CN111257091A - Metallographic corrosion method for laser welding joint of hastelloy C-276 and 304 stainless steel - Google Patents

Metallographic corrosion method for laser welding joint of hastelloy C-276 and 304 stainless steel Download PDF

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CN111257091A
CN111257091A CN202010193349.7A CN202010193349A CN111257091A CN 111257091 A CN111257091 A CN 111257091A CN 202010193349 A CN202010193349 A CN 202010193349A CN 111257091 A CN111257091 A CN 111257091A
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corrosion
welded joint
metallographic
etching
hastelloy
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徐德生
王颖
赵小辉
余浩轩
赵才宇
金歌
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Jilin University
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Jilin University
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
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Abstract

The invention relates to the technical field of metallographic corrosion of a corrosion-resistant dissimilar alloy welded joint, in particular to a metallographic corrosion method for a laser welded joint of Hastelloy C-276 and 304 stainless steel, which is characterized in that the metallographic corrosion of the laser welded joint of the Hastelloy C-276 and 304 stainless steel is carried out at room temperature by adopting a chemical etching and electrolytic etching combined corrosion method, wherein the chemical etching method adopts aqua regia solution corrosion, and the electrolytic etching method adopts saturated oxalic acid solution electrolytic corrosion. The invention effectively solves the problem that the metallographic structure of a single corrosion welded joint is not obvious. Therefore, the corrosive and the corrosion method can be used for obtaining the metallographic microstructure of the hastelloy C-276 and 304 stainless steel, the operation method is simple and easy to implement, and the grain boundary contour of the structure is clear.

Description

Metallographic corrosion method for laser welding joint of hastelloy C-276 and 304 stainless steel
Technical Field
The invention relates to the technical field of metallographic corrosion of a corrosion-resistant dissimilar alloy welded joint, and provides a metallographic corrosion method for a laser welded joint of C-276 Hastelloy and 304 stainless steel.
Background
Hastelloy C-276 is an alloy with good corrosion resistance, and is often applied to important fields of chemical industry, nuclear power stations, aviation industry and the like. Due to the high price, on the premise of meeting the use requirement, in order to save cost, the hastelloy alloy is often welded with other materials for use, and most commonly, hastelloy alloy C-276 and 304 stainless steel are welded. Because of different alloy components in the metal, the structures are slightly different, so that the corrosion performance is different. In the metallographic corrosion process, the serious corrosion of 304 stainless steel or the too light corrosion of C-276 alloy often occurs, the metallographic structure of a welded joint is not obvious, and the difficulty is caused in analyzing the structural characteristics of the welded joint.
The metallographic etching method generally used includes: (1) chemical etching method, (2) electrolytic etching method. The corrosion solution commonly used by the stainless steel chemical etching method is aqua regia, as the corrosion resistance of the Hastelloy C-276 is better than that of 304 stainless steel, the corrosion of the 304 stainless steel always appears by using the aqua regia, and the surface of the Hastelloy C-276 is smooth, so the observation effect is poor; the electrolytic corrosion of the base material 304 is poor in corrosion, and the metallographic observation effect cannot be achieved.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a metallographic corrosion method for a laser welding joint of hastelloy C-276 and 304 stainless steel, which corrodes a welding joint of the hastelloy and the stainless steel by adopting a chemical etching and electrolytic corrosion combined corrosion method to obtain a better metallographic structure.
The technical scheme for solving the technical problems is as follows:
a metallographic corrosion method for a laser welding joint of Hastelloy C-276 and 304 stainless steel is characterized in that the metallographic corrosion method is adopted for carrying out metallographic corrosion on the laser welding joint of the Hastelloy C-276 and 304 stainless steel at room temperature by adopting a chemical etching and electrolytic etching combined corrosion method, the chemical etching method adopts aqua regia solution for corrosion, and the electrolytic etching method adopts saturated oxalic acid solution for electrolytic corrosion.
The method comprises the following steps:
1) preparing aqua regia solution, and standing at a vent;
2) preparing a saturated oxalic acid solution: dissolving 10g of oxalic acid in 100ml of water, fully stirring, and filtering out precipitates to obtain the oxalic acid water solution;
3) cutting the welding joint, grinding and polishing by adopting a special fixture, washing the surface of the joint to be welded with water and drying;
4) firstly, corroding a welded joint by adopting aqua regia solution at room temperature, and then washing the welded joint by using clear water and drying the welded joint;
5) and performing electrolytic corrosion on the welded joint by using a saturated oxalic acid solution at room temperature, washing the welded joint by using clear water, and drying the welded joint by blowing.
Further, the aqua regia solution used for corroding the welded joint is left standing for 3-4 hours in a ventilated place before corrosion.
Further, the corrosion time of the aqua regia solution for corroding the welding joint in the step 4) is 10-12s, and the preferred corrosion time is 10 s.
Further, the electrolytic corrosion in the step 5) is to connect the welding joint to the anode of the electrolytic device, connect the aluminum alloy electrode to the cathode of the electrolytic device, set the electrolytic voltage at 8-10V, and the corrosion time at 20-22s, preferably 20 s.
The invention has the beneficial effects that:
according to the invention, the metallographic corrosion of the laser welding joint of hastelloy c-276 and 304 stainless steel is carried out by sequentially adopting a combined corrosion mode of aqua regia solution and saturated oxalic acid solution, so that the problem that the metallographic structure of a single corrosion welding joint is not obvious can be effectively solved. Therefore, the corrosive and the corrosion method can be used for obtaining the metallographic microstructure of the hastelloy C-276 and 304 stainless steel, the operation method is simple and easy to implement, and the grain boundary contour of the structure is clear.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a metallographic structure diagram of a laser welded joint of hastelloy C-276 and 304 stainless steel under single electrolytic corrosion;
FIG. 2 is a metallographic structure diagram of a laser welded joint of hastelloy C-276 and 304 stainless steel corroded by a single aqua regia solution;
FIG. 3 is a metallographic representation of the metallographic structure of a laser welded joint of Hastelloy C-276 and 304 stainless steel using a combination corrosion regime according to the method of the present invention.
Detailed Description
Preparing aqua regia solution and saturated oxalic acid solution according to the following method: aqua regia solution: the concentrated nitric acid and the concentrated hydrochloric acid are mixed according to the volume fraction of 1: 3. Saturated oxalic acid solution: dissolving 10g of oxalic acid in 100ml of water, fully stirring, and filtering out precipitates to obtain the oxalic acid.
And standing the solder joint for 3-4h in a ventilated place before the aqua regia solution for corroding the solder joint is corroded.
The laser welding equipment is HKW-1050.
Butt welding Hastelloy and 304 stainless steel, wherein the thickness of each plate is 0.381mm, and cutting a welded sample into 10mm multiplied by 12 mm; because the used material is very thin, the cut sample needs to be clamped by a special clamp, and then the cross section of the welding line is polished and flattened by No. 2000 abrasive paper and polished; and when the surface of the sample meets the quality requirement, washing the sample with water and drying the sample.
Example 1:
firstly, absorbing a small amount of aqua regia solution by a suction pipe at room temperature of 20-22 ℃ to corrode a welded joint of a sample, and slowly flowing corrosive liquid along the surface of the sample for corrosion for 10 s; then washing the fabric by using clear water and drying the fabric;
and then, at room temperature of 20-22 ℃, putting the sample into a saturated oxalic acid solution to carry out electrolytic corrosion on the welding joint, connecting the welding joint of the sample into the anode of an electrolytic device, connecting an aluminum alloy electrode into the cathode of the electrolytic device, setting the electrolytic voltage to be 8V and the corrosion time to be 20s, and then, washing the sample clean with clear water and drying the sample clean.
Fig. 3 is a metallographic microstructure of hastelloy C-276 and 304 stainless steel obtained in the present embodiment, as can be seen from fig. 3, the grain boundary profile of the microstructure is clear, and fig. 3(e) is a metallographic picture of 304 stainless steel, which is clear.
In order to expand, the electrolytic etching time is adjusted in the embodiment, and experiments of comparing the electrolytic etching time for 15s and 25s respectively are performed under the same conditions, and the results show that the shape of 15s etched grains is slightly shallow, some grains are not etched, and the surface unevenness occurs when the grain boundary after 25s etching is deep. The etching time is 20-22s, and the crystal grains are clearly and badly seen, so that the etching time is most suitable.
Example 2:
firstly, absorbing a small amount of aqua regia solution by a suction pipe at room temperature of 20-22 ℃ to corrode a welded joint of a sample, and slowly flowing corrosive liquid along the surface of the sample for corrosion for 11 s; then washing the fabric by using clear water and drying the fabric;
and then, at room temperature of 20-22 ℃, putting the sample into a saturated oxalic acid solution to carry out electrolytic corrosion on the welding joint, connecting the welding joint of the sample into the anode of an electrolytic device, connecting an aluminum alloy electrode into the cathode of the electrolytic device, setting the electrolytic voltage to be 10V and the corrosion time to be 21s, and then, washing the sample clean with clear water and drying the sample clean.
Example 3:
firstly, absorbing a small amount of aqua regia solution by a suction pipe at the room temperature of 20-22 ℃ to corrode a welded joint of a sample, and slowly flowing corrosive liquid along the surface of the sample for corrosion for 12 s; then washing the fabric by using clear water and drying the fabric;
and then, at room temperature of 20-22 ℃, putting the sample into a saturated oxalic acid solution to carry out electrolytic corrosion on the welding joint, connecting the welding joint of the sample into the anode of an electrolytic device, connecting an aluminum alloy electrode into the cathode of the electrolytic device, setting the electrolytic voltage to be 9V and the corrosion time to be 22s, and then, washing the sample clean with clear water and drying the sample clean.
Comparative example 1:
absorbing a small amount of aqua regia solution by using a suction pipe at room temperature of 20-22 ℃ to corrode a welded joint of a sample, and slowly flowing the corrosive solution along the surface of the sample for corrosion for 10 s; then the mixture is washed clean by clean water and dried.
FIG. 2 is a metallographic microstructure of hastelloy C-276 and 304 stainless steel obtained in the comparative example, and observed under a light microscope, the surfaces of the C-276 alloy and the welding line are smooth, the welding line and the C-276 alloy have obvious boundary, and the metallographic structure is not obvious.
Comparative example 2:
and (2) at room temperature of 20-22 ℃, putting the sample into a saturated oxalic acid solution to carry out electrolytic corrosion on the welding joint, connecting the welding joint of the sample into an anode of an electrolytic device, connecting an aluminum alloy electrode into a cathode of the electrolytic device, setting the electrolytic voltage to be 8V, and setting the corrosion time to be 20s, and then, washing the sample clean with clear water and drying the sample clean.
FIG. 1 shows the metallographic microstructure of hastelloy C-276 and 304 stainless steel obtained in this comparative example, and when observed under a light microscope, the surface of the 304 base metal near the weld joint is flat, and the metallographic structure is unclear.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications and equivalent variations of the above embodiment according to the present invention are within the scope of the present invention.

Claims (7)

1. A metallographic corrosion method for a laser welding joint of Hastelloy C-276 and 304 stainless steel is characterized in that the metallographic corrosion method is adopted to carry out metallographic corrosion on the laser welding joint of the Hastelloy C-276 and 304 stainless steel at room temperature by adopting a chemical etching and electrolytic etching combined corrosion method, the chemical etching method adopts aqua regia solution corrosion, and the electrolytic etching method adopts saturated oxalic acid solution electrolytic corrosion.
2. The method of metallographic corrosion of a laser welded joint of hastelloy C-276 and 304 stainless steel according to claim 1, comprising the steps of:
1) preparing aqua regia solution, and standing at a vent;
2) preparing a saturated oxalic acid solution: dissolving 10g of oxalic acid in 100ml of water, fully stirring, and filtering out precipitates to obtain the oxalic acid water solution;
3) cutting the welding joint, grinding and polishing by adopting a special fixture, washing the surface of the joint to be welded with water and drying;
4) firstly, corroding a welded joint by adopting aqua regia solution at room temperature, and then washing the welded joint by using clear water and drying the welded joint;
5) and performing electrolytic corrosion on the welded joint by using a saturated oxalic acid solution at room temperature, washing the welded joint by using clear water, and drying the welded joint by blowing.
3. The method for metallographic etching of a laser welded joint of hastelloy C-276 and 304 stainless steel according to claim 1 or 2, wherein the aqua regia solution used for etching the welded joint is left standing for 3 to 4 hours in a ventilated place before etching.
4. The metallographic etching method for a laser welded joint of hastelloy C-276 and 304 stainless steel according to claim 2, wherein the etching time of the aqua regia solution etching the welded joint in step 4) is 10 to 12 seconds.
5. The method of metallographic etching a laser welded joint of hastelloy C-276 and 304 stainless steel of claim 4 wherein the etching time is 10 seconds.
6. The metallographic etching method for the laser welded joint of hastelloy C-276 and 304 stainless steel as claimed in claim 2, wherein in the step 5), the electrolytic etching is performed by connecting the welded joint to an anode of an electrolytic device, connecting an aluminum alloy electrode to a cathode of the electrolytic device, setting the electrolytic voltage to be 8-10V, and the etching time to be 20-22 s.
7. The method of metallographic etching a laser welded joint of hastelloy C-276 and 304 stainless steel of claim 6 wherein the etching time is 20 seconds.
CN202010193349.7A 2020-03-18 2020-03-18 Metallographic corrosion method for laser welding joint of hastelloy C-276 and 304 stainless steel Pending CN111257091A (en)

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CN112816299A (en) * 2021-02-19 2021-05-18 唐山钢铁集团有限责任公司 Metallographic corrosion and detection method for low-temperature steel welded joint
CN114526978A (en) * 2022-02-25 2022-05-24 中国工程物理研究院材料研究所 Metallographic corrosive liquid of vanadium alloy and preparation method of metallographic sample of vanadium alloy

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CN112816299A (en) * 2021-02-19 2021-05-18 唐山钢铁集团有限责任公司 Metallographic corrosion and detection method for low-temperature steel welded joint
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Application publication date: 20200609