CN106967981B - A kind of color method of iron-based zinc coat or zinc coat colour metallograpy - Google Patents

A kind of color method of iron-based zinc coat or zinc coat colour metallograpy Download PDF

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Publication number
CN106967981B
CN106967981B CN201710168632.2A CN201710168632A CN106967981B CN 106967981 B CN106967981 B CN 106967981B CN 201710168632 A CN201710168632 A CN 201710168632A CN 106967981 B CN106967981 B CN 106967981B
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iron
polishing
zinc coat
sample
zinc
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CN106967981A (en
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李小波
彭淀
高海云
王灿
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Xiangtan University
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Xiangtan University
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00Etching metallic material by chemical means
    • C23F1/10Etching compositions
    • C23F1/14Aqueous compositions
    • C23F1/16Acidic compositions
    • C23F1/28Acidic compositions for etching iron group metals
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating And Analyzing Materials By Characteristic Methods (AREA)
  • ing And Chemical Polishing (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention belongs to metallographic sample preparation and field of display technology, disclose the color method of a kind of iron-based zinc coat or zinc coat colour metallograpy, color method includes: polishing, polishing, pre- etch, coloring.The color method of iron-based zinc coat provided by the invention or zinc coat colour metallograpy, iron-based (infiltration) zinc coat colour metallograpy crystal boundary complete display, it is high to speculate display, can also obtain clearly microscopic structure even without polarised light and sensitive tint, can obviously differentiate different phase and its distribution;Step of the present invention is simple, reproducible, and coloring effect is good and stability is good, and the preparation of sample carries out at room temperature, and the sample prepared can save for a long time at normal temperature.

Description

A kind of color method of iron-based zinc coat or zinc coat colour metallograpy
Technical field
The invention belongs to metallographic sample preparation and field of display technology more particularly to a kind of iron-based zinc coat or zinc coat are color The color method of coloured gold phase.
Background technique
The various performances of microstructure and metal material inside metal material have it is direct and close contact, benefit Observation, which is carried out, with microscopic structure of the metallographic microscope to metal material is presently the most a kind of convenient, fast and effective mode. Metallographic refers to the physical state and chemical state of the chemical component and various composition of metal or alloy inside alloy.Pass through gold The reason of facies analysis can be assessed and be prejudged to the performance of material, while metallographic can be used for material failure and destroy Analysis.
At present metallographic field be most widely black and white metallographic, black and white metallographic speculate it is not high etc. due to more Mutually and infiltration, the distinguishing ability of coating are limited.Colour metallograpy speculates variation of the very high formation for cutting inteferometer coating to material composition Value that is very sensitive, therefore having its irreplaceable in colour metallograpy production practices.
Zinc has that good corrosion resistance, fusing point are low, are easy to coat and the features such as " sacrifice " anode electrochemical protective effect, therefore Zincizing, zincincation are to be applied to widest method in coating protection materials at present.
In conclusion problem of the existing technology is:
Zincizing at present, zinc-plated metallographic specimen mainly use 4% nitric acid alcohol to be corroded, in Display of Grain Boundary clarity Upper, phase region divides on significant degree, speculates in display and there is poor phenomenon in result precision, and colour metallograpy currently not yet Dye technology is in zincizing, zinc-plated metallographic structure successful story.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of iron-based zinc coat or zinc coat colour metallograpy Color method.
The invention is realized in this way the color method of a kind of iron-based zinc coat or zinc coat colour metallograpy, including it is following Step:
Polishing: successively polishing to iron-based zincizing or galvanizing sample using the abrasive paper for metallograph of different size, and every one dozen To ensure specimen surface scratch in the process of the sand paper of mill in one direction and be evenly distributed, and be rinsed with water completely, will try One of polishing operation is carried out down again after sample rotation;
Polishing: it by iron-based zincizing or galvanizing sample after grinding process, holds and is polished on polishing machine;
Pre- etch: by after polishing iron-based zincizing or galvanizing sample immerse in pre- etching solution 10 seconds~45 seconds, etch is completed It is rinsed, ethyl alcohol cleaning, then dried up with flowing water afterwards;
Coloring: it will be put into coloring liquid by the iron-based zincizing of pre- etch or galvanizing sample, and colour 30 seconds~60 seconds, then use Dehydrated alcohol is rinsed well and is air-dried with hair dryer.
Further, in the polishing step, successively using the abrasive paper for metallograph of 400#, 600#, 800# to iron-based zincizing or plating Zinc sample is polished;One of polishing operation is carried out down after sample is rotated by 90 ° again.
Further, in polishing step, antiscuffing paste is coated on polishing cloth before polishing and smears smooth, hand guarantor in polishing process Maintain an equal level steady and is continuously added clear water;Wherein polishing cloth is canvas, and antiscuffing paste is the diamond polishing cream that granularity is W2.5.
Further, in pre- etch step, pre- etching solution is dissolved in obtained by dehydrated alcohol by nitric acid, and volume ratio is 4 nitric acid: 96 Dehydrated alcohol.
Further, in tinting steps, the solution that coloring liquid is made of sodium molybdate, sulfamic acid, distilled water, mass ratio is 0.8g~2.3g sodium molybdate: 0.4g~1.7g sulfamic acid: 50g~130g distilled water.
Another object of the present invention is to provide a kind of colorings using above-mentioned iron-based zinc coat or zinc coat colour metallograpy The zinc-plated common carbon structural steel of method coloring.
Advantages of the present invention and good effect are as follows: the coloring of iron-based zinc coat provided by the invention or zinc coat colour metallograpy Method, iron-based (infiltration) zinc coat colour metallograpy crystal boundary complete display speculate display height, even without polarised light and sensitive tint Clearly microscopic structure can be obtained, different phase and its distribution can be obviously differentiated.Step of the present invention is simple, reproducible, coloring Effect is good and stability is good, and the preparation of sample carries out at room temperature, and the sample prepared can be protected for a long time at normal temperature It deposits.
Detailed description of the invention
Fig. 1 is the color method flow chart of iron-based zinc coat provided in an embodiment of the present invention or zinc coat colour metallograpy.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
Application principle of the invention is further described with reference to the accompanying drawing.
As shown in Figure 1, the color method of iron-based zinc coat provided in an embodiment of the present invention or zinc coat colour metallograpy, including Following steps:
S101: polishing: successively polishing to iron-based infiltration (plating) zinc sample using the abrasive paper for metallograph of 400#, 600#, 800#, To ensure sample surfaces scratch in one direction in per the process of the sand paper of polishing together and be evenly distributed, and be rinsed with water dry Only, one of polishing operation will be carried out down again after 90 ° of sample rotates;
S102: polishing: by sample, iron-based infiltration (plating) zinc sample holds and polishes on polishing machine after S101 is handled; Antiscuffing paste is coated on polishing cloth before polishing and smears smooth, hand held stationary and is continuously added clear water in polishing process;Wherein Polishing cloth is canvas, and antiscuffing paste is the diamond polishing cream that granularity is W2.5;
S103: pre- etch: iron-based infiltration (plating) the zinc sample after polishing is immersed in pre- etching solution 10~45 seconds, and etch is completed It is rinsed, ethyl alcohol cleaning, then dried up with flowing water afterwards;Pre- etching solution is dissolved in obtained by dehydrated alcohol by nitric acid, and ratio is 4 nitric acid: 96 nothings Water-ethanol;
S104: coloring: it will be put into coloring liquid by iron-based infiltration (plating) the zinc sample of pre- etch, and colour 30-60 seconds, then use Dehydrated alcohol is rinsed well and is air-dried with hair dryer, and iron-based infiltration can be clearly seen under common metallographic microscope The metallurgical structure of (plating) zinc layers;Wherein colorant solution as composed by sodium molybdate, sulfamic acid, distilled water, mass ratio For 0.8g~2.3g sodium molybdate: 0.4g~1.7g sulfamic acid: 50g~130g distilled water.
The color method of iron-based zinc coat provided by the invention or zinc coat colour metallograpy, iron-based (infiltration) zinc coat mosaic gold Phase crystal boundary complete display, speculates display height, can also obtain clearly microscopic structure even without polarised light and sensitive tint, can be bright It is aobvious to differentiate different phase and its distribution.Step of the present invention is simple, reproducible, and coloring effect is good and stability is good, the system of sample Standby to carry out at room temperature, the sample prepared can save for a long time at normal temperature.
The present invention is further described combined with specific embodiments below.
Embodiment 1:
The color method of iron-based zinc coat provided in an embodiment of the present invention or zinc coat colour metallograpy, comprising the following steps:
Polishing: successively polishing to iron-based infiltration (plating) zinc sample using the abrasive paper for metallograph of 400#, 600#, 800#, each To ensure sample surfaces scratch in the process of the sand paper of road polishing in one direction and be evenly distributed, and be rinsed with water completely, One of polishing operation will be carried out down again after 90 ° of sample rotates;
Polishing: by sample, iron-based infiltration (plating) zinc sample holds and polishes on polishing machine after grinding process;Polishing It is preceding that antiscuffing paste is coated on polishing cloth and smears smooth, hand held stationary and clear water is continuously added in polishing process;Wherein polish Cloth is canvas, and antiscuffing paste is the diamond polishing cream that granularity is W2.5;
Pre- etch: iron-based infiltration (plating) the zinc sample after polishing is immersed in pre- etching solution 10 seconds, and flowing water is used after the completion of etch It rinses, ethyl alcohol cleaning, then dries up;Pre- etching solution is dissolved in obtained by dehydrated alcohol by nitric acid, and ratio is 4 nitric acid: 96 dehydrated alcohols;
Coloring: it will be put into coloring liquid by iron-based infiltration (plating) the zinc sample of pre- etch, and colour 30 seconds, then use dehydrated alcohol It rinses well and is air-dried with hair dryer, iron-based infiltration (plating) zinc layers can be clearly seen under common metallographic microscope Metallurgical structure;Wherein colorant solution as composed by sodium molybdate, sulfamic acid, distilled water, mass ratio are 0.8g molybdic acid Sodium: 0.4g sulfamic acid: 50g distilled water.
Embodiment 2:
The color method of iron-based zinc coat provided in an embodiment of the present invention or zinc coat colour metallograpy, comprising the following steps:
Polishing: successively polishing to iron-based infiltration (plating) zinc sample using the abrasive paper for metallograph of 400#, 600#, 800#, each To ensure sample surfaces scratch in the process of the sand paper of road polishing in one direction and be evenly distributed, and be rinsed with water completely, One of polishing operation will be carried out down again after 90 ° of sample rotates;
Polishing: by sample, iron-based infiltration (plating) zinc sample holds and polishes on polishing machine after grinding process;Polishing It is preceding that antiscuffing paste is coated on polishing cloth and smears smooth, hand held stationary and clear water is continuously added in polishing process;Wherein polish Cloth is canvas, and antiscuffing paste is the diamond polishing cream that granularity is W2.5;
Pre- etch: iron-based infiltration (plating) the zinc sample after polishing is immersed in pre- etching solution 45 seconds, and flowing water is used after the completion of etch It rinses, ethyl alcohol cleaning, then dries up;Pre- etching solution is dissolved in obtained by dehydrated alcohol by nitric acid, and ratio is 4 nitric acid: 96 dehydrated alcohols;
Coloring: it will be put into coloring liquid by iron-based infiltration (plating) the zinc sample of pre- etch, and colour 60 seconds, then use dehydrated alcohol It rinses well and is air-dried with hair dryer, iron-based infiltration (plating) zinc layers can be clearly seen under common metallographic microscope Metallurgical structure;Wherein colorant solution as composed by sodium molybdate, sulfamic acid, distilled water, mass ratio are 2.3g g molybdenum Sour sodium: 1.7g sulfamic acid: 130g distilled water.
Embodiment 3:
The color method of iron-based zinc coat provided in an embodiment of the present invention or zinc coat colour metallograpy, comprising the following steps:
Polishing: successively polishing to iron-based infiltration (plating) zinc sample using the abrasive paper for metallograph of 400#, 600#, 800#, each To ensure sample surfaces scratch in the process of the sand paper of road polishing in one direction and be evenly distributed, and be rinsed with water completely, One of polishing operation will be carried out down again after 90 ° of sample rotates;
Polishing: by sample, iron-based infiltration (plating) zinc sample holds and polishes on polishing machine after grinding process;Polishing It is preceding that antiscuffing paste is coated on polishing cloth and smears smooth, hand held stationary and clear water is continuously added in polishing process;Wherein polish Cloth is canvas, and antiscuffing paste is the diamond polishing cream that granularity is W2.5;
Pre- etch: iron-based infiltration (plating) the zinc sample after polishing is immersed in pre- etching solution 30 seconds, and flowing water is used after the completion of etch It rinses, ethyl alcohol cleaning, then dries up;Pre- etching solution is dissolved in obtained by dehydrated alcohol by nitric acid, and ratio is 4 nitric acid: 96 dehydrated alcohols;
Coloring: it will be put into coloring liquid by iron-based infiltration (plating) the zinc sample of pre- etch, and colour 40 seconds, then use dehydrated alcohol It rinses well and is air-dried with hair dryer, iron-based infiltration (plating) zinc layers can be clearly seen under common metallographic microscope Metallurgical structure;Wherein colorant solution as composed by sodium molybdate, sulfamic acid, distilled water, mass ratio are 1g sodium molybdate: 1g sulfamic acid: 80g distilled water.
Embodiment 4:Q235 steel galvanizing by dipping sample was according to the pre- etch of step shown in the present invention 15 seconds, and 200 times of coloring 60 seconds Colour metallograpy, observe used in equipment be using equipment be ZEISS Primotech metallographic microscope, as a result are as follows: ζ phase is The green and pink mixture of colours;δ phase is yellow green transition region;Γ phase is blackish green;Matrix is once yellowish green indigo plant from edge to center Purplish red gradient color.
Embodiment 5:Q235 steel galvanizing by dipping sample was according to the pre- etch of step shown in the present invention 15 seconds, and 500 times of coloring 45 seconds Colour metallograpy, observe used in equipment be using equipment be ZEISS Primotech metallographic microscope, ζ phase is green;δ It is mutually red;Γ phase is yellow and black;Matrix is red.
Embodiment 6:Q235 steel galvanizing by dipping sample was according to the pre- etch of step shown in the present invention 15 seconds, and 200 times of coloring 35 seconds Colour metallograpy, observe used in equipment be using equipment be ZEISS Primotech metallographic microscope, as a result are as follows: ζ phase is It is red;δ phase is green;Γ phase is blackish green, and the crystal boundary of δ phase and Γ phase black is spaced apart;Matrix is primary from edge to center For the red gradient color of yellowish green royal purple.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (5)

1. the color method of a kind of iron-based zinc coat or zinc coat colour metallograpy, which is characterized in that the iron-based zinc coat or plating The color method of zinc layers colour metallograpy is the following steps are included: polishing: successively using the abrasive paper for metallograph of different size to iron-based zincizing Or galvanizing sample is polished, and specimen surface scratch is ensured in the process per the sand paper polished together in one direction and is divided Cloth is uniform, and is rinsed with water completely, carries out down one of polishing operation after sample is rotated again;Polishing: by iron-based zincizing or zinc-plated Sample holds and is polished on polishing machine after grinding process;Pre- etch: by after polishing iron-based zincizing or galvanizing sample It immerses in pre- etching solution 10 seconds~45 seconds, is rinsed after the completion of etch with flowing water, ethyl alcohol cleaning, then dry up;Coloring: will be by preimpregnation It loses iron-based zincizing or galvanizing sample is put into coloring liquid, colour 30 seconds~60 seconds, then rinsed well and used with dehydrated alcohol and blown Blower air-dries;The solution that coloring liquid is made of sodium molybdate, sulfamic acid, distilled water in the tinting steps, mass ratio 0.8g ~2.3g sodium molybdate: 0.4g~1.7g sulfamic acid: 50g~130g distilled water.
2. the color method of iron-based zinc coat as described in claim 1 or zinc coat colour metallograpy, which is characterized in that described to beat It grinds in step, is successively polished using the abrasive paper for metallograph of 400#, 600#, 800# iron-based zincizing or galvanizing sample;By sample One of polishing operation is carried out down after being rotated by 90 ° again.
3. the color method of iron-based zinc coat as described in claim 1 or zinc coat colour metallograpy, which is characterized in that polishing step In rapid, antiscuffing paste is coated on polishing cloth before polishing and smears smooth, hand held stationary and is continuously added clear water in polishing process; Wherein polishing cloth is canvas, and antiscuffing paste is the diamond polishing cream that granularity is W2.5.
4. the color method of iron-based zinc coat as described in claim 1 or zinc coat colour metallograpy, which is characterized in that pre- etch In step, pre- etching solution is dissolved in obtained by dehydrated alcohol by nitric acid, and volume ratio is 4 nitric acid: 96 dehydrated alcohols.
5. a kind of utilize the zinc-plated common of the coloring of the color method of iron-based zinc coat or zinc coat colour metallograpy described in claim 1 Structural carbon steel.
CN201710168632.2A 2017-03-21 2017-03-21 A kind of color method of iron-based zinc coat or zinc coat colour metallograpy Expired - Fee Related CN106967981B (en)

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TWI480538B (en) * 2013-05-21 2015-04-11 China Steel Corp Method of optically determining metallography of iron-zinc galvannealed intermetallic layer
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