CN113896953A - Metallographic coated test paper and preparation method thereof - Google Patents
Metallographic coated test paper and preparation method thereof Download PDFInfo
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- CN113896953A CN113896953A CN202111153195.XA CN202111153195A CN113896953A CN 113896953 A CN113896953 A CN 113896953A CN 202111153195 A CN202111153195 A CN 202111153195A CN 113896953 A CN113896953 A CN 113896953A
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- test paper
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000975 dye Substances 0.000 claims abstract description 50
- 239000002904 solvent Substances 0.000 claims abstract description 50
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 36
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 36
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000006228 supernatant Substances 0.000 claims description 13
- ZXJXZNDDNMQXFV-UHFFFAOYSA-M crystal violet Chemical group [Cl-].C1=CC(N(C)C)=CC=C1[C+](C=1C=CC(=CC=1)N(C)C)C1=CC=C(N(C)C)C=C1 ZXJXZNDDNMQXFV-UHFFFAOYSA-M 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 238000003892 spreading Methods 0.000 claims description 4
- 230000000007 visual effect Effects 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- 238000005070 sampling Methods 0.000 description 8
- 238000001514 detection method Methods 0.000 description 7
- 238000009472 formulation Methods 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000007431 microscopic evaluation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/29—Compounds containing one or more carbon-to-nitrogen double bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
- C08K5/523—Esters of phosphoric acids, e.g. of H3PO4 with hydroxyaryl compounds
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Paper (AREA)
Abstract
The invention discloses metallographic coated test paper and a preparation method thereof. The proportion of ethyl cellulose, triphenyl phosphate, dye and solvent is (20-80) g, (0.1-20) g, (0.001-0.1) g and (200-500) mL, and the test paper has the characteristics of good flexibility, low cost, high definition, and excellent contrast and visual field brightness.
Description
Technical Field
The invention belongs to the field of metallographic detection, and relates to metallographic coated test paper and a preparation method thereof.
Background
The metallographic structure reflects the specific form of the metal metallographic phase, and the internal structure of the metal or the alloy can be observed by a metallographic method. The commonly used metallographic detection method is metallographic microscope observation or sampling with metallographic coated test paper. The metallographic microscope can be used for conveniently observing metallographic images and analyzing metallographic maps, and the metallographic microscope is used for observing, inspecting and analyzing the internal structure of the metal, is a common metallographic detection method and is widely used for microscopic analysis of metals and alloys. However, the application of the metallographic microscope is limited, the requirements on the field are high, some parts are not suitable for being divided and brought back for analysis, and the metallographic microscope is inconvenient to detect on the field. The metallographic coated test paper can solve the problem.
The metallographic coated test paper is a plastic film manufactured by means of a replica principle of a transmission electron microscope, the traditional coating is that cellulose acetate, triphenyl phosphate (TPP) and dye are dissolved in acetone, the melted solution is spread on a flat, clean and dry surface, and after acetone is volatilized, the manufactured film can also meet field detection, but has the characteristics of difficult solvent purchase and approval, difficult carrying, higher cost and the like. Compared with the traditional acetone film coating technology, the novel film coating technology solves the problems of carrying and cost, but the dissolution and toughness of the dye are still poor, and the prepared solution can be used after being further treated after being placed for a long time.
Therefore, there is a need for improved test strip formulations that increase flexibility, improve clarity, increase contrast and field brightness, and reduce cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the metallographic coated test paper and the preparation method thereof.
In order to achieve the purpose, the metallographic coated test paper is prepared from ethyl cellulose, triphenyl phosphate, dye and a solvent.
The proportions of ethyl cellulose, triphenyl phosphate, dye and solvent are (20-80) g, (0.1-20) g, (0.001-0.1) g and (200-500) mL.
The solvent is absolute ethyl alcohol.
The dye is methyl violet.
A preparation method of metallographic coated test paper comprises the following steps:
and adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, and flatly spreading and drying to form a film, thereby obtaining the metallographic coated test paper.
The proportions of ethyl cellulose, triphenyl phosphate, dye and solvent are (20-80) g, (0.1-20) g, (0.001-0.1) g and (200-500) mL.
The solvent is absolute ethyl alcohol.
The method specifically comprises the following steps:
adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, filtering or standing, taking supernatant, then flatly paving on a bottom plate with a smooth surface, and then drying to form a film, thus obtaining the metallographic coated test paper.
The surface of the base plate was cleaned by absolute ethanol before tiling.
The dye is methyl violet.
The invention has the following beneficial effects:
the metallographic coated test paper and the preparation method thereof are prepared from ethyl cellulose, triphenyl phosphate, dye and solvent during specific operation, and the definition and the detection effect are improved by changing the formula of the metallographic coated test paper for detection; after sampling, the sample can be directly observed and observed by an optical microscope, so that the detection method is more convenient and faster, the solvent is easily obtained, the cost is greatly reduced, the flexibility and the contrast of the finished product are good, and the finished product can be obtained by the solution after long-time storage without further treatment.
Drawings
FIG. 1a is a schematic diagram of a gold phase according to the first embodiment;
FIG. 1b is an on-site metallographic picture of an acetone formulation;
FIG. 2a is the metallographic image obtained in example two;
FIG. 2b is an on-site metallographic picture of an acetone formulation;
FIG. 3a is the metallographic image obtained in the third example;
figure 3b is an in situ gold phase diagram of an acetone formulation.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments, and are not intended to limit the scope of the present disclosure. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present disclosure. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
There is shown in the drawings a schematic block diagram of a disclosed embodiment in accordance with the invention. The figures are not drawn to scale, wherein certain details are exaggerated and possibly omitted for clarity of presentation. The shapes of various regions, layers and their relative sizes and positional relationships shown in the drawings are merely exemplary, and deviations may occur in practice due to manufacturing tolerances or technical limitations, and a person skilled in the art may additionally design regions/layers having different shapes, sizes, relative positions, according to actual needs.
Example one
The metallographic coated test paper is prepared from ethyl cellulose, triphenyl phosphate, dye and solvent.
The proportion of ethyl cellulose, triphenyl phosphate, dye and solvent is 20 g: 5 g: 0.005g and 300 ml.
The solvent is absolute ethyl alcohol.
The dye is methyl violet.
The preparation method of the metallographic coated test paper comprises the following steps:
adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, filtering or standing to obtain a supernatant, then flatly paving the supernatant on a bottom plate with a smooth surface, drying to form a film to obtain metallographic coated test paper, and sampling a 12Cr1MoV material on site, wherein the sampling result is shown in figure 1 a.
Before tiling, the surface of the bottom plate is cleaned by absolute ethyl alcohol, and the bottom plate is made of 12Cr1 MoV.
Example two
The metallographic coated test paper is prepared from ethyl cellulose, triphenyl phosphate, dye and solvent.
The proportions of ethylcellulose, triphenyl phosphate, dye and solvent were 25g, 15g, 0.005g and 500 mL.
The solvent is absolute ethyl alcohol.
The dye is methyl violet.
The preparation method of the metallographic coated test paper comprises the following steps:
adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, filtering or standing to obtain a supernatant, then spreading the supernatant on a bottom plate with a smooth surface, drying to form a film to obtain metallographic coated test paper, and sampling the TP347H material on site, wherein the sampling result is shown in figure 2 a.
Wherein the surface of the base plate is cleaned by absolute ethyl alcohol before tiling.
EXAMPLE III
The metallographic coated test paper is prepared from ethyl cellulose, triphenyl phosphate, dye and solvent.
The proportions of ethylcellulose, triphenyl phosphate, dye and solvent were 30g, 20g, 0.1g and 500 mL.
The solvent is absolute ethyl alcohol.
The dye is methyl violet.
The preparation method of the metallographic coated test paper comprises the following steps:
adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, filtering or standing to obtain a supernatant, then spreading the supernatant on a bottom plate with a smooth surface, drying to form a film to obtain metallographic coated test paper, and carrying out on-site sampling on a welding seam of T22 and TP347H dissimilar steel, wherein the sampling result is shown in figure 3 a.
Wherein the surface of the base plate is cleaned by absolute ethyl alcohol before tiling.
Example four
The metallographic coated test paper is prepared from ethyl cellulose, triphenyl phosphate, dye and solvent.
The proportions of ethyl cellulose, triphenyl phosphate, dye and solvent were 20g, 0.001g and 500 mL.
The solvent is absolute ethyl alcohol.
The dye is methyl violet.
The preparation method of the metallographic coated test paper comprises the following steps:
adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, filtering or standing, taking supernatant, then flatly paving on a bottom plate with a smooth surface, and then drying to form a film, thus obtaining the metallographic coated test paper.
Wherein the surface of the base plate is cleaned by absolute ethyl alcohol before tiling.
EXAMPLE five
The metallographic coated test paper is prepared from ethyl cellulose, triphenyl phosphate, dye and solvent.
The proportions of ethyl cellulose, triphenyl phosphate, dye and solvent were 80g, 0.1g and 200 mL.
The solvent is absolute ethyl alcohol.
The dye is methyl violet.
The preparation method of the metallographic coated test paper comprises the following steps:
adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, filtering or standing, taking supernatant, then flatly paving on a bottom plate with a smooth surface, and then drying to form a film, thus obtaining the metallographic coated test paper.
Wherein the surface of the base plate is cleaned by absolute ethyl alcohol before tiling.
EXAMPLE six
The metallographic coated test paper is prepared from ethyl cellulose, triphenyl phosphate, dye and solvent.
The proportions of ethylcellulose, triphenyl phosphate, dye and solvent were 50g, 10g, 0.06g and 350 mL.
The solvent is absolute ethyl alcohol.
The dye is methyl violet.
The preparation method of the metallographic coated test paper comprises the following steps:
adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, filtering or standing, taking supernatant, then flatly paving on a bottom plate with a smooth surface, and then drying to form a film, thus obtaining the metallographic coated test paper.
Wherein the surface of the base plate is cleaned by absolute ethyl alcohol before tiling.
EXAMPLE seven
The metallographic coated test paper is prepared from ethyl cellulose, triphenyl phosphate, dye and solvent.
The proportions of ethylcellulose, triphenyl phosphate, dye and solvent were 30g, 5g, 0.005g and 250 mL.
The solvent is absolute ethyl alcohol.
The dye is methyl violet.
The preparation method of the metallographic coated test paper comprises the following steps:
adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, filtering or standing, taking supernatant, then flatly paving on a bottom plate with a smooth surface, and then drying to form a film, thus obtaining the metallographic coated test paper.
Wherein the surface of the base plate is cleaned by absolute ethyl alcohol before tiling.
Example eight
The metallographic coated test paper is prepared from ethyl cellulose, triphenyl phosphate, dye and solvent.
The proportions of ethylcellulose, triphenyl phosphate, dye and solvent were 70g, 18g, 0.08g and 450 mL.
The solvent is absolute ethyl alcohol.
The dye is methyl violet.
The preparation method of the metallographic coated test paper comprises the following steps:
adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, filtering or standing, taking supernatant, then flatly paving on a bottom plate with a smooth surface, and then drying to form a film, thus obtaining the metallographic coated test paper.
Wherein the surface of the base plate is cleaned by absolute ethyl alcohol before tiling.
Claims (10)
1. The metallographic coated test paper is characterized by being prepared from ethyl cellulose, triphenyl phosphate, a dye and a solvent.
2. The metallographic coated test paper according to claim 1, wherein the ratio of ethyl cellulose, triphenyl phosphate, dye and solvent is (20-80) g, (0.1-20) g, (0.001-0.1) g and (200-500) mL.
3. The metallographic coated test paper according to claim 1, wherein the solvent is absolute ethanol.
4. The metallographic coated test paper according to claim 1, wherein the dye is methyl violet.
5. The preparation method of the metallographic coated test paper is characterized by comprising the following steps of:
and adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, and flatly spreading and drying to form a film, thereby obtaining the metallographic coated test paper.
6. The method for preparing metallographic coated test paper according to claim 5, wherein the ratio of ethyl cellulose, triphenyl phosphate, dye and solvent is (20-80) g, (0.1-20) g, (0.001-0.1) g and (200-500) mL.
7. The method for preparing metallographic coated test paper according to claim 5, wherein the solvent is absolute ethyl alcohol.
8. The preparation method of the metallographic coated test paper according to claim 5, which comprises the following steps:
adding ethyl cellulose, triphenyl phosphate and dye into a solvent, uniformly stirring and dissolving, filtering or standing, taking supernatant, then flatly paving on a bottom plate with a smooth surface, and then drying to form a film, thus obtaining the metallographic coated test paper.
9. The method for preparing metallographic coated test paper according to claim 5, wherein the surface of the base plate is cleaned with absolute ethanol before being laid flat.
10. The method for preparing metallographic coated test paper according to claim 5, wherein the dye is methyl violet.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111153195.XA CN113896953A (en) | 2021-09-29 | 2021-09-29 | Metallographic coated test paper and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111153195.XA CN113896953A (en) | 2021-09-29 | 2021-09-29 | Metallographic coated test paper and preparation method thereof |
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| CN113896953A true CN113896953A (en) | 2022-01-07 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB346040A (en) * | 1930-01-09 | 1931-04-09 | Ig Farbenindustrie Ag | Process for the manufacture of solutions, plasticized products and the like from cellulose ethers |
| JP2000206336A (en) * | 1998-12-17 | 2000-07-28 | Akzo Nobel Nv | Manufacture of optical film on triphenyl phosphate- containing cellulose triacetate substrate |
| CN103454217A (en) * | 2012-06-05 | 2013-12-18 | 上海宝冶工程技术有限公司 | Metallographic coated test paper and preparation method thereof |
| CN112268903A (en) * | 2020-10-15 | 2021-01-26 | 华能国际电力股份有限公司 | On-site metallographic coated test paper and preparation and use methods thereof |
| CN112280250A (en) * | 2020-10-30 | 2021-01-29 | 国电锅炉压力容器检验有限公司 | Metallographic replica material, preparation method and replica process thereof |
-
2021
- 2021-09-29 CN CN202111153195.XA patent/CN113896953A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB346040A (en) * | 1930-01-09 | 1931-04-09 | Ig Farbenindustrie Ag | Process for the manufacture of solutions, plasticized products and the like from cellulose ethers |
| JP2000206336A (en) * | 1998-12-17 | 2000-07-28 | Akzo Nobel Nv | Manufacture of optical film on triphenyl phosphate- containing cellulose triacetate substrate |
| CN103454217A (en) * | 2012-06-05 | 2013-12-18 | 上海宝冶工程技术有限公司 | Metallographic coated test paper and preparation method thereof |
| CN112268903A (en) * | 2020-10-15 | 2021-01-26 | 华能国际电力股份有限公司 | On-site metallographic coated test paper and preparation and use methods thereof |
| CN112280250A (en) * | 2020-10-30 | 2021-01-29 | 国电锅炉压力容器检验有限公司 | Metallographic replica material, preparation method and replica process thereof |
Non-Patent Citations (1)
| Title |
|---|
| 谢汝良: "现场金相复膜纸的制作方法与技巧", 《理化检验(物理分册)》 * |
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