CN106967981A - 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
CN106967981A
CN106967981A CN201710168632.2A CN201710168632A CN106967981A CN 106967981 A CN106967981 A CN 106967981A CN 201710168632 A CN201710168632 A CN 201710168632A CN 106967981 A CN106967981 A CN 106967981A
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iron
polishing
zinc coat
sample
color method
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CN106967981B (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

Prepared the invention belongs to metallographic sample and display technology field, 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.Iron-based zinc coat or the color method of zinc coat colour metallograpy that the present invention is provided, iron-based (oozes) zinc coat colour metallograpy crystal boundary complete display, speculate display high, clearly microscopic structure can be also obtained even without polarised light and sensitive tint, can substantially differentiate different phase and its distribution;Step of the present invention is simple, and reproducible, coloring effect is good and stability is good, and the preparation of sample is carried out at room temperature, and the sample prepared can be preserved for a long time at normal temperatures.

Description

A kind of color method of iron-based zinc coat or zinc coat colour metallograpy
Technical field
Prepared the invention belongs to metallographic sample and display technology field, more particularly to a kind of iron-based zinc coat or zinc coat coloured silk The color method of coloured gold phase.
Background technology
The various performances of microstructure and metal material inside metal material have it is direct and close contact, profit A kind of mode that observation is presently the most convenient, fast and effective is carried out to the microscopic structure of metal material with metallographic microscope. Metallographic refers to the physical state and chemical state of the chemical composition and various composition of metal or alloy inside alloy.Pass through gold Facies analysis, can be estimated and anticipation to the performance of material, while metallographic can be used for the reason for material failure and destruction Analysis.
Use to be most widely black and white metallographic in metallographic field at present, black and white metallographic is due to speculating the reason such as not high to many Mutually and ooze, the distinguishing ability of coating it is limited.Colour metallograpy speculates change of the very high formation for cutting inteferometer coating to material composition It is very sensitive, therefore have its irreplaceable value in colour metallograpy production practices.
Zinc has that good corrosion resistance, fusing point are low, is easy to the features such as coating and " sacrifice " anode electrochemical protective effect, therefore Zincizing, zincincation are to be applied to widest method in coating protection materials at present.
In summary, the problem of prior art is present be:
Current zincizing, zinc-plated metallographic specimen are mainly corroded using 4% nitric acid alcohol, in Display of Grain Boundary definition On upper, phase region point significant degree, speculate that display is upper and result precision on there is poor phenomenon, and currently there are no colour metallograpy Dye technology is in zincizing, zinc-plated metallographic structure successful story.
The content of the invention
The problem of existing for prior art, the invention provides a kind of iron-based zinc coat or zinc coat colour metallograpy Color method.
The present invention is achieved in that the color method of a kind of iron-based zinc coat or zinc coat colour metallograpy, including following Step:
Polishing:Iron-based zincizing or galvanizing sample are polished using the abrasive paper for metallograph of different size successively, every one dozen Specimen surface cut is ensured in the process of the sand paper of mill in one direction and is evenly distributed, and is rinsed well with water, will be tried One of polishing operation is carried out down again after sample rotation;
Polishing:It is hand-held to be polished on polishing machine by iron-based zincizing or galvanizing sample after grinding process;
Pre- etch:Iron-based zincizing after polishing or galvanizing sample are immersed in pre- etching solution 10 seconds~45 seconds, etch is completed Rinsed, ethanol cleaning, then dried up with flowing water afterwards;
Coloring:It will be put into by pre- etch iron-based zincizing or galvanizing sample in coloring liquid, coloring 30 seconds~60 seconds, Ran Houyong Absolute ethyl alcohol is rinsed well and air-dried with hair-dryer.
Further, in the polishing step, successively using 400#, 600#, 800# abrasive paper for metallograph 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 and smears smooth before polishing, hand is protected in polishing process Maintain an equal level steady and be 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 absolute ethyl alcohol by nitric acid, and volume ratio is 4 nitric acid:96 Absolute ethyl alcohol.
Further, in tinting steps, the solution that coloring liquid is made up of sodium molybdate, sulfamic acid, distilled water, mass ratio is 0.8g~2.3g sodium molybdates:0.4g~1.7g sulfamic acids:50g~130g distilled water.
Another object of the present invention is to provide a kind of coloring using above-mentioned iron-based zinc coat or zinc coat colour metallograpy The zinc-plated carbon structural steel of method coloring.
Advantages of the present invention and good effect are:Iron-based zinc coat or the coloring of zinc coat colour metallograpy that the present invention is provided Method, iron-based (oozes) zinc coat colour metallograpy crystal boundary complete display, display height is speculated, even without polarised light and sensitive tint Clearly microscopic structure can be obtained, different phase and its distribution can be substantially differentiated.Step of the present invention is simple, reproducible, coloring Effect is good and stability is good, and the preparation of sample is carried out at room temperature, and the sample prepared can be protected for a long time at normal temperatures Deposit.
Brief description of the drawings
Fig. 1 is iron-based zinc coat provided in an embodiment of the present invention or the color method flow chart of zinc coat colour metallograpy.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be 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.
The application principle of the present invention is further described below in conjunction with the accompanying drawings.
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:(plating) zinc sample is oozed to iron-based using 400#, 600#, 800# abrasive paper for metallograph successively to polish, To ensure sample surfaces cut in one direction in per the process of the sand paper of polishing together and be evenly distributed, and rinse dry with water Only, one of polishing operation will be carried out down again after 90 ° of rotary sample;
S102:Polishing:By sample, iron-based oozes that (plating) zinc sample is hand-held to be polished on polishing machine after S101 is handled; Antiscuffing paste is coated on polishing cloth and smears smooth before polishing, hand held stationary and clear water is continuously added 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 after polishing is oozed into (plating) zinc sample to immerse in pre- etching solution 10~45 seconds, etch is completed Rinsed, ethanol cleaning, then dried up with flowing water afterwards;Pre- etching solution is dissolved in obtained by absolute ethyl alcohol by nitric acid, and ratio is 4 nitric acid:96 nothings Water-ethanol;
S104:Coloring:(plating) zinc sample will be oozed by pre- etch iron-based to be put into coloring liquid, colour 30-60 seconds, Ran Houyong Absolute ethyl alcohol is rinsed well and air-dried with hair-dryer, is just clear that iron-based oozes under common metallographic microscope The metallurgical structure of (plating) zinc layers;The solution that wherein colouring agent is made up of sodium molybdate, sulfamic acid, distilled water, mass ratio For 0.8g~2.3g sodium molybdates:0.4g~1.7g sulfamic acids:50g~130g distilled water.
Iron-based zinc coat or the color method of zinc coat colour metallograpy that the present invention is provided, iron-based (ooze) zinc coat mosaic gold Phase crystal boundary complete display, speculates display height, clearly microscopic structure can be also obtained even without polarised light and sensitive tint, can be bright The different phase of aobvious resolution and its distribution.Step of the present invention is simple, and reproducible, coloring effect is good and stability is good, the system of sample Standby to carry out at room temperature, the sample prepared can be preserved for a long time at normal temperatures.
The present invention is further described with reference to specific embodiment.
Embodiment 1:
The color method of iron-based zinc coat provided in an embodiment of the present invention or zinc coat colour metallograpy, comprises the following steps:
Polishing:(plating) zinc sample is oozed to iron-based using 400#, 600#, 800# abrasive paper for metallograph successively to polish, it is each Sample surfaces cut is ensured in the process of the sand paper of road polishing in one direction and is evenly distributed, and is rinsed well with water, One of polishing operation will be carried out down again after 90 ° of rotary sample;
Polishing:By sample, iron-based oozes that (plating) zinc sample is hand-held to be polished 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 it is continuously added clear water 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 after polishing is oozed into (plating) zinc sample to immerse in pre- etching solution 10 seconds, flowing water is used after the completion of etch Rinse, ethanol cleaning, then dry up;Pre- etching solution is dissolved in obtained by absolute ethyl alcohol by nitric acid, and ratio is 4 nitric acid:96 absolute ethyl alcohols;
Coloring:(plating) zinc sample will be oozed by pre- etch iron-based to be put into coloring liquid, colour 30 seconds, then use absolute ethyl alcohol Rinse well and air-dried with hair-dryer, be just clear that iron-based oozes (plating) zinc layers under common metallographic microscope Metallurgical structure;The solution that wherein colouring agent is made up of sodium molybdate, sulfamic acid, distilled water, mass ratio is 0.8g molybdic acids Sodium:0.4g sulfamic acids: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, comprises the following steps:
Polishing:(plating) zinc sample is oozed to iron-based using 400#, 600#, 800# abrasive paper for metallograph successively to polish, it is each Sample surfaces cut is ensured in the process of the sand paper of road polishing in one direction and is evenly distributed, and is rinsed well with water, One of polishing operation will be carried out down again after 90 ° of rotary sample;
Polishing:By sample, iron-based oozes that (plating) zinc sample is hand-held to be polished 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 it is continuously added clear water 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 after polishing is oozed into (plating) zinc sample to immerse in pre- etching solution 45 seconds, flowing water is used after the completion of etch Rinse, ethanol cleaning, then dry up;Pre- etching solution is dissolved in obtained by absolute ethyl alcohol by nitric acid, and ratio is 4 nitric acid:96 absolute ethyl alcohols;
Coloring:(plating) zinc sample will be oozed by pre- etch iron-based to be put into coloring liquid, colour 60 seconds, then use absolute ethyl alcohol Rinse well and air-dried with hair-dryer, be just clear that iron-based oozes (plating) zinc layers under common metallographic microscope Metallurgical structure;The solution that wherein colouring agent is made up of sodium molybdate, sulfamic acid, distilled water, mass ratio is 2.3g g molybdenums 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, comprises the following steps:
Polishing:(plating) zinc sample is oozed to iron-based using 400#, 600#, 800# abrasive paper for metallograph successively to polish, it is each Sample surfaces cut is ensured in the process of the sand paper of road polishing in one direction and is evenly distributed, and is rinsed well with water, One of polishing operation will be carried out down again after 90 ° of rotary sample;
Polishing:By sample, iron-based oozes that (plating) zinc sample is hand-held to be polished 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 it is continuously added clear water 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 after polishing is oozed into (plating) zinc sample to immerse in pre- etching solution 30 seconds, flowing water is used after the completion of etch Rinse, ethanol cleaning, then dry up;Pre- etching solution is dissolved in obtained by absolute ethyl alcohol by nitric acid, and ratio is 4 nitric acid:96 absolute ethyl alcohols;
Coloring:(plating) zinc sample will be oozed by pre- etch iron-based to be put into coloring liquid, colour 40 seconds, then use absolute ethyl alcohol Rinse well and air-dried with hair-dryer, be just clear that iron-based oozes (plating) zinc layers under common metallographic microscope Metallurgical structure;The solution that wherein colouring agent is made up of sodium molybdate, sulfamic acid, distilled water, mass ratio is 1g sodium molybdates: 1g sulfamic acids:80g distilled water.
Embodiment 4:Q235 steel galvanizing by dipping samples were according to the pre- etch of step shown in the present invention 15 seconds, 200 times of coloring 60 seconds Colour metallograpy, observation used in equipment be that the equipment used is ZEISS Primotech metallographic microscopes, as a result for:ζ phases are The green and pink mixture of colours;δ phases are yellow green transition region;Γ phases are blackish green;Matrix is once yellowish green indigo plant from edge to center Purplish red gradient color.
Embodiment 5:Q235 steel galvanizing by dipping samples were according to the pre- etch of step shown in the present invention 15 seconds, 500 times of coloring 45 seconds Colour metallograpy, equipment used in observation is that the equipment used is ZEISS Primotech metallographic microscopes, and ζ phases are green;δ It is mutually red;Γ phases are yellow and black;Matrix is red.
Embodiment 6:Q235 steel galvanizing by dipping samples were according to the pre- etch of step shown in the present invention 15 seconds, 200 times of coloring 35 seconds Colour metallograpy, observation used in equipment be that the equipment used is ZEISS Primotech metallographic microscopes, as a result for:ζ phases are It is red;δ phases are green;Γ phases are blackish green, and the crystal boundary of δ phases and Γ phases black is spaced apart;Matrix from edge to center once 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 essences in the present invention Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.

Claims (6)

1. the color method of a kind of iron-based zinc coat or zinc coat colour metallograpy, it is characterised in that the iron-based zinc coat or plating The color method of zinc layers colour metallograpy comprises the following steps:
Polishing:Iron-based zincizing or galvanizing sample are polished using the abrasive paper for metallograph of different size successively, per polishing together Specimen surface cut is ensured in the process of sand paper in one direction and is evenly distributed, and is rinsed well with water, sample is revolved One of polishing operation is carried out down again after turning;
Polishing:It is hand-held to be polished on polishing machine by iron-based zincizing or galvanizing sample after grinding process;
Pre- etch:Iron-based zincizing after polishing or galvanizing sample are immersed in pre- etching solution 10 seconds~45 seconds, used after the completion of etch Flowing water is rinsed, ethanol cleaning, then is dried up;
Coloring:It will be put into coloring liquid, colour 30 seconds~60 seconds, then with anhydrous by pre- etch iron-based zincizing or galvanizing sample Alcohol flushing is clean and is air-dried with hair-dryer.
2. the color method of iron-based zinc coat as claimed in claim 1 or zinc coat colour metallograpy, it is characterised in that described to beat Grind in step, iron-based zincizing or galvanizing sample are polished using 400#, 600#, 800# abrasive paper for metallograph successively;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 claimed in claim 1 or zinc coat colour metallograpy, it is characterised in that polishing step In rapid, antiscuffing paste is coated on polishing cloth and smears smooth before polishing, hand held stationary and clear water is continuously added 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 claimed in claim 1 or zinc coat colour metallograpy, it is characterised in that pre- etch In step, pre- etching solution is dissolved in obtained by absolute ethyl alcohol by nitric acid, and volume ratio is 4 nitric acid:96 absolute ethyl alcohols.
5. the color method of iron-based zinc coat as claimed in claim 1 or zinc coat colour metallograpy, it is characterised in that coloring step In rapid, the solution that coloring liquid is made up of sodium molybdate, sulfamic acid, distilled water, mass ratio is 0.8g~2.3g sodium molybdates:0.4g~ 1.7g sulfamic acid:50g~130g distilled water.
6. the color method coloring of iron-based zinc coat or zinc coat colour metallograpy described in a kind of utilization claim 1 is zinc-plated common Carbon structural steels.
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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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107703032A (en) * 2017-09-29 2018-02-16 成都旭光电子股份有限公司 The anti-silver-based solder accessibility method of inspection of mixed powder copper chromium contact

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1525167A (en) * 2003-02-27 2004-09-01 宝山钢铁股份有限公司 Alloying hot galvanizing plating coat analysis method
CN101144158A (en) * 2006-09-15 2008-03-19 周婉秋 Hot dipping galvanized steel sheet molybdate/phosphate composite system chromium-free deactivation method
CN103439169A (en) * 2013-07-30 2013-12-11 国家电网公司 On-site high magnification inspection method applicable to tower material tissue
CN103471897A (en) * 2013-09-09 2013-12-25 河北科技大学 Color metallography coloring method of aluminum alloy
TW201445130A (en) * 2013-05-21 2014-12-01 China Steel Corp Method of optically determining metallography of iron-zinc galvannealed intermetallic layer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1525167A (en) * 2003-02-27 2004-09-01 宝山钢铁股份有限公司 Alloying hot galvanizing plating coat analysis method
CN101144158A (en) * 2006-09-15 2008-03-19 周婉秋 Hot dipping galvanized steel sheet molybdate/phosphate composite system chromium-free deactivation method
TW201445130A (en) * 2013-05-21 2014-12-01 China Steel Corp Method of optically determining metallography of iron-zinc galvannealed intermetallic layer
CN103439169A (en) * 2013-07-30 2013-12-11 国家电网公司 On-site high magnification inspection method applicable to tower material tissue
CN103471897A (en) * 2013-09-09 2013-12-25 河北科技大学 Color metallography coloring method of aluminum alloy

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107703032A (en) * 2017-09-29 2018-02-16 成都旭光电子股份有限公司 The anti-silver-based solder accessibility method of inspection of mixed powder copper chromium contact

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