A method for preparing a YZZnAl4Cu1 spectrum standard sample

Abstract

The invention discloses a YZZnAl 4 Cu 1 The invention discloses a method for preparing a spectral standard sample, belonging to the technical field of preparing a spectral standard sample of a zinc alloy. The invention puts various raw materials weighed by mass percentage into a vacuum melting furnace, first melts the Zn raw material, then adds Cu and Fe raw materials with high melting points, then adds Al raw material, and after Al is melted, adds Pb, Sn, Cd and Mg raw materials, pours the molten zinc alloy liquid into a mold with a cylindrical cavity for solidification, obtains a zinc alloy blank, performs a first heat treatment on the zinc alloy blank, performs a second heat treatment on the zinc alloy blank obtained by extrusion processing, and finally obtains a zinc alloy spectral standard sample with component uniformity and organizational uniformity meeting requirements, meets multi-point sampling test, and has very high spectral test accuracy.

Description

Technical Field

[0001] The invention belongs to the technical field of zinc alloy spectrum standard sample preparation, and in particular relates to a method for preparing a YZZnAl4Cu1 spectrum standard sample. Background Art

[0002] Among nonferrous metals, zinc has a storage volume and consumption demand second only to aluminum and copper. Pure zinc is greatly limited in its direct application as an engineering structural material due to its low mechanical properties. Alloy elements such as Al, Cu, and Mg are usually added to improve the mechanical properties and alloy fluidity of zinc alloy materials. As a new type of engineering material, zinc alloy has the characteristics of corrosion resistance, low production cost, excellent casting performance, excellent wear resistance and friction reduction, and excellent damping performance, making it very competitive in the market for steel coatings, hardware, bearings, gears, etc. Among them, YZZnAl4Cu1 zinc alloy is widely used in automotive parts, building hardware, mechanical parts, electrical components, and instrument parts due to its good tensile strength, hardness, and wear resistance.

[0003] Since the performance of zinc alloys is very sensitive to their composition, zinc alloy manufacturers need to conduct real-time detection and analysis of the zinc alloy composition during the production process to ensure the quality of zinc alloy products. As an alloy composition detection device that can quickly test multiple elements at the same time, is environmentally friendly to use, and is simple to operate, the direct reading spectrometer meets the needs of zinc alloy manufacturers for the detection efficiency and accuracy of zinc alloy products, and is widely used in the development and production of zinc alloy products. At present, direct reading spectrometers are equipped with test method curves for the alloy elements to be tested when they leave the factory. In actual use, it is only necessary to configure standard samples with a composition close to the alloy to be tested and a consistent physical state to perform a single-point correction on the test method curve to ensure the accuracy of the test results. Since there are many zinc alloy grades and the alloy compositions of different grades vary greatly, in order to ensure the accuracy of the test results, standard samples need to be configured for each alloy.

[0004] At present, the spectral standard samples of different zinc alloy grades on the market are incomplete. The commercially available standard samples cannot meet the composition detection requirements of YZZnAl4Cu1 alloy in terms of composition, and the commercially available standard samples have large measurement errors for impurity elements in zinc alloys. Therefore, zinc alloy manufacturers often make their own zinc alloy spectral standard samples. However, self-made standard samples often have shortcomings such as large composition unevenness and serious segregation of some elements, which can easily lead to inaccurate test results in actual use. Summary of the invention

[0005] The purpose of the present invention is to solve the problem that there is no suitable standard sample corresponding to the YZZnAl4Cu1 alloy in composition, resulting in poor accuracy of spectrum testing, and to propose a method for preparing a YZZnAl4Cu1 spectrum standard sample.

[0006] In order to achieve the above object, the present invention adopts the following technical scheme: a method for preparing a YZZnAl4Cu1 spectrum standard sample, characterized in that it comprises the following steps:

[0007] 1) preparing the raw materials according to the following weight percentages: Al 3.9-4.3%, Cu 0.7-1.1%, Mg 0.03-0.06%, Fe 0.005-0.020%, Pb 0.002-0.004%, Sn 0.001-0.002%, Cd 0.002-0.004%, and the rest is Zn, which is conducive to achieving effective control of the composition of the YZZnAl4Cu1 zinc alloy spectrum standard sample and improving the success rate of preparing the YZZnAl4Cu1 zinc alloy spectrum standard sample;

[0008] 2) Prepare a vacuum melting furnace, place the raw material Zn in the graphite crucible of the vacuum melting furnace, place other raw materials in the filling position of the vacuum melting furnace, turn on the heating device to heat the graphite crucible, close the furnace chamber for vacuuming, and wait until the vacuum degree reaches 10 -3 Pa, the vacuum was stopped and high-purity argon was filled into the furnace to make the pressure inside the furnace reach 2×10 4 ~3×10 4 pa, perform vacuum operation again, and wait until the vacuum degree reaches 10 -3 Pa, stop evacuating and fill the furnace with high-purity argon to a temperature of 2×10 4 ~3×10 4 Pa, raise the temperature of the graphite crucible, and wait for the raw material Zn in the graphite crucible to melt to form zinc liquid;

[0009] 3) adding raw materials of high melting point metals such as Cu and Fe into the graphite crucible from the filling position, starting to stir the alloy melt, adding raw material Al, and after Al is completely melted, adding raw materials Pb, Sn, Cd, and Mg into the graphite crucible from the filling position, and continuing to stir for 10 to 30 minutes to obtain a zinc alloy liquid, pouring the zinc alloy liquid into a steel mold, the internal cavity of the steel mold is cylindrical, and removing the mold to obtain the zinc alloy after the zinc alloy liquid solidifies, which helps to reduce the oxidation degree of each alloy element, reduce the impurity and gas content of the YZZnAl4Cu1 zinc alloy spectrum standard sample, and help to achieve effective control of the composition of the YZZnAl4Cu1 zinc alloy spectrum standard sample, and obtain a dense structure YZZnAl4Cu1 zinc alloy spectrum standard sample;

[0010] 4) The zinc alloy blank is subjected to the first heat treatment, which can significantly improve the plastic deformation ability of the YZZnAl4Cu1 zinc alloy spectrum standard sample, reduce the strength and hardness of the zinc alloy spectrum standard sample, and is beneficial to the subsequent extrusion processing of the YZZnAl4Cu1 zinc alloy spectrum standard sample;

[0011] 5) Extruding the zinc alloy billet to obtain a zinc alloy spectrum standard sample with a length of 100 to 150 mm. Extrusion processing can significantly break up dendrites, effectively eliminate or reduce casting defects such as shrinkage cavities and looseness, and improve the composition uniformity and organizational uniformity of the alloy;

[0012] 6) The zinc alloy spectral standard sample is subjected to a second heat treatment to obtain the final zinc alloy spectral standard sample, which can effectively eliminate the internal stress of the YZZnAl4Cu1 zinc alloy spectral standard sample caused by extrusion processing, and at the same time eliminate the changes in its microstructure morphology and macroscopic appearance during subsequent long-term use.

[0013] As a further description of the above technical solution:

[0014] In the step 1), each raw material is in the form of a small block or a small rod with a size not exceeding 20 mm, and the purity of each raw material is higher than 99.9%.

[0015] As a further description of the above technical solution:

[0016] In the step 2), the temperature of the graphite crucible is 400-650°C.

[0017] As a further description of the above technical solution:

[0018] In the step 4), the zinc alloy blank is kept at 250-360° C. for 3-20 hours and then cooled, and then the zinc alloy blank is kept at 100-200° C. for 1-30 hours and then cooled.

[0019] As a further description of the above technical solution:

[0020] In the step 5), the extrusion temperature is 150-250° C., the extrusion speed is 1-5 mm / s, and the number of extrusions is 3-10 times.

[0021] As a further description of the above technical solution:

[0022] In the step 6), the zinc alloy spectrum standard sample is kept at 100-150° C. for 1-30 hours and then cooled.

[0023] As a further description of the above technical solution:

[0024] In the step 6), samples are taken at different positions of the zinc alloy spectral standard sample, and the zinc alloy spectral standard sample is subjected to composition analysis by ICP-OES, and a composition uniformity test is performed on the sample. After the standard deviation SD of all measurement data is calculated, it is compared with the repeatability limit r of the measurement method. When 1.5SD≤r, the uniformity is considered to be qualified, and when 1.5SD>r, the uniformity is considered to be unqualified.

[0025] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0026] In the present invention, various raw materials weighed by mass percentage are put into a vacuum melting furnace, the Zn raw material is first melted, and then Cu and Fe raw materials with high melting points are added, and then the Al raw material is added, and after the Al is melted, the Pb, Sn, Cd and Mg raw materials are added, and the molten zinc alloy liquid is poured into a mold with a cylindrical cavity for solidification to obtain a zinc alloy billet, the zinc alloy billet is subjected to a first heat treatment, and then the zinc alloy billet is extruded, and the zinc alloy billet obtained by the extrusion process is subjected to a second heat treatment, and finally a zinc alloy spectrum standard sample with component uniformity and organizational uniformity meeting the requirements is obtained, which meets the requirements of multi-point sampling test and has very high spectrum test accuracy. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 The present invention is a flow chart of a method for preparing a YZZnAl4Cu1 spectral standard sample. DETAILED DESCRIPTION

[0028] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0029] Embodiment 1:

[0030] 1) Prepare the raw materials according to the following weight percentages: Al 4.1%, Cu 0.9%, Mg 0.045%, Fe0.01%, Pb 0.003%, Sn 0.0015%, Cd 0.003%, and the rest is Zn, each raw material is in the form of a small block or rod with a size not exceeding 20 mm, and the purity of each raw material is higher than 99.9%;

[0031] 2) Prepare a vacuum melting furnace, place the raw material Zn in the graphite crucible of the vacuum melting furnace, place other raw materials in the filling position of the vacuum melting furnace, turn on the heating device to heat the graphite crucible, set the temperature to 400°C, close the furnace chamber for vacuuming, and wait until the vacuum degree reaches 10 -3 Pa, the vacuum was stopped and high-purity argon was filled into the furnace to make the pressure inside the furnace reach 3×10 4 Pa, vacuumize again, and wait until the vacuum degree reaches 10 -3 Pa, stop evacuating and fill the furnace with high-purity argon gas to 3×10 4Pa, raise the temperature of the graphite crucible, set the temperature of the graphite crucible to 560°C, and wait for the raw material Zn in the graphite crucible to melt to form zinc liquid;

[0032] 3) adding raw materials of high melting point metals such as Cu and Fe into the graphite crucible from the filling position, starting to stir the alloy melt, adding raw material Al, and after Al is completely melted, adding raw materials Pb, Sn, Cd, and Mg into the graphite crucible from the filling position, and continuing to stir for 10 minutes to obtain zinc alloy liquid, pouring the zinc alloy liquid into a steel mold, the internal cavity of the steel mold is cylindrical, and after the zinc alloy liquid solidifies, removing the mold to obtain the zinc alloy billet;

[0033] 4) subjecting the zinc alloy blank to a first heat treatment, wherein the zinc alloy blank is kept at 250° C. for 3 hours and then cooled, and then the zinc alloy blank is kept at 100° C. for 5 hours and then cooled;

[0034] 5) Extruding the zinc alloy billet, keeping the zinc alloy billet and the extrusion die at 250° C. for 1 hour, the extrusion temperature is 200° C., the extrusion speed is 1 mm / s, the extrusion times are 5 times, and after processing, a zinc alloy spectrum standard sample with a length of 120 mm is obtained. At this time, the specification of the zinc alloy spectrum standard sample is φ60 mm×120 mm;

[0035] 6) The zinc alloy spectral standard sample was subjected to a second heat treatment, and the zinc alloy spectral standard sample was kept at 150°C for 8 hours and then cooled to obtain the final zinc alloy spectral standard sample. The zinc alloy spectral standard sample was processed by machining to make its specifications reach φ60mm×100mm, and samples were taken at different positions of the zinc alloy spectral standard sample. A disc was taken every 10mm along the axial direction of the cylinder, and 3 component test samples were taken along the radial direction of each disc. A total of 30 samples were taken, and the zinc alloy spectral standard sample was analyzed by ICP-OES. The component uniformity was tested, and the standard deviation SD of all measurement data was calculated and compared with the repeatability limit r of the measurement method. When 1.5SD≤r, the uniformity was considered qualified, and when 1.5SD>r, the uniformity was considered unqualified. The results are shown in the following table.

[0036]

[0037]

[0038] Embodiment 2:

[0039] 1) Prepare the raw materials according to the following weight percentages: AI 3.9%, Cu 0.7%, Mg 0.04%, Fe0.005%, Pb 0.002%, Sn 0.001%, Cd 0.002%, and the rest is Zn, each raw material is in the form of small blocks or small rods with a size not exceeding 20 mm, and the purity of each raw material is higher than 99.9%;

[0040] 2) Prepare a vacuum melting furnace, place the raw material Zn in the graphite crucible of the vacuum melting furnace, place other raw materials in the filling position of the vacuum melting furnace, turn on the heating device to heat the graphite crucible, set the temperature to 450°C, close the furnace chamber for vacuuming, and wait until the vacuum degree reaches 10 -3 Pa, the vacuum was stopped and high-purity argon was filled into the furnace to make the pressure inside the furnace reach 2×10 4 pa, perform vacuum operation again, and wait until the vacuum degree reaches 10 -3 When the vacuum is stopped, high-purity argon gas is filled into the furnace to reach 3×10 4 Pa, raise the temperature of the graphite crucible, set the temperature of the graphite crucible to 540°C, and wait for the raw material Zn in the graphite crucible to melt to form zinc liquid;

[0041] 3) Add raw materials such as Cu and Fe and other high melting point metals into the graphite crucible from the filling position, start stirring the alloy melt, add raw material Al, and after Al is completely melted, add raw materials Pb, Sn, Cd, and Mg into the graphite crucible from the filling position, continue stirring for 10 to 30 minutes, and obtain zinc alloy liquid, pour the zinc alloy liquid into a steel mold, the internal cavity of the steel mold is cylindrical, and after the zinc alloy liquid solidifies, remove the mold to obtain the zinc alloy billet;

[0042] 4) subjecting the zinc alloy blank to a first heat treatment, wherein the zinc alloy blank is kept at 300° C. for 5 hours and then cooled, and then the zinc alloy blank is kept at 120° C. for 10 hours and then cooled;

[0043] 5) Extruding the zinc alloy billet, keeping the zinc alloy billet and the extrusion die at 250° C. for 1 hour, the extrusion temperature is 200° C., the extrusion speed is 2 mm / s, the extrusion times are 3 times, and after processing, a zinc alloy spectrum standard sample with a length of 150 mm is obtained. At this time, the specification of the zinc alloy spectrum standard sample is φ60 mm×150 mm;

[0044] 6) The zinc alloy spectral standard sample was subjected to a second heat treatment, and the zinc alloy spectral standard sample was kept at 100°C for 15 hours and then cooled to obtain the final zinc alloy spectral standard sample. Samples were taken at different positions of the zinc alloy spectral standard sample, and a disc was taken every 10 mm along the axial direction of the cylinder. Three component test samples were taken along the radial direction of each disc, and samples were taken from a total of 45 positions. The zinc alloy spectral standard sample was subjected to component analysis by ICP-OES, and a component uniformity test was performed on it. The standard deviation SD of all measurement data was calculated and compared with the repeatability limit r of the measurement method. When 1.5SD≤r, the uniformity was considered to be qualified, and when 1.5SD>r, the uniformity was considered to be unqualified. The results are shown in the following table.

[0045]

[0046]

[0047] Embodiment 3:

[0048] 1) Prepare the raw materials according to the following weight percentages: Al 4.2%, Cu 1.0%, Mg 0.05%, Fe0.015%, Pb 0.004%, Sn 0.002%, Cd 0.004%, and the rest is Zn, each raw material is in the form of a small block or rod with a size not exceeding 20 mm, and the purity of each raw material is higher than 99.9%;

[0049] 2) Prepare a vacuum melting furnace, place the raw material Zn in the graphite crucible of the vacuum melting furnace, place other raw materials in the filling position of the vacuum melting furnace, turn on the heating device to heat the graphite crucible, set the temperature to 500°C, close the furnace chamber for vacuuming, and wait until the vacuum degree reaches 10 -3 Pa, the vacuum was stopped and high-purity argon was filled into the furnace to make the pressure inside the furnace reach 2×10 4 Pa, vacuumize again, and wait until the vacuum degree reaches 10 -3 Pa, stop evacuating and fill the furnace with high-purity argon gas to 3×10 4 Pa, raise the temperature of the graphite crucible, set the temperature of the graphite crucible to 520°C, and wait for the raw material Zn in the graphite crucible to melt to form zinc liquid;

[0050] 3) adding raw materials of high melting point metals such as Cu and Fe into the graphite crucible from the filling position, starting to stir the alloy melt, adding raw material Al, and after Al is completely melted, adding raw materials Pb, Sn, Cd, and Mg into the graphite crucible from the filling position, and continuing to stir for 15 minutes to obtain zinc alloy liquid, pouring the zinc alloy liquid into a steel mold, the internal cavity of the steel mold is cylindrical, and after the zinc alloy liquid solidifies, removing the mold to obtain the zinc alloy billet;

[0051] 4) subjecting the zinc alloy blank to a first heat treatment, wherein the zinc alloy blank is kept at 350° C. for 4 hours and then cooled, and then the zinc alloy blank is kept at 200° C. for 7 hours and then cooled;

[0052] 5) The zinc alloy billet is subjected to extrusion processing. The zinc alloy billet and the extrusion die are kept at 250°C for 1 hour. The extrusion temperature is 230°C, the extrusion speed is 5 mm / s, and the number of extrusions is 4. After processing, a zinc alloy spectrum standard sample with a length of 140 mm is obtained. At this time, the specification of the zinc alloy spectrum standard sample is φ60 mm×140 mm:

[0053] 6) The zinc alloy spectral standard sample was subjected to a second heat treatment, and the zinc alloy spectral standard sample was kept at 120°C for 10 hours and then cooled to obtain the final zinc alloy spectral standard sample. The zinc alloy spectral standard sample was processed by machining to make its specifications reach φ60mm×120mm, and samples were taken at different positions of the zinc alloy spectral standard sample. A disc was taken every 10mm along the axial direction of the cylinder, and 3 component test samples were taken along the radial direction of each disc. A total of 36 samples were taken, and the zinc alloy spectral standard sample was analyzed by ICP-OES. The component uniformity was tested, and the standard deviation SD of all measurement data was calculated and compared with the repeatability limit r of the measurement method. When 1.5SD≤r, the uniformity was considered qualified, and when 1.5SD>r, the uniformity was considered unqualified. The results are shown in the following table.

[0054]

[0055]

[0056] It can be seen from the test results of the zinc alloy spectral standard samples obtained in Example 1, Example 2 and Example 3 that the uniformity of the zinc alloy spectral standard samples is qualified, so the zinc alloy spectral standard samples prepared by the above method have very high spectral test accuracy.

[0057] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for preparing a YZZnAl4Cu1 spectrum standard sample, characterized in that: The steps include: 1) Prepare the raw materials according to the following weight percentages: Al 3.9-4.3%, Cu 0.7-1.1%, Mg 0.03-0.06%, Fe 0.005-0.020%, Pb 0.002-0.004%, Sn 0.001-0.002%, Cd 0.002-0.004%, and the rest is Zn; 2) Prepare a vacuum melting furnace, place the raw material Zn in the graphite crucible of the vacuum melting furnace, place other raw materials in the filling position of the vacuum melting furnace, turn on the heating device to heat the graphite crucible, close the furnace chamber for vacuuming, and wait until the vacuum degree reaches 10 -3 Pa, the vacuum was stopped and high-purity argon was filled into the furnace to make the pressure inside the furnace reach 2×10 4 ~3×10 4 Pa, vacuumize again, and wait until the vacuum degree reaches 10 -3 Pa, stop evacuating and fill the furnace with high-purity argon to a temperature of 2×10 4 ~3×10 4 Pa, raise the temperature of the graphite crucible, and wait for the raw material Zn in the graphite crucible to melt to form zinc liquid; 3) Add raw materials such as Cu and Fe and other high melting point metals into the graphite crucible from the filling position, start stirring the alloy melt, add raw material Al, and after Al is completely melted, add raw materials Pb, Sn, Cd, and Mg into the graphite crucible from the filling position, continue stirring for 10 to 30 minutes, and obtain zinc alloy liquid, pour the zinc alloy liquid into a steel mold, the internal cavity of the steel mold is cylindrical, and after the zinc alloy liquid solidifies, remove the mold to obtain the zinc alloy billet; 4) subjecting the zinc alloy blank to a first heat treatment; 5) Extruding the zinc alloy blank to obtain a zinc alloy spectrum standard sample with a length of 100 to 150 mm; 6) subjecting the zinc alloy spectrum standard sample to a second heat treatment to obtain a final zinc alloy spectrum standard sample; In the step 2), the temperature of the graphite crucible is 400-650°C; in the step 4), the zinc alloy blank is kept at 250-360°C for 3-20 hours and then cooled, and then the zinc alloy blank is kept at 100-200°C for 1-30 hours and then cooled; in the step 5), the extrusion temperature is 150-250°C, the extrusion speed is 1-5 mm / s, and the number of extrusions is 3-10 times; in the step 6), the zinc alloy spectrum standard sample is kept at 100-150°C for 1-30 hours and then cooled.

2. The method for preparing a YZZnAl4Cu1 spectrum standard sample according to claim 1, characterized in that: In the step 1), each raw material is in the form of a small block or a small rod with a size not exceeding 20 mm, and the purity of each raw material is higher than 99.9%.

3. The method for preparing a YZZnAl4Cu1 spectrum standard sample according to claim 1, characterized in that: In the step 6), samples are taken at different positions of the zinc alloy spectral standard sample, and the zinc alloy spectral standard sample is subjected to composition analysis by ICP-OES, and a composition uniformity test is performed on the sample. After the standard deviation SD of all measurement data is calculated, it is compared with the repeatability limit r of the measurement method. When 1.5SD≤r, the uniformity is considered to be qualified, and when 1.5SD>r, the uniformity is considered to be unqualified.

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