CN110044763B - Method for detecting content of nitric acid insoluble substances in high-purity silver ingot - Google Patents
Method for detecting content of nitric acid insoluble substances in high-purity silver ingot Download PDFInfo
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- CN110044763B CN110044763B CN201910369497.7A CN201910369497A CN110044763B CN 110044763 B CN110044763 B CN 110044763B CN 201910369497 A CN201910369497 A CN 201910369497A CN 110044763 B CN110044763 B CN 110044763B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 196
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 196
- 239000004332 silver Substances 0.000 title claims abstract description 196
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 91
- 239000000126 substance Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000001514 detection method Methods 0.000 claims abstract description 52
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000002844 melting Methods 0.000 claims abstract description 22
- 230000008018 melting Effects 0.000 claims abstract description 22
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 238000010309 melting process Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000007770 graphite material Substances 0.000 claims description 12
- 239000012535 impurity Substances 0.000 abstract description 19
- 239000002699 waste material Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 7
- 239000012528 membrane Substances 0.000 description 7
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 238000005553 drilling Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910052745 lead Inorganic materials 0.000 description 4
- 229910052711 selenium Inorganic materials 0.000 description 4
- 229910052714 tellurium Inorganic materials 0.000 description 4
- 229910052797 bismuth Inorganic materials 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000011978 dissolution method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012982 microporous membrane Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
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- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
- G01N15/0606—Investigating concentration of particle suspensions by collecting particles on a support
- G01N15/0618—Investigating concentration of particle suspensions by collecting particles on a support of the filter type
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Abstract
The application discloses a method for detecting the content of nitric acid insoluble substances in a high-purity silver ingot, belongs to the technical field of impurity detection, and solves the problems that the detection cost is high and the detection is inaccurate easily caused by the existing method for detecting the content of the nitric acid insoluble substances in the high-purity silver ingot, the mass percentage content of silver in the high-purity silver ingot is not less than 99.99 percent, and the detection method comprises the following steps: melting a high-purity silver ingot in a protective gas atmosphere, and moving the high-purity silver ingot intermittently in the melting process; cooling after the melting is finished to obtain a discharged silver ingot, wherein a foreign object area and a mirror surface bright area are formed on the upper surface of the discharged silver ingot; and determining the content of the nitric acid insoluble substances in the high-purity silver ingot according to the ratio of the area of the foreign material area to the mass of the high-purity silver ingot. The detection method is simple and convenient, and waste of silver ingots is prevented.
Description
Technical Field
The application relates to the technical field of impurity detection, in particular to a method for detecting the content of nitric acid insoluble substances in high-purity silver ingots.
Background
In GB/T4135-2016 silver ingot, the impurity contents of Cu, Pb, Fe, Sb, Se, Te, Bi, Pd and the total impurity of the silver ingot are regulated, and the silver ingot is divided into three brands of IC-Ag99.99, IC-Ag99.95 and IC-Ag99.90 according to the total impurity, wherein the IC-Ag99.99 is called as a high-purity silver ingot in the application.
However, when many enterprises purchase high-purity silver ingots, only the elements of Cu, Pb, Fe, Sb, Se, Te, Bi, and Pd are detected, and if the detection is qualified, the high-purity silver ingots are put into use, and the detection of impurities insoluble in nitric acid in the high-purity silver ingots is ignored. For this further analysis, the high-purity silver ingots were sampled by drilling, dissolved with analytically pure nitric acid, and the silver nitrate solution was filtered through a microporous filter membrane, whereupon the appearance of gray or yellow foreign matter was found. As a control, no foreign matter was found on the microporous membrane after an equal amount of analytically pure nitric acid was filtered through the microporous membrane. In view of this situation, it can be deduced that the existence of the nitric acid insoluble substance in the high-purity silver ingot affects the purity of the high-purity silver ingot. The content requirement of impurity elements such as Cu, Pb, Fe, Sb, Se, Te, Bi and Pd is subtracted from the total impurity content of the IC-Ag99.99 high-purity silver ingot, so that the impurity content of the nitric acid insoluble substance is not allowed to exceed 0.0014% (14ppm, ppm is parts per million), and if the content of the nitric acid insoluble substance exceeds 14ppm, the total impurity content does not meet the national standard requirement of GB/T4135-2016 silver ingot.
Because the impurity distribution in the silver ingot is not very uniform, if the drilling sampling detection is less, the content of the nitric acid insoluble substance in the high-purity silver ingot can not be accurately measured, so that whether the impurity sum of the high-purity silver ingot meets the national standard or not can not be accurately judged. However, if the content of the nitric acid insoluble matter in the high-purity silver ingots is detected by dissolving the high-purity silver ingots by using more than 5kg of nitric acid, a large amount of nitric acid is used in the detection process, and the high-purity silver ingots cannot be used after being dissolved, so that the detection cost is extremely high.
At present, no detection method aiming at the content of the nitric acid insoluble substances exists in the national standard GB/T4135-2016 silver ingot, and various documents and patents are not related.
Disclosure of Invention
The embodiment of the application provides a method for detecting the content of nitric acid insoluble substances in high-purity silver ingots, and solves the problems of high detection cost and inaccurate detection result of the existing method for detecting impurities in the silver ingots.
In order to achieve the above purpose, the present application mainly provides the following technical solutions:
the embodiment of the application provides a method for detecting the content of nitric acid insoluble substances in a high-purity silver ingot, wherein the mass percentage of silver in the high-purity silver ingot is not less than 99.99%, and the detection method comprises the following steps:
melting a high-purity silver ingot in a protective gas atmosphere, and moving the high-purity silver ingot intermittently in the melting process;
cooling after the melting is finished to obtain a discharged silver ingot, wherein a foreign material area and a mirror surface bright area are formed on the upper surface of the discharged silver ingot;
and determining the content of the nitric acid insoluble substances in the high-purity silver ingot according to the ratio of the area of the foreign material area to the mass of the high-purity silver ingot.
Preferably, the detection method further comprises: determining the area of a foreign material area formed by the high-purity silver ingots with known nitric acid insoluble content, the quality of the known high-purity silver ingots and the linear relation among the nitric acid insoluble content, and determining the content of the nitric acid insoluble in the high-purity silver ingots to be measured according to the linear relation.
Preferably, the thickness of the discharged silver ingot is 13-15 mm.
Preferably, the content of the nitric acid insoluble substances in the high-purity silver ingot is determined according to the ratio of the area of the foreign material area to the area of the upper surface of the discharged silver ingot.
Preferably, the upper surface of the discharged silver ingot is rectangular.
Preferably, the melting temperature is 1000-.
Preferably, the melting temperature is 1100 ± 10 ℃.
Preferably, the melting time is 1 to 3 hours.
Preferably, the intermittent movement adopts a mode that the single movement time is 20-40min, the single movement speed is 4-6cm/min, and the single intermittent time is 20-40 s.
Preferably, the high-purity silver ingot is melted in a high-temperature furnace, and the intermittent movement of the high-purity silver ingot is to place the high-purity silver ingot into a graphite material boat and intermittently push the graphite material boat from an inlet of the high-temperature furnace to an outlet of the high-temperature furnace through a push rod in the high-temperature furnace.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
the method for detecting the impurities of the silver ingots by changing the conventional method for detecting the impurities of the silver ingots by using the nitric acid dissolution method does not need to dissolve the silver ingots, the silver ingots only need to be melted, whether the content of nitric acid insoluble substances in the detected high-purity silver ingots meets the requirements of national standards can be simply and visually judged, the use of nitric acid is avoided, the silver ingots discharged after detection can be put into use again, the problem of overhigh cost caused by the nitric acid dissolution method is solved, and compared with the drilling sampling method, the detection result of the detection method is more reliable. The method for detecting the content of the nitric acid insoluble substances in the high-purity silver ingots has the advantages that whether the content of the nitric acid insoluble substances in the high-purity silver ingots meets the national standard requirement or not is judged in the production stage, high detection precision is not needed, and only whether the content of the nitric acid insoluble substances in the high-purity silver ingots is below 14ppm or not is judged.
Drawings
FIG. 1 is a graph showing the effect of measuring the area ratio of a foreign object region to the upper surface of a discharged silver ingot in the detection method according to an embodiment of the present invention;
FIG. 2 is a graph showing the effect of measuring the area ratio of the foreign material area to the upper surface of the discharged silver ingot in the detection method according to still another embodiment of the present application;
FIG. 3 is a graph showing the effect of measuring the area ratio of the foreign material region to the upper surface of the discharged silver ingot in the detection method according to still another embodiment of the present application;
FIG. 4 is a graph showing the effect of measuring the area ratio of the foreign material region to the upper surface of the discharged silver ingot in the detection method according to still another embodiment of the present application;
FIG. 5 is a graph showing the effect of measuring the area ratio of the foreign material region to the upper surface of the discharged silver ingot in the detection method according to still another embodiment of the present application;
FIG. 6 is a graph showing the effect of measuring the area ratio of the foreign material area to the upper surface of the discharged silver ingot in the detection method according to yet another embodiment of the present application.
Detailed Description
In order to facilitate the understanding of the scheme of the present application by those skilled in the art, the following further description is provided with specific examples, and it should be understood that the examples are illustrative of the scheme of the present application and are not intended to limit the scope of the present application.
Through a large amount of experimental researches, the applicant finds that 0.1kg, 0.5kg, 1kg, 2kg, 4kg, 5kg, 6kg and 7kg of high-purity silver ingots with the specification of 30kg are respectively sampled, the sampled weight deviation is within 10g, and the following detection is respectively carried out: dissolving a sample by using nitric acid, drying impurities on the microporous filter membrane and the filter membrane together after filtering a silver nitrate solution by using the microporous filter membrane, weighing the weight difference of the microporous filter membrane before and after use, determining the content of the nitric acid insoluble impurities, and obtaining data shown in table 1:
TABLE 1
From the data, when the sampling is more than 5kg, the detection data is stable, the content of the nitric acid insoluble substances in the high-purity silver ingot can be more accurately judged, and whether the purity of the high-purity silver ingot meets the national standard requirement or not can be more accurately judged by combining the detection data of the elements of Cu, Pb, Fe, Sb, Se, Te, Bi and Pd. If the method for detecting the nitric acid insoluble substances in the high-purity silver ingots is a method for dissolving the high-purity silver ingots by using more than 5kg of nitric acid, a large amount of nitric acid is used in the detection process, and the high-purity silver ingots cannot be used after being dissolved, so that the detection cost is extremely high.
The applicant also found through research that: sampling a high-purity silver ingot, dissolving the silver ingot by using nitric acid, filtering silver nitrate by using a microporous filter membrane, drying a nitric acid insoluble substance and the filter membrane, and detecting by using a scanning electron microscope to find that main components of the nitric acid insoluble substance are alumina, silica, tin oxide and the like.
According to the properties of the impurities, the embodiment of the application provides a set of methods for measuring the content of the nitric acid insoluble substances in the high-purity silver ingots, which specifically comprises the following steps:
a method for detecting the content of nitric acid insoluble substances in a high-purity silver ingot, wherein the mass percentage of silver in the high-purity silver ingot is not less than 99.99%, comprises the following steps:
melting high-purity silver ingots in a protective gas atmosphere, and intermittently moving the high-purity silver ingots in the melting process;
cooling after the melting is finished to obtain a discharged silver ingot, wherein a foreign material area and a mirror surface bright area are formed on the upper surface of the discharged silver ingot;
and determining the content of the nitric acid insoluble substances in the high-purity silver ingot according to the ratio of the area of the foreign material area to the mass of the high-purity silver ingot.
Here, it is to be noted that: because the melting point of the nitric acid insoluble substance is high, the viscosity of the silver melt slurry is reduced after the high-purity silver ingot is melted in the high-temperature furnace, and therefore the nitric acid insoluble substance floats upwards under the action of wettability and density difference. Meanwhile, the high-purity silver ingot intermittently moves in the melting process, and under the inertia action of intermittent pushing and stopping, the nitric acid insoluble substances floating on the surface of the silver melt slurry can be gathered on one side. At the same temperature, the tension of the surface of the silver molten paste is basically equivalent, so the spreading thickness of the nitric acid insoluble substances on the surface of the silver molten paste is more uniform. When the silver molten slurry is solidified, the thickness of the nitric acid insoluble substance is uniformly deposited on the upper surface of the discharged silver ingot, and a mirror bright area without impurities and a foreign object area containing the nitric acid insoluble substance are formed on the upper surface of the discharged silver ingot. The thickness of the foreign object area containing the nitric acid insoluble substances is constant, so that the area of the formed foreign object area is in direct proportion to the absolute content of the nitric acid insoluble substances in the high-purity silver ingot, the linear relation among the area of the high-purity silver ingot with the known content of the nitric acid insoluble substances, the mass of the known high-purity silver ingot and the content of the nitric acid insoluble substances can be determined, and then according to the linear relation, the content of the nitric acid insoluble substances in the high-purity silver ingot to be determined can be determined by measuring the ratio of the area of the high-purity silver ingot to be determined, which forms the foreign object area, to the mass of the high-purity silver ingot to be determined. According to the detection method, the silver ingots do not need to be dissolved, and the content of the nitric acid insoluble substances in the high-purity silver ingots can be detected whether to meet the national standard requirement or not only by melting the silver ingots; in addition, when the detection of the nitric acid insoluble substances in the high-purity silver ingots is carried out, the use of nitric acid is avoided, the silver ingots discharged after detection can be put into use again, the problem of overhigh cost caused by a nitric acid dissolving method is solved, and compared with drilling sampling, the detection result of the detection method is more accurate.
The scheme can realize accurate detection of the content of the nitric acid insoluble substances in the high-purity silver ingots, and can reduce the waste of the silver ingots; preferred embodiments are given below on this basis:
preferably, the thickness of the discharged silver ingot is 13 to 15 mm. When the detection method provided by the embodiment of the application is used for detecting the content of the nitric acid insoluble substances in the high-purity silver ingots, the absolute content of the nitric acid insoluble substances in the high-purity silver ingots is different due to different qualities of the high-purity silver ingots, different areas forming the foreign object areas on the upper surfaces of the discharged silver ingots are different, and the foreign object areas can completely cover the upper surfaces of the discharged silver ingots, so that the thickness of the nitric acid insoluble substances in the foreign object areas cannot be kept stable, and the detection method provided by the embodiment of the application is not applicable. According to the method, the thickness range of the discharged silver ingots in the detection method is obtained by combining factors such as the detectable range of the detection method, according to the approximate content of the nitric acid insoluble substances in the high-purity silver ingots, when the thickness of the discharged silver ingots is 13-15mm, the foreign object area and the mirror surface bright area exist on the upper surface of the discharged silver ingots, and the content of the nitric acid insoluble substances can be detected by adopting the detection method of the application for the high-purity silver ingots with any quality. In addition, high-purity silver ingots are generally placed in a graphite material boat for high-temperature melting, the surface area of the discharged silver ingots can be rapidly calculated through the thickness of the discharged silver ingots and the quality of the discharged silver ingots, and therefore the size of the required graphite material boat can be known, repeated detection operation is avoided, and detection efficiency and detection success rate are improved. It should be noted that the thickness of the discharged silver ingot in the present scheme refers to the thickness of the discharged silver ingot in a cylindrical shape, and for convenience of measurement, in some embodiments of the present application, the discharged silver ingot is a rectangular parallelepiped or a square, but may be another cylindrical shape.
Preferably, the content of the nitric acid insoluble matter in the high purity silver ingot is determined based on the ratio of the area of the foreign material region to the area of the upper surface of the discharged silver ingot. According to the scheme, when the thickness of the discharged silver ingot is kept constant, the ratio of the area of the foreign object area on the discharged silver ingot to the area of the upper surface of the discharged silver ingot is in direct proportion to the mass percentage content of the nitric acid insoluble substances in the high-purity silver ingot, so that the corresponding relation between the ratio of the area of the foreign object area to the area of the upper surface of the discharged silver ingot and the mass percentage content of the nitric acid insoluble substances after the high-purity silver ingot with the known content of the nitric acid insoluble substances is melted can be determined, and then according to the corresponding relation, the content of the nitric acid insoluble substances in the high-purity silver ingot to be determined can be determined by measuring the ratio of the area of the foreign object area formed by the high-purity silver ingot to be determined to the area of the upper surface of the discharged silver ingot.
After a large amount of research and experiments, the applicant obtains the corresponding relation between the ratio of the area of the foreign matter region to the upper surface area of the discharged silver ingot measured by the detection method and the content of the nitric acid insoluble substances in the high-purity silver ingot.
Taking a high-purity silver ingot with 5 +/-0.1 kg of dissolved nitric acid as an example, the content of the nitric acid insoluble substances in the high-purity silver ingot is obtained by using a filtering-drying-weighing method, and the content of the nitric acid insoluble substances in the high-purity silver ingot can be judged to be unqualified when the content exceeds 14ppm, and the data is shown in table 2:
table 2.
In the embodiment, the silver ingot is not required to be dissolved, the silver ingot is only required to be melted, and whether the content of the nitric acid insoluble substance in the detected high-purity silver ingot meets the national standard requirement or not can be simply and visually judged by measuring the area ratio of the foreign object area containing the nitric acid insoluble substance to the upper surface of the discharged silver ingot; the method for detecting the content of the nitric acid insoluble substances in the high-purity silver ingots has the advantages that whether the content of the nitric acid insoluble substances in the high-purity silver ingots meets the national standard requirements or not is judged, high detection precision is not needed, and only whether the content of the nitric acid insoluble substances in the high-purity silver ingots is below 14ppm or not is judged.
In some embodiments of the present application, the upper surface of the discharged silver ingot is rectangular. Here, it is to be noted that: when the silver ingot upper surface of coming out of a furnace is the rectangle, survey area ratio only need survey length ratio can for the survey is simple and convenient more, should understand, this application embodiment does not do specifically and restricts the upper surface shape of silver ingot coming out of a furnace, as long as make things convenient for the calculated area ratio can, in some other embodiments of this application, the shape of silver ingot coming out of a furnace still can be for trapezoidal, circular etc..
In some embodiments of the present application, the ratio of the area of the foreign material zone containing nitric acid insoluble matter to the upper surface of the tapped silver ingot is measured by measuring the length ratio of the foreign material zone to the tapped silver ingot. It should be understood that the present application is not particularly limited as to how the length of the foreign object zone is measured, and preferably, in some embodiments of the present application, the length of the foreign object zone is measured by measuring the longest length and the shortest length of the foreign object zone and averaging to obtain the length of the foreign object zone.
In some embodiments herein, the length of the foreign material zone is measured by measuring the length of the foreign material zone from 5 to 10, and averaging the measured lengths to obtain the length of the foreign material zone, where the length from 5 to 10 includes the longest length and the shortest length of the foreign material zone. Here, it is to be noted that: although the shape of the foreign material region is irregular, the shape is close to a rectangle in terms of the melting method of the intermittent movement and the principle of forming the foreign material region, and the length is conveniently and accurately determined by taking the average of the lengths of several places.
In some embodiments of the present application, the melting temperature of the high purity silver ingot is 1000-. The melting time is 1-3 h.
In some embodiments of the present application, the intermittent movement of the high purity silver ingot is performed in a manner that a single movement time is 20-40min, a single movement speed is 4-6cm/min, and a single intermittent time is 20-40s, that is, the movement of the high purity silver ingot is stopped for 20-40s every 20-40min at a speed of 4-6cm/min, and then the movement is repeated.
In some embodiments of the present application, the melting of the high-purity silver ingot is performed in a high-temperature furnace, and the intermittent movement of the high-purity silver ingot is to place the high-purity silver ingot into a graphite boat, and intermittently push the graphite boat from an inlet of the high-temperature furnace to an outlet of the high-temperature furnace through a push rod in the high-temperature furnace.
In some embodiments of the present application, the atmosphere of the protective gas during melting of the high-purity silver ingot is a chemically inert protective gas, which may be an inert gas such as nitrogen, helium, etc., and the specific kind of the protective gas is not particularly limited herein.
Example 1
(1) 5 plus or minus 0.1kg of high-purity silver ingots are loaded into a graphite material boat;
(2) placing the graphite material boat filled with the high-purity silver ingot into a high-temperature furnace at 1100 ℃ and protected by nitrogen atmosphere, wherein the length of an effective temperature zone of the high-temperature furnace is 750 cm;
(3) a push rod in the high-temperature furnace pushes the graphite boat filled with the high-purity silver ingots from an inlet of the high-temperature furnace to an outlet of the high-temperature furnace, the pushing speed is 5cm/min, the push rod stops pushing for 30s every 30min, and then the push rod continues to push forwards;
(4) when the silver ingot reaches the outlet of the high-temperature furnace, the appearance of the upper surface of the discharged silver ingot in the graphite material boat is observed, the total length of the discharged silver ingot is about 20cm by using a ruler as shown in fig. 5, the length of a foreign matter zone containing the nitric acid insoluble substances is about 10cm, the foreign matter zone containing the nitric acid insoluble substances accounts for about 50% of the total area of the upper surface of the discharged silver ingot, and the content of the nitric acid insoluble substances in the high-purity silver ingot can be judged to be qualified through the corresponding relation in the table 2.
Example 2
(1) 5 plus or minus 0.1kg of high-purity silver ingots are loaded into a graphite material boat;
(2) placing the graphite material boat filled with the high-purity silver ingot into a high-temperature furnace at 1100 ℃ and protected by nitrogen atmosphere, wherein the length of an effective temperature zone of the high-temperature furnace is 750 cm;
(3) a push rod in the high-temperature furnace pushes the graphite boat filled with the high-purity silver ingots from an inlet of the high-temperature furnace to an outlet of the high-temperature furnace, the pushing speed is 5cm/min, the push rod stops pushing for 30s every 30min, and then the push rod continues to push forwards;
(4) when the silver ingot reaches the outlet of the high-temperature furnace, the appearance of the upper surface of the discharged silver ingot in the graphite material boat is observed, the total length of the discharged silver ingot is about 20cm by using a straight ruler as shown in fig. 6, the length of a foreign matter area containing nitric acid insoluble substances is about 15cm, the foreign matter area containing the nitric acid insoluble substances accounts for about 75% of the total area of the upper surface of the discharged silver ingot, and the content of the nitric acid insoluble substances in the high-purity silver ingot can be judged to be unqualified through the corresponding relation in table 2.
Finally, the above embodiments are only used for illustrating the technical solutions of the present application and not for limiting, although the present application is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present application without departing from the spirit and scope of the technical solutions of the present application, and all the technical solutions of the present application should be covered by the claims of the present application.
Claims (6)
1. A method for detecting the content of nitric acid insoluble substances in a high-purity silver ingot is characterized by comprising the following steps of:
melting a high-purity silver ingot in a protective gas atmosphere, and moving the high-purity silver ingot intermittently in the melting process;
cooling after the melting is finished to obtain a discharged silver ingot, wherein a foreign object area and a mirror surface bright area are formed on the upper surface of the discharged silver ingot;
determining the content of nitric acid insoluble substances in the high-purity silver ingot according to the ratio of the area of the foreign material area to the mass of the high-purity silver ingot;
the high-purity silver ingots are melted in a high-temperature furnace, and the intermittent movement of the high-purity silver ingots is to place the high-purity silver ingots in a graphite material boat and push the graphite material boat from an inlet of the high-temperature furnace to an outlet of the high-temperature furnace through a push rod in the high-temperature furnace; the intermittent movement adopts a mode that the single movement time is 20-40min, the single movement speed is 4-6cm/min, and the single intermittent time is 20-40 s; the upper surface of the discharged silver ingot is rectangular;
the detection method further comprises the following steps: determining the area of a foreign material area formed by the high-purity silver ingots with known nitric acid insoluble content, the quality of the known high-purity silver ingots and the linear relation among the nitric acid insoluble content, and determining the content of the nitric acid insoluble in the high-purity silver ingots to be measured according to the linear relation.
2. The detection method according to claim 1, wherein the thickness of the tapped silver ingot is 13-15 mm.
3. The detection method according to claim 1, wherein the content of the nitric acid insoluble matter in the high purity silver ingot is determined based on a ratio of an area of the foreign material region to an area of an upper surface of the discharged silver ingot.
4. The detection method as claimed in claim 1, wherein the melting temperature is 1000-1200 ℃.
5. The method of claim 4, wherein the melting temperature is 1100 ± 10 ℃.
6. The detection method according to claim 1, wherein the melting time is 1 to 3 hours.
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| CN1150839A (en) * | 1995-03-14 | 1997-05-28 | 新日本制铁株式会社 | Metal purity evaluation device and method |
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| NO177875C (en) | 1993-07-26 | 1995-12-06 | Elkem As | Process for direct chemical analysis of molten metal |
| CN102279176B (en) | 2011-08-19 | 2013-01-23 | 山东黄金矿业(莱州)有限公司精炼厂 | Simultaneous measuring method for impurity elements in silver |
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| CN1150839A (en) * | 1995-03-14 | 1997-05-28 | 新日本制铁株式会社 | Metal purity evaluation device and method |
| JPH1026618A (en) * | 1995-05-19 | 1998-01-27 | Nippon Steel Corp | Quick evaluating method of material present in metal |
| CN101850975A (en) * | 2009-04-01 | 2010-10-06 | 高文秀 | Method for purifying silicon by removing phosphorus and metal impurities |
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| DE102019120763B4 (en) | 2022-05-12 |
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