishing the polished sample, wherein the polishing equipment adopts a speed-adjustable bench drill, the polishing tool adopts a sand paper hundred-blade wheel, the mesh number of the louver wheel is 240 meshes, the surface of the original pipe is polished, then the mesh number is increased step by step to 600 meshes and 1000 meshes, a nylon wheel and a felt cloth wheel are polished step by step, the condition that the scratch of the previous step cannot be observed after each step of polishing is ensured, and alcohol is adopted for cooling in the polishing process to prevent heating;
(9) cleaning: carrying out ultrasonic cleaning on the polished surface, adopting acetone as a cleaning solution, and after air drying, observing that the surface has no abrasion defect and then using;
(10) calculating the surface area: and (3) modeling by using three-dimensional software SolidWorks according to the dimension measured in the step (1), and directly measuring and reading the surface area of the sample.
And 7) and 8) adopting a speed-adjustable bench drilling machine to rotate at a speed of 20r/min, wherein the rotating speed is lower when the mesh number is smaller, so that the surface of the sample is prevented from being damaged by too high speed.
Example 2
A method of preparing a pipe electrochemical test specimen, wherein: the method comprises the following steps:
(1) preparation of a sample: selecting a test pipe, measuring the outer diameter, the inner diameter, the wall thickness and other dimensions of the pipe, measuring at least 3 points of each dimension of a sample, taking an average value, cutting the test arc-shaped sample by linear cutting perpendicular to the axis of the pipe, wherein the cut sample has the size of 10mm in length, 10mm in width and the same length and width, and the cutting cooling liquid of the linear cutting cannot generate a corrosion reaction with the tested sample;
(2) welding a lead: soldering copper wire to the center of the back of the sample observation surface with an electric iron, wherein the electric iron is used for soldering, the wire is an insulated hard wire, and the section size is 2mm2；
(3) Manufacturing an insulating sleeve: cutting an insulating sleeve from an insulating pipe, wherein the height of the insulating sleeve is 16mm longer than that of the test sample, the insulating sleeve is made of PVC, the inner diameter of the insulating sleeve in the size of the pipe is smaller than the outer diameter of the measured metal pipe, and the insulating sleeve is made by cutting the insulating pipe;
(4) placing a sample: fixing the sample in an insulating sleeve by using an insulating elastic sheet, wherein the sample is centered and is 8mm away from the edge of the insulating sleeve, and the observation surface of the sample is tightly attached to the inner surface of the pipe;
(5) filling and sealing: sealing the bottom of the insulating sleeve by using an adhesive tape, adhering the insulating sleeve on a smooth glass plate, filling prepared epoxy resin, wherein the epoxy resin is transparent and a sample can be observed;
(6) drying: drying the sealed sample in an oven at 50 ℃;
(7) polishing: grinding the hardened sample, wherein the grinding equipment adopts a speed-adjustable bench drill, the polishing tool adopts an abrasive paper louver wheel, the number of the louver wheels is 80 meshes, the whole observation surface of the sample can be seen by naked eyes after grinding, and a small amount of epoxy resin is added;
(8) polishing: polishing the polished sample, wherein the polishing equipment adopts a speed-adjustable bench drill, the polishing tool adopts a sand paper hundred-blade wheel, the mesh number of the louver wheel is 240 meshes, the surface of the original pipe is polished, then the mesh number is increased step by step to 600 meshes and 1000 meshes, a nylon wheel and a felt cloth wheel are polished step by step, the condition that the scratch of the previous step cannot be observed after each step of polishing is ensured, and alcohol is adopted for cooling in the polishing process to prevent heating;
(9) cleaning: carrying out ultrasonic cleaning on the polished surface, adopting acetone as a cleaning solution, and after air drying, observing that the surface has no abrasion defect and then using;
(10) calculating the surface area: and (3) modeling by using three-dimensional software SolidWorks according to the dimension measured in the step (1), and directly measuring and reading the surface area of the sample.
And in the step 7) and the step 8), the rotating speed of the bench drilling machine with adjustable speed is 50r/min, and the rotating speed is lower when the mesh number is smaller, so that the surface of the sample is prevented from being damaged due to too high speed.
Example 3
A method of preparing a pipe electrochemical test specimen, wherein: the method comprises the following steps:
(1) preparation of a sample: selecting a test pipe, measuring the outer diameter, the inner diameter, the wall thickness and other dimensions of the pipe, cutting an arc-shaped test sample for the test by linear cutting perpendicular to the axis of the pipe, wherein the cut test sample has the length of 20mm, the width of 20mm and the length and the width of the same, each dimension of the test sample is measured at least at 3 points to obtain an average value, and the cutting cooling liquid for the linear cutting cannot generate a corrosion reaction with the tested sample;
(2) welding a lead: soldering copper wire at the center of the back of the sample observation surface with an electric iron, wherein the electric iron is used for soldering, the wire is an insulated hard wire, and the section size is 3mm2；
(3) Manufacturing an insulating sleeve: cutting an insulating sleeve by adopting an insulating pipe, wherein the height of the insulating sleeve is 20mm longer than that of the test sample, the insulating sleeve is made of PVC (polyvinyl chloride), and the inner diameter of the insulating sleeve in the pipe size is smaller than the outer diameter of the measured metal pipe;
(4) placing a sample: fixing a sample in an insulating sleeve by using an insulating elastic sheet, wherein the insulating sleeve is made by cutting an insulating tube, the sample is centered and 10mm away from the edge of the insulating sleeve, and the observation surface of the sample is tightly attached to the inner surface of the tube;
(5) filling and sealing: sealing the bottom of the insulating sleeve by using an adhesive tape, adhering the insulating sleeve on a smooth glass plate, filling prepared epoxy resin, wherein the epoxy resin is transparent and a sample can be observed;
(6) drying: drying the sealed sample by using an oven at the temperature of 60 ℃;
(7) polishing: grinding the hardened sample, wherein the grinding equipment adopts a speed-adjustable bench drill, the polishing tool adopts an abrasive paper louver wheel, the number of the louver wheels is 80 meshes, the whole observation surface of the sample can be seen by naked eyes after grinding, and a small amount of epoxy resin is added;
(8) polishing: polishing the polished sample, wherein the polishing equipment adopts a speed-adjustable bench drill, the polishing tool adopts a sand paper hundred-blade wheel, the mesh number of the louver wheel is 240 meshes, the surface of the original pipe is polished, then the mesh number is increased step by step to 600 meshes and 1000 meshes, a nylon wheel and a felt cloth wheel are polished step by step, the condition that the scratch of the previous step cannot be observed after each step of polishing is ensured, and alcohol is adopted for cooling in the polishing process to prevent heating;
(9) cleaning: carrying out ultrasonic cleaning on the polished surface, adopting acetone as a cleaning solution, and after air drying, observing that the surface has no abrasion defect and then using;
(10) calculating the surface area: and (3) modeling by using three-dimensional software SolidWorks according to the dimension measured in the step (1), and directly measuring and reading the surface area of the sample.
And in the step 7) and the step 8), the rotating speed of the table drilling machine with adjustable speed is 100r/min, and the rotating speed is lower when the mesh number is smaller, so that the surface of the sample is prevented from being damaged due to too high speed.
The main principle of the invention lies in grinding and polishing of the arc-shaped sample, the traditional grinding and polishing adopts metallographic polishing equipment or manual polishing equipment, the metallographic polishing equipment can only grind and polish the plane sample, the manual polishing equipment needs to fix the sample for polishing, the method is very easy to damage the surface of the pipe sample and can not polish the arc-shaped sample, and the defects of the equipment are overcome by adopting flexible fixed polishing equipment. And the arc-shaped sample is packaged, and the edge of the sample is fully attached to the inner wall of the insulating pipe by adopting the insulating pipe with the inner diameter of the insulating pipe smaller than the outer diameter of the pipe, so that the pipe is conveniently packaged by epoxy resin, and the problem that the surface area of the arc-shaped sample is difficult to calculate is solved by adopting three-dimensional software to calculate the surface area of the sample.
The invention solves the problems that the arc-shaped sample of the pipe is difficult to polish, seal and calculate the surface area, and provides a sample preparation method for the electrochemical analysis of the pipe; the invention keeps the original structure and surface of the pipe, and the measured data is more real and reliable.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may 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, which should be covered by the claims of the present invention.
Claims (7)
1. A method for preparing a tubular product electrochemical test sample is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of the test: providing a pipe and measuring the size of the pipe, and cutting an arc-shaped test sample for testing by using linear cutting;
(2) welding a lead: welding a copper wire at the center of the back of the observation surface of the arc-shaped sample;
(3) manufacturing an insulating sleeve: cutting an insulating sleeve from an insulating pipe, wherein the height of the insulating sleeve is 10-20 mm longer than that of the test sample;
(4) placing a sample: fixing a sample in an insulating sleeve, and keeping the distance between the sample and the edge of the insulating sleeve to be 5-10 mm;
(5) filling and sealing: fixing the bottom of the insulating sleeve, and filling epoxy resin into the insulating sleeve to seal the sample;
(6) drying: drying and hardening the sealed sample;
(7) polishing: polishing the hardened sample by a drilling machine until the whole observation surface of the sample can be seen;
(8) polishing: polishing the polished sample by a drilling machine, wherein a polishing tool adopts a louver wheel, the mesh number of the louver wheel is 240 meshes, the polishing tool polishes the surface of an original pipe, then gradually increases the mesh number to 600 meshes and 1000 meshes, and gradually polishes a nylon wheel and a felt wheel, so that the scratches of the previous pass cannot be observed after each pass of polishing;
(9) cleaning: carrying out ultrasonic cleaning on the polished surface;
(10) calculating the surface area: modeling according to the size measured in the step (1) by using three-dimensional software, and measuring and reading the surface area of the sample.
2. The method for preparing the electrochemical test sample of the pipe according to claim 1, wherein: the size of the sample in the step (1) is 5-20 mm long and 5-20 mm wide.
3. The method for preparing the electrochemical test sample of the pipe according to claim 1, wherein: and (3) welding a copper wire at the center of the back of the sample observation surface by using an electric iron in the step (2), wherein the electric iron is used for soldering.
4. The method for preparing the electrochemical test sample of the pipe according to claim 1, wherein: the copper wire in the step (2) is an insulated hard wire, and the section size is 1-3 mm2。
5. The method for preparing the electrochemical test sample of the pipe according to claim 1, wherein: the insulating cover is made of PVC materials, and the inner diameter of the insulating cover is smaller than the outer diameter of the arc-shaped sample.
6. The method for preparing the electrochemical test sample of the pipe according to claim 1, wherein: the drying in the step (6) is room temperature air drying or oven drying, and the oven drying temperature is less than or equal to 60 ℃.
7. The method for preparing the electrochemical test sample of the pipe according to claim 1, wherein: and (5) the rotating speed of the drilling machine in the step (6) and the step (7) is 20-100 r/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101692029A (en) * | 2009-04-30 | 2010-04-07 | 上海大学 | Method for testing antiwear characteristic of ultrathin modified coating |
| CN207051071U (en) * | 2017-07-04 | 2018-02-27 | 山东建筑大学 | A kind of experiment inlays electrochemical sample fixing device with epoxy resin |
| CN109632457A (en) * | 2019-02-22 | 2019-04-16 | 西安文理学院 | A kind of device and method being used to prepare electrochemical corrosion test sample |
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2020
- 2020-08-18 CN CN202010831768.9A patent/CN111982625A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101692029A (en) * | 2009-04-30 | 2010-04-07 | 上海大学 | Method for testing antiwear characteristic of ultrathin modified coating |
| CN207051071U (en) * | 2017-07-04 | 2018-02-27 | 山东建筑大学 | A kind of experiment inlays electrochemical sample fixing device with epoxy resin |
| CN109632457A (en) * | 2019-02-22 | 2019-04-16 | 西安文理学院 | A kind of device and method being used to prepare electrochemical corrosion test sample |
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