CN104458745A - Method for displaying color metallographic structure of 6009 aluminum alloy welded joint - Google Patents

Method for displaying color metallographic structure of 6009 aluminum alloy welded joint Download PDF

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CN104458745A
CN104458745A CN201410770479.7A CN201410770479A CN104458745A CN 104458745 A CN104458745 A CN 104458745A CN 201410770479 A CN201410770479 A CN 201410770479A CN 104458745 A CN104458745 A CN 104458745A
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sample
acid
polishing
ethyl alcohol
absolute ethyl
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CN201410770479.7A
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张德芬
陈孝文
杨阳
王同举
谭盖
李曾珍
朱亚
李仁仆
王松
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Southwest Petroleum University
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Southwest Petroleum University
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Abstract

The invention provides a method for displaying the color metallographic structure of a 6009 aluminum alloy welded joint, belonging to the technical field of preparation of metallographic samples. The method comprises the following steps: grinding a sample by respectively using 800-mesh, 1000-mesh, 1500-mesh and 3000-mesh waterproof abrasive paper; then, carrying out electrolytic polishing: namely putting the sample into an electrolytic polishing liquid, carrying out electrolytic polishing under the effect that the voltage is 12-15V and the current is 1.0-1.3A, wherein the polishing liquid is prepared from perchloric acid and absolute ethyl alcohol (the volume ratio of perchloric acid to absolute ethyl alcohol is 1: 3); and finally, carrying out anode laminating treatment, wherein an anode laminating liquid is prepared from sulfuric acid, phosphoric acid and distilled water (the volume ratio of sulfuric acid, phosphoric acid to distilled water is 38: 43: 19), the laminating current is 0.3-0.6A and the laminating time is 60-70 seconds; and then, washing and airing. A clear color metallographic structure can be observed by using a polarizing microscope and the grain boundary is intact and clear. The grain boundary is intact and clear, the contrast display is high, the coloring effect is good and the operation is simple.

Description

A kind of display packing of 6009 welded joints in aluminium alloy metallurgical structures
Technical field
The invention belongs to metallographic and detect analysis technical field, especially design a kind of display packing of 6009 welded joints in aluminium alloy metallurgical structures.
Background technology
The performance such as intensity, hardness of metal material and its internal organizational structure have direct and close contacting, and metallographic observation is then research metal material internal organizational structure is the most also method the most general.Metallographic refers to that the chemical composition of metal is in the chemical state of metal inside and physical state.By metallographic examination, can predict and judge metallicity, analyzing the reason losing efficacy and destroyed.
Color Metallographic Technology is the one in metallographic examination technology, it utilizes chemistry or physical method to form a layer thickness interference thin film not etc. in metal surface, the wavelength that the inteferometer coating of different-thickness reflects under the interference effect of light is different, present the complementary color of wavelength relevant separately, thus make the different parts of metal demonstrate different colours.
6009 aluminium alloys possess high corrosion stability and weldability, excellent manufacturability because of it, and are widely used in the industry such as automobile, door and window.Inevitable, increasingly extensive to the research of the weld strength of 6009 aluminium alloys, and metallographic examination technology, be the means commonly used the most.
Table 1 is the main chemical compositions of the present invention's 6009 aluminium alloys used and welding wire ER5356 thereof.What adopt is Laser-MIG Composite Welding method.Welding current 200A, weldingvoltage is 24.5V, speed of welding 900mm/min, laser power 3.8KW, wire feed rate 12m/min, and blanket gas adopts pure argon.Welding joint generally includes three parts: weld metal zone, fusion area, heat-affected zone.
Main chemical compositions (massfraction) % of table 16009 aluminium alloy and ER5356 welding wire
Table.1chemical composition of 6009 aluminum alloys and ER5356 welding wire(mass)%
6009 aluminium alloys are softer, when preparing metallographic specimen, and comparatively easy grinding, under standard machinery polishing means, surface very easily scratches, and is difficult to throw desirable degree, and after this brightless sample etches, the crystal boundary of microstructure can be caused to be difficult to display, even can not differentiate crystal boundary.So far also not with acid mixture very successful erode away the case that 6009 welded joints in aluminium alloys organize crystal boundary.Like this with regard to bringing difficulty to our research, also affect the use of 6009 aluminium alloys to a certain extent.Therefore, how preparing the 6009 welded joints in aluminium alloy colour metallograpy samples meeting the requirement of colour metallograpy Analysis on Microstructure is problem demanding prompt solutions.
Summary of the invention
For prior art above shortcomings, the problem to be solved in the present invention is to provide a kind of crystal boundary complete display, contrast display is high, the preparation method of the 6009 welded joints in aluminium alloy colour metallograpies that test result accuracy is high.
The technical scheme that patent of the present invention addresses this problem is:
A preparation method for display 6009 welded joints in aluminium alloy metallurgical structures, is characterized in that concrete steps are as follows:
A. polish: use 800 orders, 1000 orders, 1500 orders successively, 3000 object waterproof abrasive papers polish to sample, in each procedure, sample surfaces is ground to cut only towards a direction and the degree be evenly distributed, and rinse well with clear water, by rotary sample 90 °, then enter down operation of polishing together.
B. electropolishing: the aluminum alloy sample after step a process is put into electrolytic polishing liquid, under the function of current of the voltage of 12 ~ 15V, 1.0 ~ 1.3A, electropolishing 12 ~ 15 seconds, swing sample slight every 3 seconds during polishing, polishing terminates rear absolute ethyl alcohol and rinses well and dry up with cold wind; The ratio that wherein electrolytic polishing liquid is 1:3 by perchloric acid and absolute ethyl alcohol by volume mixes; The mass concentration of described perchloric acid is 70% ~ 72%.
C. anode overlay film: the aluminum alloy sample after step b process is put into anode overlay film liquid, under the electric current of 0.3 ~ 0.6A, anode overlay film 60 ~ 70 seconds, then rinse well with absolute ethyl alcohol and dry up with cold wind, under polarizing microscope, just can see 6009 welded joints in aluminium alloy metallurgical structures clearly; The ratio that its Anodic overlay film liquid is 38:43:19 by sulfuric acid, phosphoric acid and distilled water by volume mixes; Described h 2 so 4 concentration is 93.0% ~ 98.0%, Lin Suan Nong Du≤85.0%.
Preferably, the corase grind of described sample uses pre-mill or direct hand mill.
Preferably, described waterproof abrasive paper is for being silicon carbide material.
Owing to adopting technical scheme as above, the advantage that the present invention has is: the metallurgical structure of 6009 welded joints in aluminium alloys can clearly display by (1), under polarized light microscope observing, the size of crystal grain, form and distribution are clear can distinguish, is very beneficial for the statistics of grain size; (2) consuming time few, reappearance is good, and coloring effect is good, and labour intensity is low; (3) colour metallograpy of 6009 aluminium alloys and other six line aluminium alloys can be prepared easily; (4) easy and simple to handle, electrolytic polishing liquid, anode overlay film liquid composition are easy to obtain, and prepare easy; (5) without the need to heating, can carry out under normal temperature.
Accompanying drawing explanation
The non-limiting example that the present invention can be provided by accompanying drawing further illustrates.
Fig. 1 is that the metallurgical structure picture obtained is taken in 6009 welded joints in aluminium alloy weld metal zones after the step in embodiment under polarizing microscope;
Fig. 2 is that the metallurgical structure picture obtained is taken in 6009 welded joints in aluminium alloy fusion areas after the step in embodiment under polarizing microscope;
Fig. 3 is that the metallurgical structure picture obtained is taken in 6009 welded joints in aluminium alloy heat-affected zones after the step in embodiment under polarizing microscope.
Embodiment
Below in conjunction with accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described.
Embodiment:
During concrete enforcement, the vertical direction of 6009 welded joints in aluminium alloys along weld seam is cut, gets the sample being of a size of 6 × 40 × 30mm, prepare colour metallograpy according to following steps:
A. carry out grinding process to sample, described grinding process specifically comprises: with water be wetting agent by sample wetness, then polish.Use 800 orders, 1000 orders, 1500 orders successively, 3000 object liquid honings need to observe the surface of metallographic, the time of each polishing can be generally 1 ~ 5 minute, can obtain roughly smooth like this and not have the flour milling of excessive cut.When polishing, waterproof abrasive paper is placed on pre-mill, by its driven rotary, the rotating speed of pre-mill can be 250 ~ 500r/min, constantly have above pre-mill under current to play effect that is wetting and cooling sand paper, make the surface of metallographic to be seen towards sand paper, and keep surface and sand paper uniform contact, pin sample and polish on sand paper.By described rotary sample 90 ° after each replacing sand paper, until the cut of a upper procedure grinds off completely, make that new cut direction is consistent, size is even, need before changing sand paper with water, sample and new sand paper to be cleaned up, to remove sand grains at every turn.With clear water, sample surfaces is cleaned up after polishing, and spray alcohol and dry up.
B. electropolishing: the aluminum alloy sample after coarse grinding treatment is put into electrolytic polishing liquid, under the function of current of the voltage of 12 ~ 15V, 1.0 ~ 1.3A, electropolishing 12 ~ 15 seconds, swing sample slight every 3 seconds during polishing, polishing terminates rear absolute ethyl alcohol and rinses well and dry up; The ratio that wherein electrolytic polishing liquid is 1:3 by perchloric acid and absolute ethyl alcohol by volume mixes; Described perchloric acid preferred mass concentration is the perchloric acid of 70% ~ 72%; The formulation example of described polishing fluid is as follows:
With graduated cylinder measure 10ml mass concentration be 72% perchloric acid pour in large beaker, then the absolute ethyl alcohol adding 30ml in beaker dilutes perchloric acid, stirs about 5min, solution is mixed with glass bar.
C. anode overlay film: the aluminum alloy sample after step b process is put into anode overlay film liquid, under the electric current of 0.3 ~ 0.6A, anode overlay film 60 ~ 70 seconds, then rinses well with absolute ethyl alcohol and dries up with cold wind; The ratio that its Anodic overlay film liquid is 38:43:19 by sulfuric acid, phosphoric acid and distilled water by volume mixes; Described sulfuric acid preferred mass concentration is the concentrated sulphuric acid of 93.0% ~ 98.0%, the strong phosphoric acid of phosphoric acid preferred mass Nong Du≤85.0%; Described anode overlay film liquid configuration is as follows:
The distilled water measuring 19ml with graduated cylinder is poured in large beaker, again with graduated cylinder measure 43ml mass concentration be 85% phosphoric acid be slowly poured in beaker, finally, with graduated cylinder measure 38ml mass concentration be 98% the concentrated sulphuric acid pour in beaker along wall of cup, and stir with glass bar, solution is mixed.
Sample through above-mentioned process just can be seen 6009 welded joints in aluminium alloy metallurgical structures clearly under polarizing microscope, as shown in Figure 1, Figure 2, Figure 3 shows.
Obviously, all embodiments of foregoing description are a part of embodiments of the present invention, instead of whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art are not making other embodiments all obtained under creative work prerequisite, all belong to the category of the present invention's protection.

Claims (3)

1. a display packing for 6009 welded joints in aluminium alloy metallurgical structures, is characterized in that the concrete implementation step of the method is as follows:
A. polish: use 800 orders, 1000 orders, 1500 orders successively, 3000 object waterproof abrasive papers polish to sample, in each procedure, guarantee that sample surfaces cut is only uniformly distributed towards a direction, and rinse well with clear water, by rotary sample 90 °, then enter down operation of polishing together;
B. electropolishing: the aluminum alloy sample after step a process is put into electrolytic polishing liquid, under the function of current of the voltage of 12 ~ 15V, 1.0 ~ 1.3A, electropolishing 12 ~ 15 seconds, swing sample slight every 3 seconds during polishing, polishing terminates rear absolute ethyl alcohol and rinses well and dry up with cold wind; The ratio mixed preparing that wherein electrolytic polishing liquid is 1:3 by perchloric acid and absolute ethyl alcohol by volume forms; Described perchloric acid preferred mass concentration is the perchloric acid of 70% ~ 72%;
C. anode overlay film: the aluminum alloy sample after step b process is put into anode overlay film liquid, under the function of current of 0.3 ~ 0.6A, anode overlay film 60 ~ 70 seconds, then rinse well with absolute ethyl alcohol and blow with cold air drying, under polarizing microscope, just can see 6009 welded joints in aluminium alloy metallurgical structures clearly; The ratio that its Anodic overlay film liquid is 38:43:19 by sulfuric acid, phosphoric acid and distilled water by volume mixes; Described sulfuric acid preferred mass concentration is the concentrated sulphuric acid of 95.0% ~ 98.0%, the strong phosphoric acid of phosphoric acid preferred mass Nong Du≤85.0%.
2. the display packing of a kind of 6009 welded joints in aluminium alloy metallurgical structures according to claims 1, is characterized in that the polishing of described sample uses pre-mill or direct hand mill.
3. the display packing of a kind of 6009 welded joints in aluminium alloy metallurgical structures according to claims 1, is characterized in that described waterproof abrasive paper is silicon carbide material.
CN201410770479.7A 2014-12-15 2014-12-15 Method for displaying color metallographic structure of 6009 aluminum alloy welded joint Pending CN104458745A (en)

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CN106757299A (en) * 2016-12-15 2017-05-31 上海电气核电设备有限公司 The electrobrightening corrosive agent and its application method of a kind of nickel-base alloy metallographic structure
CN110208264A (en) * 2019-06-17 2019-09-06 新疆众和股份有限公司 A kind of method for making sample of high-purity aluminium busbar metallographic sample
CN110835778A (en) * 2019-11-21 2020-02-25 哈尔滨工业大学 Aluminum alloy electrolytic polishing solution and electrolytic polishing method
CN111024697A (en) * 2019-12-18 2020-04-17 新疆众和股份有限公司 Preparation method of 6061 aluminum alloy metallographic specimen
CN113607749A (en) * 2021-08-02 2021-11-05 浙江永杰铝业有限公司 Rapid detection method for material line after oxidation of aluminum alloy
CN115407046A (en) * 2022-08-05 2022-11-29 西南石油大学 Comprehensive grindability characterization method based on rock microscopic structure and equivalent quartz content

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CN110835778B (en) * 2019-11-21 2021-12-31 哈尔滨工业大学 Aluminum alloy electrolytic polishing solution and electrolytic polishing method
CN111024697A (en) * 2019-12-18 2020-04-17 新疆众和股份有限公司 Preparation method of 6061 aluminum alloy metallographic specimen
CN113607749A (en) * 2021-08-02 2021-11-05 浙江永杰铝业有限公司 Rapid detection method for material line after oxidation of aluminum alloy
CN115407046A (en) * 2022-08-05 2022-11-29 西南石油大学 Comprehensive grindability characterization method based on rock microscopic structure and equivalent quartz content
CN115407046B (en) * 2022-08-05 2024-04-16 西南石油大学 Comprehensive abrasiveness characterization method based on rock microstructure and equivalent quartz content

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