CN115343275A - YZZnAl 4 Cu 1 Preparation method of spectral standard sample - Google Patents
YZZnAl 4 Cu 1 Preparation method of spectral standard sample Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000003595 spectral effect Effects 0.000 title claims description 16
- 229910001297 Zn alloy Inorganic materials 0.000 claims abstract description 131
- 238000001228 spectrum Methods 0.000 claims abstract description 62
- 239000002994 raw material Substances 0.000 claims abstract description 55
- 239000011701 zinc Substances 0.000 claims abstract description 27
- 238000001125 extrusion Methods 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000003723 Smelting Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 11
- 229910052802 copper Inorganic materials 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 10
- 229910052745 lead Inorganic materials 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 5
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 35
- 229910002804 graphite Inorganic materials 0.000 claims description 35
- 239000010439 graphite Substances 0.000 claims description 35
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000000956 alloy Substances 0.000 claims description 16
- 229910045601 alloy Inorganic materials 0.000 claims description 15
- 229910000831 Steel Inorganic materials 0.000 claims description 11
- 239000010959 steel Substances 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 5
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims description 5
- 150000002739 metals Chemical class 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 13
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 24
- 238000012360 testing method Methods 0.000 description 12
- 238000001816 cooling Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- -1 ferrous metals Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C18/00—Alloys based on zinc
- C22C18/04—Alloys based on zinc with aluminium as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
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Abstract
The invention discloses YZZnAl 4 Cu 1 A preparation method of a spectrum standard sample belongs to the technical field of zinc alloy spectrum standard sample preparation, and comprises the following steps: preparing the following raw materials in percentage by weight: 3.9 to 4.3 percent of Al, 0.7 to 1.1 percent of Cu, 0.03 to 0.06 percent of Mg, 0.005 to 0.020 percent of Fe, 0.002 to 0.004 percent of Pb, 0.001 percent of Sn0.002 percent of Zn, 0.002 percent to 0.004 percent of Cd and the balance of Zn; the method comprises the steps of putting various raw materials weighed according to the mass percentage into a vacuum smelting furnace, firstly melting Zn raw materials, then adding Cu and Fe raw materials with high melting points, then adding Al raw materials, adding Pb, sn, cd and Mg raw materials after Al is melted, pouring the melted zinc alloy liquid into a die with a cylindrical cavity for solidification to obtain a zinc alloy blank, carrying out primary heat treatment on the zinc alloy blank, carrying out secondary heat treatment on the zinc alloy blank obtained by extrusion processing, and finally obtaining a zinc alloy spectrum standard sample with the component uniformity and the tissue uniformity meeting the requirements.
Description
Technical Field
The invention belongs to the technical field of preparation of zinc alloy spectrum standard samples, and particularly relates to YZZnAl 4 Cu 1 Preparation method of standard sample of spectrum.
Background
Among the non-ferrous metals, zinc has storage and consumer demand next to aluminum and copper. The pure zinc has lower mechanical property, so the application of the pure zinc as an engineering structure material is greatly limited. Usually, alloying elements such as Al, cu, mg and the like are added to improve the mechanical property, alloy fluidity and other problems of the zinc alloy material. The zinc alloy as a novel engineering material has the characteristics of corrosion resistance, low production cost, excellent casting performance, excellent wear resistance and friction reduction performance, excellent damping performance and the like, so that the zinc alloy has strong market competitiveness in the aspects of steel plating layers, hardware, bearings, gears and the like. Wherein YZZnAl 4 Cu 1 The zinc alloy has good tensile strength, hardness and wear resistance, and is widely used for automobile parts, building hardware, mechanical parts, electrical components, instrument parts and the like.
Because the performance of the zinc alloy is very sensitive to the components, zinc alloy production enterprises need to detect and analyze the components of the zinc alloy in real time in the production process, so that the quality of zinc alloy products is ensured. The direct-reading spectrometer is used as alloy component detection equipment which can test multiple elements simultaneously and is rapid, environment-friendly in use process and simple in operation, meets the requirements of zinc alloy production enterprises on the detection efficiency and the detection accuracy of zinc alloy products, and is widely applied to the development and production processes of the zinc alloy products. At present, a direct-reading spectrometer is provided with a test method curve of an alloy element to be tested when the direct-reading spectrometer leaves a factory, and only a standard sample which is close to the alloy element to be tested and has the same physical state is required to be configured to carry out single-point correction on the test method curve during actual use, so that the accuracy of a test result can be ensured. Because zinc alloy grades are multiple, and the composition difference of different grades of alloys is large, in order to ensure the accuracy of a test result, a standard sample needs to be respectively configured for each alloy.
At present, spectral standard samples with different zinc alloy grades in the market are not complete, and the standard samples in the market cannot meet YZZnAl in terms of components 4 Cu 1 The method has the advantages that the component detection of the alloy is required, and the measurement error of the commercially available standard sample on impurity elements in the zinc alloy is large, so that zinc alloy production enterprises often self-prepare zinc alloy spectrum standard samples, but the self-prepared standard samples often have the defects of large component nonuniformity, serious segregation of part of elements and the like, and the test result is easy to be inaccurate in actual use.
Disclosure of Invention
The invention aims to: for the purpose of understanding, no suitable standard sample is present in composition with YZZnAl 4 Cu 1 The alloy corresponds to the alloy, which causes the problem of poor spectral test accuracy, and provides a YZZnAl 4 Cu 1 Preparation method of standard sample of spectrum.
In order to achieve the purpose, the invention adopts the following technical scheme: YZZnAl 4 Cu 1 The preparation method of the spectrum standard sample is characterized by comprising the following steps: the method comprises the following steps:
1) Preparing the following raw materials in percentage by weight: 3.9 to 4.3 percent of Al, 0.7 to 1.1 percent of Cu, 0.03 to 0.06 percent of Mg, 0.005 to 0.020 percent of Fe, 0.002 to 0.004 percent of Pb, 0.001 to 0.002 percent of Sn, 0.002 to 0.004 percent of Cd and the balance of Zn, which is beneficial to realizing YZZnAl 4 Cu 1 Effective control of zinc alloy spectrum standard sample components and improvement of YZZnAl 4 Cu 1 The success rate of preparing a zinc alloy spectrum standard sample;
2) Preparing a vacuum smelting furnace, putting raw material Zn into a graphite crucible of the vacuum smelting furnace, putting other raw materials into a filling position of the vacuum smelting furnace, starting a heating device to heat the graphite crucible, sealing the furnace chamber to vacuumize, and when the vacuum degree reaches 10 -3 Stopping pumping when PaVacuum, and filling high-purity argon gas into the furnace to make the pressure in the furnace reach 2X 10 4 ～3×10 4 pa, performing vacuum pumping operation again until the vacuum degree reaches 10 -3 When Pa is needed, the vacuum pumping is stopped and high-purity argon is filled into the furnace to reach 2 multiplied by 10 4 ～3×10 4 Pa, raising the temperature of the graphite crucible, and melting raw material Zn in the graphite crucible to form a zinc liquid;
3) Adding high-melting-point metals such as Cu and Fe into a graphite crucible from a filling position, starting stirring an alloy melt, adding a raw material Al, after the Al is completely melted, adding raw materials Pb, sn, cd and Mg into the graphite crucible from the filling position, continuously stirring for 10-30 min to obtain a zinc alloy liquid, pouring the zinc alloy liquid into a steel mold, wherein a cavity inside the steel mold is cylindrical, and removing the mold after the zinc alloy liquid is solidified to obtain the zinc alloy, thereby being beneficial to reducing the oxidation degree of each alloy element and reducing YZZnAl 4 Cu 1 The contents of impurities and gases in the zinc alloy spectrum standard sample are beneficial to realizing the YZZnAl pair 4 Cu 1 Effective control of zinc alloy spectrum standard sample components to obtain YZZnAl with compact structure 4 Cu 1 A zinc alloy spectrum standard sample;
4) The zinc alloy blank is subjected to first heat treatment, so that YZZnAl can be remarkably improved 4 Cu 1 The plastic deformation capability of the zinc alloy spectrum standard sample reduces the strength and hardness of the zinc alloy spectrum standard sample, and is beneficial to follow-up YZZnAl 4 Cu 1 Extruding and processing a zinc alloy spectrum standard sample;
5) The zinc alloy blank is extruded to obtain a zinc alloy spectrum standard sample with the length of 100-150 mm, and the extrusion can remarkably crush dendritic crystals, effectively eliminate or reduce casting defects such as shrinkage porosity and the like, and improve the component uniformity and the tissue uniformity of the alloy;
6) The zinc alloy spectrum standard sample is subjected to secondary heat treatment to obtain a final zinc alloy spectrum standard sample, and YZZnAl can be effectively eliminated 4 Cu 1 The internal stress of the zinc alloy spectrum standard sample caused by extrusion processing can be eliminated, and the microstructure appearance and the macroscopic external deformation of the zinc alloy spectrum standard sample in the subsequent long-term use process can be eliminatedAnd (4) transforming.
As a further description of the above technical solution:
in the step 1), each raw material is in a small block shape or a small rod shape with the size not more than 20mm, and the purity of each raw material is higher than 99.9%.
As a further description of the above technical solution:
in the step 2), the temperature of the graphite crucible is 400-650 ℃.
As a further description of the above technical solution:
in the step 4), the zinc alloy blank is cooled after being kept at 250-360 ℃ for 3-20 hours, and then the zinc alloy blank is cooled after being kept at 100-200 ℃ for 1-30 hours.
As a further description of the above technical solution:
in the step 5), the extrusion temperature is 150-250 ℃, the extrusion speed is 1-5 mm/s, and the extrusion times are 3-10.
As a further description of the above technical solution:
in the step 6), the zinc alloy spectrum standard sample is cooled after being kept at the temperature of 100-150 ℃ for 1-30 hours.
As a further description of the above technical solution:
in the step 6), sampling is carried out at different positions of the zinc alloy spectrum standard sample, the ICP-OES is adopted to carry out component analysis on the zinc alloy spectrum standard sample, component uniformity detection is carried out on the zinc alloy spectrum standard sample, after the standard deviation SD of all measurement data is calculated, the standard deviation SD is compared with the repeatability limit r of the measurement method, when the SD is not less than 1.5 and is not more than r, the uniformity is considered to be qualified, and when the SD is more than 1.5 and is not more than r, the uniformity is considered to be unqualified.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
according to the invention, various raw materials weighed according to the mass percentage are put into a vacuum smelting furnace, a Zn raw material is firstly melted, cu and Fe raw materials with high melting points are then added, an Al raw material is then added, pb, sn, cd and Mg raw materials are added after the Al is melted, the melted zinc alloy liquid is poured into a die with a cylindrical cavity and is solidified to obtain a zinc alloy blank, the zinc alloy blank is subjected to first heat treatment, then the zinc alloy blank is subjected to extrusion processing, the zinc alloy blank obtained by the extrusion processing is subjected to second heat treatment, and finally a zinc alloy spectral standard sample with the composition uniformity and the tissue uniformity meeting the requirements is obtained, so that the multipoint sampling test is met, and the spectrum test accuracy is very high.
Drawings
FIG. 1 shows YZZnAl 4 Cu 1 Flow chart of the method for preparing the spectral standard sample.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
1) Preparing the following raw materials in percentage by weight: 4.1% of Al, 0.9% of Cu, 0.045% of Mg, 0.01% of Fe, 0.003% of Pb, 0.0015% of Sn, 0.003% of Cd and the balance of Zn, wherein each raw material is in a small block shape or a small rod shape with the size not exceeding 20mm, and the purity of each raw material is higher than 99.9%;
2) Preparing a vacuum smelting furnace, putting raw material Zn into a graphite crucible of the vacuum smelting furnace, putting other raw materials into a filling position of the vacuum smelting furnace, starting a heating device to heat the graphite crucible, setting the temperature at 400 ℃, sealing the furnace chamber to vacuumize, and when the vacuum degree reaches 10 -3 Stopping vacuumizing when Pa, and filling high-purity argon into the furnace to make the pressure in the furnace reach 3 x 10 4 Pa, performing vacuum pumping again until the vacuum degree reaches 10 -3 When Pa is needed, the vacuum pumping is stopped and high-purity argon is filled into the furnace to reach 3 multiplied by 10 4 Pa, raising the temperature of the graphite crucible, setting the temperature of the graphite crucible to be 560 ℃, and melting raw material Zn in the graphite crucible to form a zinc liquid;
3) Adding high-melting-point metals such as Cu and Fe serving as raw materials into a graphite crucible from a filling position, starting stirring an alloy melt, adding Al serving as a raw material, adding Pb, sn, cd and Mg serving as raw materials into the graphite crucible from the filling position after the Al is completely melted, continuously stirring for 10min to obtain a zinc alloy liquid, pouring the zinc alloy liquid into a steel mould, wherein a cavity inside the steel mould is cylindrical, and removing the mould after the zinc alloy liquid is solidified to obtain a zinc alloy blank;
4) Carrying out first heat treatment on the zinc alloy blank, carrying out heat preservation on the zinc alloy blank at 250 ℃ for 3 hours, then cooling the zinc alloy blank, and carrying out heat preservation on the zinc alloy blank at 100 ℃ for 5 hours, and then cooling the zinc alloy blank;
5) Performing extrusion processing on the zinc alloy blank, keeping the temperature of the zinc alloy blank and an extrusion die at 250 ℃ for 1 hour, wherein the extrusion temperature is 200 ℃, the extrusion speed is 1mm/s, the extrusion times are 5 times, and a zinc alloy spectral standard sample with the length of 120mm is obtained after processing, wherein the specification of the zinc alloy spectral standard sample is phi 60mm multiplied by 120mm;
6) Performing secondary heat treatment on a zinc alloy spectrum standard sample, keeping the zinc alloy spectrum standard sample at 150 ℃ for 8 hours, cooling to obtain a final zinc alloy spectrum standard sample, processing the zinc alloy spectrum standard sample by utilizing a machine to enable the specification of the zinc alloy spectrum standard sample to reach phi 60mm multiplied by 100mm, sampling at different positions of the zinc alloy spectrum standard sample, taking 1 wafer every 10mm along the axial direction of a cylinder, taking 3 component test samples along the radial direction of each 1 wafer, taking 30 position samples in total, performing component analysis on the zinc alloy spectrum standard sample by adopting ICP-OES, performing component uniformity detection on the zinc alloy spectrum standard sample, calculating the standard deviation SD of all measured data, comparing the standard deviation SD with the repeatability limit r of a measuring method, when the SD is not less than 1.5 and not more than r, considering that the uniformity is qualified, when the SD is more than 1.5 and not more than r, considering that the uniformity is unqualified, and obtaining the following results.
Example 2:
1) Preparing the following raw materials in percentage by weight: AI 3.9%, cu 0.7%, mg 0.04%, fe 0.005%, pb 0.002%, sn 0.001%, cd 0.002%, and Zn in balance, wherein each raw material is in the form of small block or rod with size not more than 20mm, and the purity of each raw material is higher than 99.9%;
2) Preparing a vacuum smelting furnace, putting raw material Zn into a graphite crucible of the vacuum smelting furnace, putting other raw materials into a filling position of the vacuum smelting furnace, starting a heating device to heat the graphite crucible, setting the temperature to be 450 ℃, sealing the furnace chamber to vacuumize, and when the vacuum degree reaches 10 -3 Stopping vacuumizing when Pa is reached, and filling high-purity argon gas into the furnace to make the pressure in the furnace reach 2 x 10 4 pa, performing vacuum pumping operation again until the vacuum degree reaches 10 -3 When pa, stopping vacuumizing and filling high-purity argon into the furnace to reach 3 multiplied by 10 4 Pa, raising the temperature of the graphite crucible, setting the temperature of the graphite crucible to be 540 ℃, and melting raw material Zn in the graphite crucible to form a zinc liquid;
3) Adding high-melting-point metals such as Cu and Fe serving as raw materials into a graphite crucible from a filling position, starting stirring an alloy melt, adding Al serving as a raw material, adding Pb, sn, cd and Mg serving as raw materials into the graphite crucible from the filling position after the Al is completely melted, continuously stirring for 10-30 min to obtain a zinc alloy liquid, pouring the zinc alloy liquid into a steel mould, wherein a cavity in the steel mould is cylindrical, and removing the mould after the zinc alloy liquid is solidified to obtain a zinc alloy blank;
4) Carrying out first heat treatment on the zinc alloy blank, carrying out heat preservation on the zinc alloy blank at 300 ℃ for 5 hours, then cooling the zinc alloy blank, and carrying out heat preservation on the zinc alloy blank at 120 ℃ for 10 hours, and then cooling the zinc alloy blank;
5) Performing extrusion processing on the zinc alloy blank, keeping the temperature of the zinc alloy blank and an extrusion die at 250 ℃ for 1 hour, wherein the extrusion temperature is 200 ℃, the extrusion speed is 2mm/s, the extrusion times are 3 times, and a zinc alloy spectral standard sample with the length of 150mm is obtained after processing, wherein the specification of the zinc alloy spectral standard sample is phi 60mm multiplied by 150mm;
6) Performing secondary heat treatment on a zinc alloy spectrum standard sample, keeping the temperature of the zinc alloy spectrum standard sample at 100 ℃ for 15 hours, cooling to obtain a final zinc alloy spectrum standard sample, sampling at different positions of the zinc alloy spectrum standard sample, taking 1 wafer every 10mm along the axial direction of a cylinder, taking 3 component test samples along the radial direction of each 1 wafer, taking samples at 45 positions in total, performing component analysis on the zinc alloy spectrum standard sample by adopting ICP-OES, performing component uniformity detection on the zinc alloy spectrum standard sample, calculating the standard deviation SD of all measurement data, comparing the standard deviation SD with the repeatability limit r of the measurement method, determining that the uniformity is qualified when the SD is less than or equal to 1.5 and r, determining that the uniformity is unqualified when the SD is more than 1.5 and obtaining the following results.
Example 3:
1) Preparing the following raw materials in percentage by weight: 4.2% of Al, 1.0% of Cu, 0.05% of Mg, 0.015% of Fe, 0.004% of Pb, 0.002% of Sn, 0.004% of Cd and the balance of Zn, wherein each raw material is in a small block shape or a small rod shape with the size not more than 20mm, and the purity of each raw material is higher than 99.9%;
2) Preparing a vacuum smelting furnace, placing raw material Zn in a graphite crucible of the vacuum smelting furnace, placing other raw materials in a filling position of the vacuum smelting furnace, starting a heating device to heat the graphite crucible, setting the temperature at 500 ℃, sealing the furnace chamber to vacuumize, and when the vacuum degree reaches 10 -3 Stopping vacuumizing when Pa is reached, and filling high-purity argon gas into the furnace to make the pressure in the furnace reach 2 x 10 4 Pa, performing vacuum pumping again until the vacuum degree reaches 10 -3 When Pa is needed, the vacuum pumping is stopped and high-purity argon is filled into the furnace to reach 3 multiplied by 10 4 Pa, raising the temperature of the graphite crucible, setting the temperature of the graphite crucible to 520 ℃, and melting raw material Zn in the graphite crucible to form a zinc liquid;
3) Adding high-melting-point metals such as Cu and Fe serving as raw materials into a graphite crucible from a filling position, starting stirring an alloy melt, adding Al serving as a raw material, adding Pb, sn, cd and Mg serving as raw materials into the graphite crucible from the filling position after the Al is completely melted, continuously stirring for 15min to obtain a zinc alloy liquid, pouring the zinc alloy liquid into a steel mould, wherein a cavity inside the steel mould is cylindrical, and removing the mould after the zinc alloy liquid is solidified to obtain a zinc alloy blank;
4) Carrying out first heat treatment on the zinc alloy blank, carrying out heat preservation on the zinc alloy blank at 350 ℃ for 4 hours, then cooling, and carrying out heat preservation on the zinc alloy blank at 200 ℃ for 7 hours, and then cooling;
5) Performing extrusion processing on the zinc alloy blank, keeping the temperature of the zinc alloy blank and an extrusion die at 250 ℃ for 1 hour, wherein the extrusion temperature is 230 ℃, the extrusion speed is 5mm/s, the extrusion times are 4 times, and obtaining a zinc alloy spectral standard sample with the length of 140mm after processing, wherein the specification of the zinc alloy spectral standard sample is phi 60mm, 140mm and
6) Performing secondary heat treatment on a zinc alloy spectrum standard sample, preserving the heat of the zinc alloy spectrum standard sample at 120 ℃ for 10 hours, cooling to obtain a final zinc alloy spectrum standard sample, processing the zinc alloy spectrum standard sample by utilizing a machine to enable the specification of the zinc alloy spectrum standard sample to reach phi 60mm multiplied by 120mm, sampling at different positions of the zinc alloy spectrum standard sample, taking 1 wafer every 10mm along the axial direction of a cylinder, taking 3 component test samples along the radial direction of each 1 wafer, taking 36 position samples in total, performing component analysis on the zinc alloy spectrum standard sample by adopting ICP-OES, performing component uniformity detection on the zinc alloy spectrum standard sample, calculating the standard deviation SD of all measured data, comparing the standard deviation SD with the repeatability limit r of a measuring method, when the SD is not less than 1.5 and not more than r, considering that the uniformity is qualified, when the SD is more than 1.5 and not more than r, considering that the uniformity is unqualified, and obtaining the following results.
From the test results of the zinc alloy spectrum standard samples obtained in the example 1, the example 2 and the example 3, it can be seen that the uniformity of the zinc alloy spectrum standard sample is qualified, so that the zinc alloy spectrum standard sample prepared by the method has very high spectrum test accuracy.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (7)
1. YZZnAl 4 Cu 1 The preparation method of the spectrum standard sample is characterized by comprising the following steps: the method comprises the following steps:
1) Preparing the following raw materials in percentage by weight: 3.9 to 4.3 percent of Al, 0.7 to 1.1 percent of Cu, 0.03 to 0.06 percent of Mg, 0.005 to 0.020 percent of Fe, 0.002 to 0.004 percent of Pb, 0.001 to 0.002 percent of Sn, 0.002 to 0.004 percent of Cd and the balance of Zn;
2) Preparing a vacuum smelting furnace, putting raw material Zn into a graphite crucible of the vacuum smelting furnace, putting other raw materials into a filling position of the vacuum smelting furnace, starting a heating device to heat the graphite crucible, sealing the furnace chamber to vacuumize, and when the vacuum degree reaches 10 -3 When pa, stopping vacuumizing, and filling high-purity argon into the furnace to make the pressure in the furnace reach 2X 10 4 ～3×10 4 pa, performing vacuum pumping operation again until the vacuum degree reaches 10 -3 When Pa is needed, the vacuum pumping is stopped and high-purity argon is filled into the furnace to reach 2 multiplied by 10 4 ～3×10 4 Pa, raising the temperature of the graphite crucible, and melting raw material Zn in the graphite crucible to form a zinc liquid;
3) Adding high-melting-point metals such as Cu and Fe serving as raw materials into a graphite crucible from a filling position, starting stirring an alloy melt, adding Al serving as a raw material, after the Al is completely melted, adding Pb, sn, cd and Mg serving as raw materials into the graphite crucible from the filling position, continuously stirring for 10-30 min to obtain a zinc alloy liquid, pouring the zinc alloy liquid into a steel mold, wherein a cavity in the steel mold is cylindrical, and removing the mold after the zinc alloy liquid is solidified to obtain a zinc alloy blank;
4) Carrying out first heat treatment on the zinc alloy blank;
5) Extruding the zinc alloy blank to obtain a zinc alloy spectrum standard sample with the length of 100-150 mm;
6) And carrying out secondary heat treatment on the zinc alloy spectrum standard sample to obtain the final zinc alloy spectrum standard sample.
2. A YZZnAl according to claim 1 4 Cu 1 The preparation method of the spectrum standard sample is characterized in that in the step 1), each raw material is in a small block shape or a small rod shape with the size not exceeding 20mm, and the purity of each raw material is higher than 99.9%.
3. A YZZnAl according to claim 1 4 Cu 1 The preparation method of the spectrum standard sample is characterized in that in the step 2), the temperature of the graphite crucible is 400-650 ℃.
4. A YZZnAl according to claim 1 4 Cu 1 The preparation method of the spectrum standard sample is characterized in that in the step 4), the zinc alloy blank is cooled after being kept at 250-360 ℃ for 3-20 hours, and then the zinc alloy blank is kept at 100-200 ℃ for 1-30 hours and then cooled.
5. A YZZnAl according to claim 1 4 Cu 1 The preparation method of the spectrum standard sample is characterized in that in the step 5), the extrusion temperature is 150-250 ℃, the extrusion speed is 1-5 mm/s, and the extrusion times are 3-10.
6. A YZZnAl according to claim 1 4 Cu 1 The preparation method of the spectrum standard sample is characterized in that in the step 6), the zinc alloy spectrum standard sample is cooled after being kept at the temperature of 100-150 ℃ for 1-30 hours.
7. A YZZnAl according to claim 1 4 Cu 1 The preparation method of the spectral standard sample is characterized in that in the step 6), sampling is carried out at different positions of the zinc alloy spectral standard sample, ICP-OES is adopted to carry out component analysis on the zinc alloy spectral standard sample, component uniformity detection is carried out on the zinc alloy spectral standard sample, after the standard deviation SD of all measured data is calculated, the standard deviation SD is compared with the repeatability limit r of the measuring method, when the SD is not less than 1.5 and not more than r, the uniformity is considered to be qualified, and when the SD is more than 1.5 and not more than r, the uniformity is considered to be unqualified.
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