WO2016058506A1 - 一种变形铝合金焊接接头彩色金相着色方法 - Google Patents

一种变形铝合金焊接接头彩色金相着色方法 Download PDF

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WO2016058506A1
WO2016058506A1 PCT/CN2015/091748 CN2015091748W WO2016058506A1 WO 2016058506 A1 WO2016058506 A1 WO 2016058506A1 CN 2015091748 W CN2015091748 W CN 2015091748W WO 2016058506 A1 WO2016058506 A1 WO 2016058506A1
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solution
etching solution
mol
deionized water
acid
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PCT/CN2015/091748
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English (en)
French (fr)
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路浩
邢立伟
韩德成
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南车青岛四方机车车辆股份有限公司
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Priority to GB1703358.0A priority Critical patent/GB2551868B/en
Priority to US15/509,081 priority patent/US20170276577A1/en
Publication of WO2016058506A1 publication Critical patent/WO2016058506A1/zh

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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
    • G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23F—NON-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
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/20—Acidic compositions for etching aluminium or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23F—NON-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
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/32—Alkaline compositions
    • C23F1/36—Alkaline compositions for etching aluminium or alloys thereof
    • 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
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/255—Details, e.g. use of specially adapted sources, lighting or optical systems

Definitions

  • the invention belongs to the technical field of metal material plating, and in particular relates to a color metallization coloring method for a deformed aluminum alloy welded joint.
  • microstructure of materials such as electronic scanning electron microscopy, electron fluoroscopy, electron probe, X-ray inspection and high-magnification metallography, which can be used to detect the microstructure of materials, but each device and method of use.
  • the detection parameters are each focused. It is very common and effective to observe the microstructure of aluminum alloy, especially the metamorphism effect, by high-magnification metallurgical microscope. Engineers can predict and judge the performance of metal by observing and analyzing high-power imaging, and analyze various failures and damages. The reason for this detection analysis process is often called metallographic analysis.
  • the color metallographic technique is one of the metallographic analysis techniques.
  • Aluminum alloy has low density, high strength, good formability and weldability, and has been widely used in aviation, high-speed trains and automobiles, and its industrial use is second only to steel.
  • the aluminum alloy is relatively soft and the metallographic preparation is difficult.
  • the composition of the weldment and the welding wire of the deformed aluminum alloy welded joint is different.
  • the deformed aluminum alloy weldment also called the base metal, is mostly in a rolled state, and its structure and shape are formed by processes such as stamping, bending, rolling and extrusion. Varying aluminum alloy; the weld is an as-cast aluminum alloy. Because the composition of the base metal and the weld at the welded joint of the deformed aluminum alloy is different, the corrosion resistance of the base metal and the weld to the etching solution is not with.
  • the pre-corrosion method of the prior art is used to treat the deformed aluminum alloy welded joint, and the problem of uneven corrosion of the base metal and the weld seam occurs, and the prepared color metallographic photograph is not clear, resulting in inaccurate analysis and test results.
  • Patent CN103471897A discloses a method for coloring metallographic color of aluminum alloy, comprising the following steps: (1) pre-etching: immersing the polished aluminum alloy metallographic sample in the etching solution for 1-10 minutes, after etching is completed Rinse water, wash with ethanol, and then blow dry; the etch solution is a solution obtained by dissolving potassium chloride or sodium chloride in phosphoric acid, or a solution prepared by etching solution of phosphoric acid, nitric acid and water; (2) coloring.
  • the method has simple steps, good coloring effect, and clear crystal structure can be obtained, and a clear microstructure can be obtained even without observation of polarized light and sensitive color tone.
  • the color metallographic weld of the welded joint of the deformed aluminum alloy sample obtained by the method is severely corroded, and the grain structure of the melted portion is not observed in the prepared photograph.
  • the object of the present invention is to provide a color metallization coloring method for a deformed aluminum alloy welded joint, which has high success rate, high repeatability and low cost, and the color metallographic phase of the deformed aluminum alloy welded joint processed by the method is It has the advantages of high contrast display, clear grain boundary and high accuracy of test results.
  • the technical proposal of the present invention is: a color metallization coloring method for a deformed aluminum alloy welded joint, comprising pre-corrosion and coloring, wherein the pre-corrosion comprises an acid etching treatment step of heating the acid etching solution to After 55-65 ° C, the solution was dropped on the surface of the test piece for 50-60 s, rinsed with a large amount of deionized water, and dried by hot air.
  • the acid etching solution contained Cl - 0.3-0.5 mol/L; H + 1.4-1.8 mol. /L; PO 4 3- 0.3-0.5 mol / L aqueous solution;
  • the coloring is to completely immerse the pre-etched test piece in the Weck reagent for 5-10 s. After the surface is colored, it is rinsed with a large amount of deionized water, and the hot air is dried.
  • the components of the weldment and the welding wire are different.
  • the weldments are mostly in the as-rolled state, and the welds are as-cast, resulting in different corrosion resistance to acid.
  • the corrosion resistance of the deformed aluminum 6 and 7 series is obviously stronger than that of the weld.
  • the invention adopts an acid etching solution with less acidity to carry out acid etching treatment on the test piece.
  • the base metal and the weld are corroded, the clear grain boundary stays for a short time, and the acid etching process is difficult to master.
  • the researchers of the present invention found that when the test piece is pre-corroded with a slightly acidic acid etching solution, the acid etching temperature is treated.
  • the base metal and the weld can have better corrosion results in a period of time. If the etching time is short during the etching process, the grain profile is not clear. If the etching time is too long, the grain boundary is strongly corroded, and many corrosion pits appear.
  • the present invention controls the etching time to 50-60 s. It is possible to obtain a clear metallographic phase in which the crystal grains of the base material and the weld bead are clear.
  • the specimen When immersing in the Weck reagent, the specimen is slightly shaken, which facilitates rapid coloration and uniform coloration, and the grain structure of the base material and the weld be well presented. If it does not shake, the coloring effect is poor, and the required coloring time is multiplied.
  • the pre-corrosion further includes an alkali etching treatment step of immersing the acid-etched test piece in the alkali etching solution for 50-120 s, rinsing with a large amount of deionized water, and drying the hot air, the alkali
  • the etching solution is an aqueous solution containing OH - 0.1 - 0.5 mol / L.
  • the applicant of the present invention unexpectedly discovered in the research that the corrosion-treated test piece was subjected to alkali etching treatment, and the metal between the grain boundaries could be further corroded to obtain a clearer grain boundary interface of the test piece, and the test piece was obtained.
  • the coloring effect is better.
  • the alkali etching treatment can further uniformly weld the base metal and the weld to avoid local corrosion of the weld.
  • the acid etching treatment is to heat the acid etching solution water bath to 65 ° C, and the solution is dropped on the surface of the test piece for 60 s, rinsed with a large amount of deionized water, and dried by hot air.
  • the alkali etching treatment is to heat the alkali etching solution to 40-60 ° C, and the test piece after the acid etching treatment is immersed in the alkali etching solution for 50-120 s, rinsed with a large amount of deionized water, and dried by hot air.
  • the alkali etching treatment is to heat the alkali etching solution to 50 ° C, and the test piece after the acid etching treatment is immersed in the alkali etching solution for ultrasonic vibration for 60-100 s, and then rinsed with a large amount of deionized water, and the hot air is dried, and the ultrasonic frequency is 15-40kHz.
  • the test piece is immersed in an alkali etching solution and ultrasonically oscillated, which has cavitation corrosion effect.
  • Ultrasonic waves generate a large number of tiny bubbles in the alkali etching solution. These bubbles form and grow in the negative pressure region of the longitudinal propagation of the ultrasonic waves, and rapidly rupture in the positive pressure region.
  • the formation, growth and rapid bursting of the microbubbles are called Cavitation.
  • the tiny bubbles form an instantaneous high pressure of more than 1000 atmospheres from the moment of generation, growth and rapid bursting.
  • the continuous high pressure is like a series of small bombs, which are constantly corroded.
  • the metal bombardment causes the aluminum alloy grain boundary metal to be quickly peeled off, so that the grain boundary interface of the aluminum alloy is more clear.
  • the cavitation can also cause the grain boundary and crystal structure of the base material and the weld of the aluminum alloy welded joint to occur. Distortion, distortion, chemical instability, galvanic corrosion is more likely to occur between grain boundaries and crystals, and the electrochemical corrosion of the test piece is aggravated. Ultrasonic cavitation enables the weld and base metal to achieve the same corrosion in a lower concentration of alkaline solution.
  • the acid etching solution is an aqueous solution containing Cl - 0.39 - 0.46 mol / L; H + 1.43-1.79 mol / L; PO 4 3- 0.35 - 0.47 mol / L; preferably the acid etching solution contains Cl - 0.40 - 0.44 mol/L; H + 1.50-1.73 mol/L; PO 4 3- 0.38-0.45 mol/L aqueous solution, more preferably the acid etching solution contains Na + or K + 0.05 mol/L; Cl - 0.43 mol /L; H + 1.64 mol / L; PO 4 3- 0.42 mol / L aqueous solution.
  • the alkali etching solution is an aqueous solution containing OH - 0.1-0.3 mol / L, preferably the alkali etching solution is an aqueous solution containing OH - 0.12 - 0.28 mol / L, more preferably the alkali etching solution contains OH - 0.125 mol /L, Na + or K + 0.125 mol / aqueous solution.
  • the acid etching solution is subjected to an acid etching treatment within 2 to 5 hours after the completion of the preparation of the acid etching solution, and preferably the acid etching treatment is performed within 4 hours after the preparation of the acid etching solution.
  • the acid etching solution contains hydrochloric acid which is easily volatilized. If it is left for a long time after being disposed, it will cause hydrochloric acid to volatilize and affect the acid etching effect. Therefore, in the process of acid etching, the acid etching solution is generally required to be used immediately after preparation. If the acid etching solution is left for more than 5 hours, the acid etching effect will be affected, and the grain boundary of the metallographic photograph is unclear.
  • the etching solution is prepared by adding 0.5-1.8 g of potassium chloride, 25-32 ml of a 35% phosphoric acid solution and 10 ml of a 37% hydrochloric acid solution to 280 ml of deionized water to obtain an acid etching solution.
  • 1.2 g of potassium chloride, 30 ml of a 35% phosphoric acid solution and 10 ml of a 37% hydrochloric acid solution are added to 280 ml of deionized water to obtain an acid etching solution.
  • the alkali etching solution is prepared by adding 1-3 g of NaOH solids to 250 ml of deionized water to obtain an alkali etching solution; preferably, 1.25 g of NaOH solid is added to 250 ml of deionized water to obtain an alkali etching solution.
  • the invention has the advantages and positive effects that: due to the above technical solution, the welded joint of the aluminum alloy welded joint can be synchronously pre-corroded with the base material, and can be quickly colored and uniformly colored, and the grain structure of the base material and the weld bead are both It can be well presented.
  • the method has high success rate, high repeatability and low cost.
  • the color metallographic phase of the deformed aluminum alloy welded joint treated by this method has high contrast display, clear grain boundary and accurate test results. The advantage of high degree.
  • FIG. 1 is a metallographic photograph of a welding wire ER4043 filled with a weld seam by the method of the present invention
  • FIG. 2 is a metallographic photograph of a multi-layer multi-pass welding wire ER5356 filled with a weld seam by the method of the present invention
  • Figure 4 is a metallographic photograph of the 7N01 deformed aluminum colored by the method of the present invention.
  • Figure 5 is a metallographic photograph of the fusion zone of 7N01 deformed aluminum and filler wire ER5356 by the method of the present invention
  • Figure 6 is a metallographic photograph of the 6N01 deformed aluminum colored by the method of the present invention.
  • Figure 7 is a metallographic photograph of the fusion zone of 6N01 deformed aluminum and filler wire ER4043 by the method of the present invention.
  • Figure 8 is a metallographic photograph of the fusion zone of 6N01 deformed aluminum and filler wire ER5356 by the method of the present invention.
  • Figure 9 is a photograph of a metallographic color obtained by coloring the fusion zone of 6N01 deformed aluminum and filler wire ER4043 by the method of Example 5 of the invention CN 103471897 A.
  • the acid-etched test piece is completely immersed in the Weck reagent and gently shaken for 5 s. After the surface is colored, it is rinsed with a large amount of deionized water, and the hot air is blown dry.
  • Fig. 1 The obtained metallographic photograph is shown in Fig. 1. From Fig. 1, it can be seen that the wire ER4043 fills the weld with clear grain boundaries and grain morphology.
  • the alkali-etched test piece is completely immersed in the Weck reagent and gently shaken for 10 s. After the surface is colored, it is rinsed with a large amount of deionized water, and the hot air is blown dry.
  • Fig. 2 The obtained metallographic photograph is shown in Fig. 2. It can be clearly seen from Fig. 2 that the multi-layer multi-pass welding wire ER5356 fill weld has a small grain size in the weld fusion zone, and the crystal grain is column-shaped from the center of the fusion zone. The circumference is arranged in a radial pattern. The grain size of the base metal is large, and the grain boundaries and grain structure of the base metal and the weld are clearly displayed.
  • the alkali etching solution is heated to 40 ° C, the acid etched test piece is immersed in the alkali etching solution for ultrasonic vibration for 60 s, rinsed with a large amount of deionized water, and dried by hot air, the ultrasonic frequency is 15 kHz;
  • the alkali-etched test piece is completely immersed in the Weck reagent and gently shaken for 5 s. After the surface is colored, it is rinsed with a large amount of deionized water, and the hot air is dried.
  • Fig. 3 The obtained metallographic photograph is shown in Fig. 3. From Fig. 3, the clear grain boundary and grain morphology of the heat affected zone of the 7N01 aluminum alloy after welding can be seen.
  • the alkali etching solution is heated to 50 ° C, and the test piece after the acid etching treatment is immersed in the alkali etching solution for ultrasonic vibration for 100 s, and then rinsed with a large amount of deionized water, and the hot air is blown dry, and the ultrasonic frequency is 40 kHz;
  • the alkali-etched test piece is completely immersed in the Weck reagent and gently shaken for 5 s. After the surface is colored, it is rinsed with a large amount of deionized water, and the hot air is dried.
  • Fig. 4 The obtained metallographic photograph is shown in Fig. 4. From Fig. 4, the clear grain boundary and grain morphology of 7N01 deformed aluminum can be seen.
  • the alkali etching solution is heated to 50 ° C, and the test piece after the acid etching treatment is immersed in the alkali etching solution for ultrasonic vibration for 100 s, and then rinsed with a large amount of deionized water, and the hot air is blown dry, and the ultrasonic frequency is 40 kHz;
  • the alkali-etched test piece is completely immersed in the Weck reagent and gently shaken for 5 s. After the surface is colored, it is rinsed with a large amount of deionized water, and the hot air is dried.
  • Fig. 5 The obtained metallographic photograph is shown in Fig. 5. From Fig. 5, it can be seen that the grain boundary and grain morphology of the fusion region of the 7N01 deformed aluminum and the filler wire ER5356 are clear. It can be seen from the comparison between FIG. 4 and FIG. 5 that the deformed aluminum of the base material 7N01 has a large grain size and is arranged in a long strip shape, and the weld area of the weld filler wire ER5356 is small and arranged in a dot shape. The base metal and weld are uniformly corroded and the grain boundaries are clear.
  • the acid-etched test piece is completely immersed in the Weck reagent and gently shaken for 5 s. After the surface is colored, it is rinsed with a large amount of deionized water, and the hot air is blown dry.
  • the alkali etching solution is heated to 50 ° C, and the test piece after the acid etching treatment is immersed in the alkali etching solution for ultrasonic vibration for 100 s, and then rinsed with a large amount of deionized water, and the hot air is blown dry, and the ultrasonic frequency is 40 kHz;
  • the alkali-etched test piece is completely immersed in the Weck reagent and gently shaken for 10 s. After the surface is colored, it is rinsed with a large amount of deionized water, and the hot air is blown dry.
  • Fig. 7 The obtained metallographic photograph is shown in Fig. 7.
  • Fig. 6 the grain of 6N01 deformed aluminum is larger and the grain boundary is more obvious.
  • the fused zone of the filler wire ER4043 has a small crystal grain and is arranged in a worm-like pattern.
  • the upper part in Fig. 7 is a weld bead, and the fusion zone of the filler wire ER4043 is filled.
  • the lower part of Fig. 7 is a base material, and 6N01 is deformed aluminum.
  • both the base metal and the weld can be seen with clear grain boundaries and grain morphology.
  • the base metal and weld seam have good simultaneous corrosion effect.
  • the alkali-etched test piece is completely immersed in the Weck reagent and gently shaken for 10 s. After the surface is colored, it is rinsed with a large amount of deionized water, and the hot air is blown dry.
  • Fig. 8 The obtained metallographic photograph is shown in Fig. 8. From Fig. 8, it can be seen that the 6N01 deformed aluminum base material having a large crystal grain on the right side and the fusion zone weld seam of the filler wire ER5356 having a small crystal grain on the left side are shown. The grain boundary and grain morphology of the base metal and the weld be clearly seen from Fig. 8.
  • the fusion zone of 6N01 deformed aluminum and filler wire ER4043 was colored by the method used in Example 5 of Patent CN 103471897 A, and a color metallographic photograph was obtained as shown in FIG. It can be seen from Fig. 9 that the portion of the 6N01 deformed aluminum base material is not corroded, the grain profile is not clear, and the clear grain boundary and grain morphology cannot be exhibited, and the weld portion of the fusion zone of the filler wire ER4043 is excessively corroded. There are many corrosion pits and no grain structure.

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Abstract

一种变形铝合金焊接接头彩色金相着色方法，包括预腐蚀和着色，其中，预腐蚀包括酸蚀处理步骤，所述酸蚀处理为将酸蚀溶液加热到55-65℃，将溶液滴在试件表面50s-60s后，用大量去离子水冲洗，热风吹干，所述酸蚀溶液为含有Cl －0.3-0.5mol/L；H ＋1.4-1.8 mol/L；PO 4 3 －0.3-0.5 mol/L的水溶液；所述着色为将预腐蚀处理后的试件完全浸入Weck试剂中轻轻晃动5-10s，待表面着色后用大量去离子水冲洗，热风吹干。该方法试样制备的成功率高、可重复性高且成本低，采用该方法处理的变形铝合金焊接接头彩色金相具有衬度显示高、晶界清晰、测试结果准确度高的优点。

Description

一种变形铝合金焊接接头彩色金相着色方法
本申请要求于2014年10月13日提交中国专利局、申请号为201410537773.3、发明名称为“一种变形铝合金焊接接头彩色金相着色方法”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本发明属于金属材料镀覆技术领域，尤其是涉及一种变形铝合金焊接接头彩色金相着色方法。
背景技术
目前检测材料微观组织的手段和方法很多，如电子扫描电镜、电子透视电镜、电子探针、X射线探伤以及高倍金相显微镜等，都可用来检测材料的微观组织，只是每种设备及使用方法对检测参数各有侧重。用高倍金相显微镜来观测铝合金的微观组织尤其是变质效果是非常普遍而有效的，工程技术人员通过对高倍成像进行观察、分析可以预测和判断金属的性能，并分析各种失效和破坏的原因，这个检测分析的过程通常称为金相分析。彩色金相技术是金相分析技术中的一种，其主要是利用化学或者物理的方法，在金属表面形成一层薄厚不等的干涉膜，在光的干涉效应下，不同厚度的干涉膜反射的波长不同，呈现出各自相干波长的补色，从而使金属的不同部位显示出不同的颜色；对于彩色金相分析来说，最重要的工作是制备彩色金相试样，若试样制备不当则可能出现假象，从而得出错误的结论，因此制备彩色金相试样的质量对试样的检测和性能判定起着至关重要的作用。
铝合金具密度低，强度高，具有良好的成形性和焊接性已被广泛应用于航空、高速列车及汽车等领域，其在工业的广泛使用仅次于钢。铝合金相对较软，金相制备难度大。
变形铝合金焊接接头处焊件和焊丝的成分不同，变形铝合金焊件，也称为母材，多为轧制态，是通过冲压、弯曲、轧、挤压等工艺使其组织、形状发生变化的铝合金；焊缝为铸态的铝合金。由于变形铝合金焊接接头处母材与焊缝的成分不同，所以母材与焊缝对侵蚀溶液的抗腐蚀能力也不 同。采用现有技术的预腐蚀方法处理变形铝合金焊接接头，会出现母材和焊缝腐蚀不均匀的问题，所制备出来的彩色金相照片不清晰，导致分析测试结果不准确。
专利CN103471897A公开了一种铝合金彩色金相着色方法，包括以下步骤：(1)预浸蚀：将抛光后的铝合金金相试样浸入浸蚀液中1-10分钟，浸蚀完成后用流水冲洗，乙醇清洗，再吹干；浸蚀液为将氯化钾或氯化钠溶于磷酸得到的溶液，或浸蚀液为磷酸、硝酸和水配制的溶液；(2)着色。该方法步骤简单，着色效果好，可获得清晰的晶粒组织，即使不采用偏振光和敏感色调观察也能获得清晰的微观组织。但是采用该方法处理获得的变形铝合金试样焊接接头熔合区的彩色金相焊缝腐蚀严重，所制备出来的照片中看不出熔化区部分的晶粒组织。
发明内容
本发明的目的是提供一种变形铝合金焊接接头彩色金相着色方法，该方法试样制备的成功率高、可重复性高且成本低，采用该方法处理的变形铝合金焊接接头彩色金相具有衬度显示高、晶界清晰以及测试结果准确度高的优点。
本发明的技术方案是：一种变形铝合金焊接接头彩色金相着色方法，包括预腐蚀和着色，其中，所述预腐蚀包括酸蚀处理步骤，所述酸蚀处理为将酸蚀溶液加热到55-65℃，将溶液滴在试件表面50-60s后，用大量去离子水冲洗，热风吹干，所述酸蚀溶液为含有Cl-0.3-0.5mol/L；H+1.4-1.8mol/L；PO4 3-0.3-0.5mol/L的水溶液；
所述着色为将预腐蚀处理后的试件完全浸入Weck试剂中轻轻晃动5-10s，待表面着色后用大量去离子水冲洗，热风吹干。
焊件和焊丝的成分不同，焊件多为轧制态，焊缝为铸态，导致对酸的抗腐蚀能力不同，变形铝6系和7系的抗腐蚀能力明显的比焊缝的强。本发明采用酸性较小的酸蚀溶液对试件进行酸蚀处理。母材和焊缝腐蚀同时出现清晰晶界停留的时间短，酸蚀过程掌握难度加大。经过大量实验，本发明研究人员发现采用酸性较小的酸蚀溶液预腐蚀试件时，将酸蚀处理温 度控制在55-65℃时，母材和焊缝在一段时间里可以同步出现较好的腐蚀结果。在酸蚀处理过程中如果酸蚀时间短，晶粒的轮廓不清晰，如果酸蚀时间过长则晶界被强烈腐蚀，出现许多的腐蚀小坑，本发明将酸蚀时间控制在50-60s，能够获得母材和焊缝的晶粒都清晰的彩色金相。
在Weck试剂中浸入着色时，轻微的晃动几下试件，这样有利于迅速着色，并着色均匀，母材和焊缝的晶粒组织结构都能够很好的呈现。如果不晃动，着色效果差，且需要的着色时间成倍增加。
所述预腐蚀还包括碱蚀处理步骤，所述碱蚀处理为将酸蚀处理后的试件浸入到碱蚀溶液中50-120s后，用大量去离子水冲洗，热风吹干，所述碱蚀溶液为含有OH-0.1-0.5mol/L的水溶液。
本发明申请人在研究中意外的发现，将酸蚀处理后的试件再进行碱蚀处理，能够将晶界间的金属更进一步的腐蚀，获得试件晶界界面更加清晰，且试件的着色效果更好。采用碱蚀处理能够将母材和焊缝更进一步的均匀腐蚀，避免造成焊缝局部侵蚀的现象。
所述酸蚀处理为将酸蚀溶液水浴加热到65℃，将溶液滴在试件表面60s后，用大量去离子水冲洗，热风吹干。
所述碱蚀处理为将碱蚀溶液加热到40-60℃，将酸蚀处理后的试件浸入到碱蚀溶液中50-120s后，用大量去离子水冲洗，热风吹干。
所述碱蚀处理为将碱蚀溶液加热到50℃，将酸蚀处理后的试件浸入到碱蚀溶液中超声震荡60-100s后，用大量去离子水冲洗，热风吹干，超声频率为15-40kHz。
将试件浸入碱蚀溶液中超声震荡，具有空化腐蚀作用。超声波在碱蚀溶液中产生大量的微小气泡，这些气泡在超声波纵向传播的负压区形成及生长，而在正压区迅速破裂，这种微小气泡的形成、生长及迅速爆裂的过程被称为空化现象。在空化现象发生时，微小气泡从产生、生长及迅速爆裂的瞬间形成超过1000个大气压的瞬间高压，连续不断的瞬间高压就像一连串的小炸弹，不断对较容易被腐蚀的铝合金晶界金属轰击，使铝合金晶界金属迅速剥离，使铝合金的晶界界面更加清晰。同时，在碱性溶液中，空化作用还能够使铝合金焊接接头母材和焊缝处的晶界和晶体结构都发生 扭曲、畸变，出现化学不稳定性，使晶界和晶体间更容易发生电偶腐蚀，加剧试件的电化学腐蚀。超声空化作用能够使焊缝和母材在较低浓度的碱性溶液中获得同样的腐蚀效果。
所述酸蚀溶液为含有Cl-0.39-0.46mol/L；H+1.43-1.79mol/L；PO4 3-0.35-0.47mol/L的水溶液；优选所述酸蚀溶液为含有Cl-0.40-0.44mol/L；H+1.50-1.73mol/L；PO4 3-0.38-0.45mol/L的水溶液，更优选所述酸蚀溶液为含有Na+或K+0.05mol/L；Cl-0.43mol/L；H+1.64mol/L；PO4 3-0.42mol/L的水溶液。
所述碱蚀溶液为含有OH-0.1-0.3mol/L的水溶液，优选所述碱蚀溶液为含有OH-0.12-0.28mol/L的水溶液，更优选所述碱蚀溶液为含有OH-0.125mol/L，Na+或K+0.125mol/的水溶液。
所述酸蚀溶液配制完成后2-5小时内进行酸蚀处理，优选酸蚀溶液配制完成后4小时内进行酸蚀处理。
酸蚀溶液中含有容易挥发的盐酸，如果配置后放置时间过长会导致盐酸挥发，影响酸蚀效果。所以在酸蚀处理的过程中一般要求酸蚀溶液配制后立即使用，如果酸蚀溶液放置时间超过5小时，就会影响酸蚀效果，导致金相照片的晶界不清晰。
所述酸蚀溶液的配制方法为：将0.5-1.8g氯化钾、25-32毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液；优选将1.2g氯化钾、30毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液。
所述碱蚀溶液的配制方法为：将1-3g的NaOH固体加入到250ml去离子水中混合，获得碱蚀溶液；优选将1.25g的NaOH固体加入到250ml去离子水中混合，获得碱蚀溶液。
本发明具有的优点和积极效果是：由于采用上述技术方案变形铝合金焊接接头焊缝与母材能够同步预腐蚀，且能够迅速着色，并着色均匀，母材和焊缝的晶粒组织结构都能够很好的呈现，该方法试样制备的成功率高、可重复性高且成本低，采用该方法处理的变形铝合金焊接接头彩色金相具有衬度显示高、晶界清晰以及测试结果准确度高的优点。
附图说明
图1为采用本发明方法对焊丝ER4043填充焊缝着色后的金相照片；
图2为采用本发明方法对多层多道焊焊丝ER5356填充焊缝着色后的金相照片；
图3为采用本发明方法对7N01铝合金焊后的热影响区着色后的金相照片；
图4为采用本发明方法对7N01变形铝着色后的金相照片；
图5为采用本发明方法对7N01变形铝与填充焊丝ER5356的熔合区着色后的金相照片；
图6为采用本发明方法对6N01变形铝着色后的金相照片；
图7为采用本发明方法对6N01变形铝与填充焊丝ER4043的熔合区着色后的金相照片；
图8为采用本发明方法对6N01变形铝与填充焊丝ER5356的熔合区着色后的金相照片；
图9为采用发明CN 103471897 A实施例5方法对6N01变形铝与填充焊丝ER4043的熔合区着色后的金相照片。
具体实施方式
实施例1
1)将0.5g氯化钾、32毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液；
2)将酸蚀溶液加热到55℃，将溶液滴在磨样、抛光后的焊丝ER4043填充焊缝试件表面60s后，用大量去离子水冲洗，热风吹干；
3)将酸蚀处理后的试件完全浸入Weck试剂中轻轻晃动5s，待表面着色后用大量去离子水冲洗，热风吹干。
获得的金相照片如图1所示，从图1中可以看到焊丝ER4043填充焊缝清晰的晶界和晶粒形态。
实施例2
1)将1.8g氯化钾、32毫升35％的磷酸溶液和10毫升37％的盐酸溶 液加入到280毫升的去离子水中混合，获得酸蚀溶液；
2)将1g的NaOH固体加入到250ml去离子水中混合，获得碱蚀溶液；
3)将酸蚀溶液加热到65℃，将溶液滴在磨样、抛光后的多层多道焊焊丝ER5356填充焊缝试件表面60s后，用大量去离子水冲洗，热风吹干；
4)将碱蚀溶液加热到50℃，将酸蚀处理后的试件浸入到碱蚀溶液100s后，用大量去离子水冲洗，热风吹干；
5)将碱蚀处理后的试件完全浸入Weck试剂中轻轻晃动10s，待表面着色后用大量去离子水冲洗，热风吹干。
获得的金相照片如图2所示，从图2中可以清晰的看到多层多道焊焊丝ER5356填充焊缝中焊缝熔合区的晶粒较小，晶粒为柱状由熔合区中心向周围呈辐射状排布。母材的晶粒较大，母材和焊缝的晶界和晶粒结构显示清晰。
实施例3
1)将1.2g氯化钾、25毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液；
2)将3g的NaOH固体加入到250ml去离子水中混合，获得碱蚀溶液；
3)将酸蚀溶液加热到60℃，将溶液滴在磨样、抛光后的7N01铝合金焊后的热影响区试件表面50s后，用大量去离子水冲洗，热风吹干；
4)将碱蚀溶液加热到40℃，将酸蚀处理后的试件浸入到碱蚀溶液中超声震荡60s后，用大量去离子水冲洗，热风吹干，超声频率为15kHz；
5)将碱蚀处理后的试件完全浸入Weck试剂中轻轻晃动5s，待表面着色后用大量去离子水冲洗，热风吹干。
获得的金相照片如图3所示，从图3中可以看到7N01铝合金焊后的热影响区清晰的晶界和晶粒形态。
实施例4
1)将1.2g氯化钾、30毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液；
2)将1.25g的NaOH固体加入到250ml去离子水中混合，获得碱蚀溶液；
3)将酸蚀溶液加热到65℃，将溶液滴在磨样、抛光后的7N01变形铝试件表面60s后，用大量去离子水冲洗，热风吹干；
4)将碱蚀溶液加热到50℃，将酸蚀处理后的试件浸入到碱蚀溶液中超声震荡100s后，用大量去离子水冲洗，热风吹干，超声频率为40kHz；
5)将碱蚀处理后的试件完全浸入Weck试剂中轻轻晃动5s，待表面着色后用大量去离子水冲洗，热风吹干。
获得的金相照片如图4所示，从图4中可以看到7N01变形铝清晰的晶界和晶粒形态。
实施例5
1)将1.2g氯化钾、30毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液；
2)将1.25g的NaOH固体加入到250ml去离子水中混合，获得碱蚀溶液；
3)将酸蚀溶液加热到65℃，将溶液滴在磨样、抛光后的7N01变形铝与填充焊丝ER5356的熔合区试件表面60s后，用大量去离子水冲洗，热风吹干；
4)将碱蚀溶液加热到50℃，将酸蚀处理后的试件浸入到碱蚀溶液中超声震荡100s后，用大量去离子水冲洗，热风吹干，超声频率为40kHz；
5)将碱蚀处理后的试件完全浸入Weck试剂中轻轻晃动5s，待表面着色后用大量去离子水冲洗，热风吹干。
获得的金相照片如图5所示，从图5中可以看到7N01变形铝与填充焊丝ER5356的熔合区清晰的晶界和晶粒形态。通过图4与图5的对比可以看出，母材7N01变形铝的晶粒较大，呈长条形规则排布，焊缝填充焊丝ER5356的熔合区晶粒较小，呈点状排布。母材和焊缝腐蚀均匀，晶界清晰。
实施例6
1)将1.5g氯化钾、32毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液；
2)将酸蚀溶液加热到65℃，将溶液滴在磨样、抛光后的6N01变形铝 试件表面50s后，用大量去离子水冲洗，热风吹干；
3)将酸蚀处理后的试件完全浸入Weck试剂中轻轻晃动5s，待表面着色后用大量去离子水冲洗，热风吹干。
获得的金相照片如图6所示，从图6中可以看到6N01变形铝清晰的晶界和晶粒形态。
实施例7
1)将0.5g氯化钾、30毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液；
2)将1.25g的NaOH固体加入到250ml去离子水中混合，获得碱蚀溶液；
3)将酸蚀溶液加热到60℃，将溶液滴在磨样、抛光后的6N01变形铝与填充焊丝ER4043的熔合区试件表面60s后，用大量去离子水冲洗，热风吹干；
4)将碱蚀溶液加热到50℃，将酸蚀处理后的试件浸入到碱蚀溶液中超声震荡100s后，用大量去离子水冲洗，热风吹干，超声频率为40kHz；
5)将碱蚀处理后的试件完全浸入Weck试剂中轻轻晃动10s，待表面着色后用大量去离子水冲洗，热风吹干。
获得的金相照片如图7所示。如图6所示，6N01变形铝的晶粒较大，晶界较为明显。如图1所示，填充焊丝ER4043的熔合区晶粒较小，呈蠕虫状不规则排布。图7中的上部为焊缝，填充焊丝ER4043的熔合区，图7的下部为母材，6N01变形铝。图7中，母材和焊缝都可以看出清晰的晶界和晶粒形态。母材和焊缝同步腐蚀效果好。
实施例8
1)将1.2g氯化钾、30毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液；
2)将1.25g的NaOH固体加入到250ml去离子水中混合，获得碱蚀溶液；
3)将酸蚀溶液加热到60℃，将溶液滴在磨样、抛光后的6N01变形铝与填充焊丝ER5356的熔合区试件表面60s后，用大量去离子水冲洗，热 风吹干；
4)将碱蚀溶液加热到50℃，将酸蚀处理后的试件浸入到碱蚀溶液中超声震荡100s后，用大量去离子水冲洗，热风吹干，超声频率为30kHz；
5)将碱蚀处理后的试件完全浸入Weck试剂中轻轻晃动10s，待表面着色后用大量去离子水冲洗，热风吹干。
获得的金相照片如图8所示，从图8中可以看到右侧为晶粒较大的6N01变形铝母材，左侧为晶粒较小的填充焊丝ER5356的熔合区焊缝。从图8中可以清晰的看到母材和焊缝的晶界和晶粒形态。
实验例1
将6N01变形铝与填充焊丝ER4043的熔合区采用专利CN 103471897 A实施例5所用方法进行着色，获得彩色金相照片如图9所示。从图9中可以看出，6N01变形铝母材部分没有得到腐蚀，晶粒轮廓不清晰，不能显示出清晰的晶界和晶粒形态，而填充焊丝ER4043的熔合区的焊缝部分腐蚀过度，出现许多的腐蚀小坑，也看不出晶粒结构。
以上对本发明的实施例进行了详细说明，但所述内容仅为本发明的较佳实施例，不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等，均应仍归属于本发明的专利涵盖范围之内。

Claims (10)

  1. 一种变形铝合金焊接接头彩色金相着色方法，包括预腐蚀和着色，其特征在于：所述预腐蚀包括酸蚀处理步骤，所述酸蚀处理为将酸蚀溶液加热到55-65℃，将溶液滴在试件表面50-60s后，用大量去离子水冲洗，热风吹干，所述酸蚀溶液为含有Cl-0.3-0.5mol/L；H+1.4-1.8mol/L；PO4 3-0.3-0.5mol/L的水溶液；
    所述着色为将预腐蚀处理后的试件完全浸入Weck试剂中轻轻晃动5-10s，待表面着色后用大量去离子水冲洗，热风吹干。
  2. 根据权利要求1所述的一种变形铝合金焊接接头彩色金相着色方法，其特征在于：所述预腐蚀还包括碱蚀处理步骤，所述碱蚀处理为将酸蚀处理后的试件浸入到碱蚀溶液中50-120s后，用大量去离子水冲洗，热风吹干，所述碱蚀溶液为含有OH-0.1-0.5mol/L的水溶液。
  3. 根据权利要求1所述的一种变形铝合金焊接接头彩色金相着色方法，其特征在于：所述酸蚀处理为将酸蚀溶液水浴加热到65℃，将溶液滴在试件表面60s后，用大量去离子水冲洗，热风吹干。
  4. 根据权利要求2所述的一种变形铝合金焊接接头彩色金相着色方法，其特征在于：所述碱蚀处理为将碱蚀溶液加热到40-60℃，将酸蚀处理后的试件浸入到碱蚀溶液中50-120s后，用大量去离子水冲洗，热风吹干。
  5. 根据权利要求4所述的一种变形铝合金焊接接头彩色金相着色方法，其特征在于：所述碱蚀处理为将碱蚀溶液加热到50℃，将酸蚀处理后的试件浸入到碱蚀溶液中超声震荡60-100s后，用大量去离子水冲洗，热风吹干，超声频率为15-40kHz。
  6. 根据权利要求1所述的一种变形铝合金焊接接头彩色金相着色方法，其特征在于：所述酸蚀溶液为含有Cl-0.39-0.46mol/L；H+1.43-1.79mol/L；PO4 3-0.35-0.47mol/L的水溶液；优选所述酸蚀溶液为含有Cl-0.40-0.44mol/L；H+1.50-1.73mol/L；PO4 3-0.38-0.45mol/L的水溶液，更优选所述酸蚀溶液为含有Na+或K+0.05mol/L；Cl-0.43mol/L；H+1.64mol/L；PO4 3-0.42mol/L的水溶液。
  7. 根据权利要求2所述的一种变形铝合金焊接接头彩色金相着色方法，其特征在于：所述碱蚀溶液为含有OH-0.1-0.3mol/L的水溶液，优选所述碱蚀溶液为含有OH-0.12-0.28mol/L的水溶液，更优选所述碱蚀溶液为含有OH-0.125mol/L，Na+或K+0.125mol/的水溶液。
  8. 根据权利要求1-7任意一项所述的一种变形铝合金焊接接头彩色金相着色方法，其特征在于：所述酸蚀溶液配制完成后2-5小时内进行酸蚀处理，优选酸蚀溶液配制完成后4小时内进行酸蚀处理。
  9. 根据权利要求1所述的一种变形铝合金焊接接头彩色金相着色方法，其特征在于：所述酸蚀溶液的配制方法为：将0.5-1.8g氯化钾、25-32毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液；优选将1.2g氯化钾、30毫升35％的磷酸溶液和10毫升37％的盐酸溶液加入到280毫升的去离子水中混合，获得酸蚀溶液。
  10. 根据权利要求2所述的一种变形铝合金焊接接头彩色金相着色方法，其特征在于：所述碱蚀溶液的配制方法为：将1-3g的NaOH固体加入到250ml去离子水中混合，获得碱蚀溶液；优选将1.25g的NaOH固体加入到250ml去离子水中混合，获得碱蚀溶液。
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114371057A (zh) * 2022-01-13 2022-04-19 西安交通大学 一种稀土镁合金金相腐蚀剂及其金相试样制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN113092226A (zh) * 2021-04-09 2021-07-09 芜湖天弋能源科技有限公司 一种铝及铝合金金相腐蚀剂、锂离子电池含铝焊接部位的金相测试方法
CN114318341B (zh) * 2021-12-16 2023-09-05 东风汽车集团股份有限公司 一种铝合金金相腐蚀方法及其金相腐蚀剂
CN115931516B (zh) * 2022-10-18 2024-04-19 新余钢铁股份有限公司 一种冷轧双相钢中金相组织的彩色染色剂及其染色方法

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06241963A (ja) * 1993-02-12 1994-09-02 Nkk Corp アルミニウム合金の抽出レプリカ膜の作成方法
US5956565A (en) * 1996-11-14 1999-09-21 Matsushita Electronics Corporation Analysis apparatus and analysis methods for semiconductor devices
KR20100037078A (ko) * 2003-11-14 2010-04-08 동우 화인켐 주식회사 알루미늄 또는 알루미늄 합금, 및/또는 몰리브덴 또는 몰리브덴 합금으로 이루어진 단일막 및 다층막 식각액 조성물
CN101864565A (zh) * 2009-04-15 2010-10-20 梁永东 利用钼酸铵为主要着色试剂的铝合金着色方法
CN102127784A (zh) * 2010-01-20 2011-07-20 中国科学院金属研究所 一种电镀Cu叠层膜及其制备方法
CN103471897A (zh) * 2013-09-09 2013-12-25 河北科技大学 一种铝合金彩色金相着色方法
CN203705355U (zh) * 2014-01-26 2014-07-09 宜昌宏箭铝业有限责任公司 一种铝型材表处后焊合线缺陷的基材即时鉴定设备
CN104359742A (zh) * 2014-10-13 2015-02-18 南车青岛四方机车车辆股份有限公司 一种变形铝合金焊接接头彩色金相着色方法

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6200693B1 (en) * 1997-05-22 2001-03-13 Henkel Corporation Water-based liquid treatment for aluminum and its alloys
CN1848322B (zh) * 2006-03-17 2010-06-30 北京科技大学 一种可控高压阳极铝箔隧道孔长度的腐蚀方法
CN102941423B (zh) * 2012-12-08 2015-02-04 中国兵器工业第五二研究所 一种铝合金焊丝的制备方法
CN103668386B (zh) * 2013-12-17 2016-04-06 广西理工职业技术学院 铝及铝合金表面处理方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06241963A (ja) * 1993-02-12 1994-09-02 Nkk Corp アルミニウム合金の抽出レプリカ膜の作成方法
US5956565A (en) * 1996-11-14 1999-09-21 Matsushita Electronics Corporation Analysis apparatus and analysis methods for semiconductor devices
KR20100037078A (ko) * 2003-11-14 2010-04-08 동우 화인켐 주식회사 알루미늄 또는 알루미늄 합금, 및/또는 몰리브덴 또는 몰리브덴 합금으로 이루어진 단일막 및 다층막 식각액 조성물
CN101864565A (zh) * 2009-04-15 2010-10-20 梁永东 利用钼酸铵为主要着色试剂的铝合金着色方法
CN102127784A (zh) * 2010-01-20 2011-07-20 中国科学院金属研究所 一种电镀Cu叠层膜及其制备方法
CN103471897A (zh) * 2013-09-09 2013-12-25 河北科技大学 一种铝合金彩色金相着色方法
CN203705355U (zh) * 2014-01-26 2014-07-09 宜昌宏箭铝业有限责任公司 一种铝型材表处后焊合线缺陷的基材即时鉴定设备
CN104359742A (zh) * 2014-10-13 2015-02-18 南车青岛四方机车车辆股份有限公司 一种变形铝合金焊接接头彩色金相着色方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114371057A (zh) * 2022-01-13 2022-04-19 西安交通大学 一种稀土镁合金金相腐蚀剂及其金相试样制备方法

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