CN110777263A - Fusion casting preparation method of low-oxygen pure silver melt material - Google Patents
Fusion casting preparation method of low-oxygen pure silver melt material Download PDFInfo
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- CN110777263A CN110777263A CN201910992898.8A CN201910992898A CN110777263A CN 110777263 A CN110777263 A CN 110777263A CN 201910992898 A CN201910992898 A CN 201910992898A CN 110777263 A CN110777263 A CN 110777263A
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- ingot
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D31/00—Cutting-off surplus material, e.g. gates; Cleaning and working on castings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
Abstract
A fusion casting preparation method of a low-oxygen pure silver melt material comprises the following specific steps: 1) putting a silver ingot into a graphite crucible, putting activated carbon powder into a hopper, putting a graphite mold into a casting mold station of a vacuum furnace, closing a vacuum furnace cover, and heating for primary vacuum melting; 2) after the silver ingot is completely melted into silver solution, pouring the activated carbon powder into a graphite crucible, preserving heat, standing for 15-30min, and beginning to cast to obtain an ingot; 3) after the cast ingot is cooled, opening a furnace cover, taking out the cast ingot from the mold, and cutting off a riser part to obtain a primary cast ingot; 4) and carrying out secondary vacuum melting on the primary cast ingot, cooling, taking out, and cutting off a riser again to obtain a secondary cast ingot, thus completing the preparation. In conclusion, the silver ingot prepared by the method has low oxygen content and high purity.
Description
Technical Field
The invention belongs to the field of pure silver fuse melt material manufacturing, and particularly relates to a fusion casting preparation method of a low-oxygen pure silver melt material.
Background
The fuse is widely applied to high-low voltage distribution systems, control systems and electric equipment, and is one of the most commonly applied protection devices as a short circuit protector and an overcurrent protector. When the fuse passes through excessive current, the melt material must be fused in time to protect the electric appliance, and the chemical composition, resistivity, dimensional accuracy and the like of the melt material all influence the service performance of the melt material. With the rapid development of modern manufacturing industry, electrical products are increasingly developed towards large capacity, small volume and differentiation, and higher requirements are put forward on melt materials, namely, the melt materials are required to be complete in variety and specification, various in shape, accurate in size, reliable in performance and low and stable in resistance in the using process. The formability and the processability of the melt material are improved, the resistivity of the melt material is reduced, and the melt material has great significance for improving the quality of the melt material.
Silver has excellent electrical and thermal conductivity, and of all metals, silver has the best electrical conductivity. Therefore, pure silver is an ideal melt material for making fuses, especially high-end fuses. In the processing process of the pure silver melt material, the component purity, the impurity content and the dimensional accuracy of the pure silver melt material need to be accurately controlled, so that stable and accurate linear resistivity can be obtained. The common pure silver melt material products are silver strips and silver wires, the main processing technological processes comprise smelting casting, extrusion, rolling or drawing and the like of silver ingots, the silver ingots are blanks used for extrusion and are also starting materials in the whole pure silver melt material processing process, and the purity of the silver ingots directly determines the purity and the resistivity of final finished products, so that the use performance of the products is influenced. Therefore, the preparation of high-purity silver ingots is a key process for processing pure silver melt materials.
The impurity elements and oxygen content of silver have great influence on the conductivity of silver, and the index representing the conductivity of silver is resistivity. The lower the content of impurity elements in silver, the lower the oxygen content, the higher the silver purity, and the lower the resistivity. For fuse melt materials, the less the mass of silver material required to reach the same meter resistance value, and the important significance for saving material cost, therefore, the resistivity is one of the key technical indexes of pure silver melt material products.
Silver is oxidized during smelting, and when the silver is strongly oxidized, no covering agent is arranged on the molten silver liquid level, and the furnace burden contains more volatile metals such as lead, zinc, arsenic, antimony and the like, the volatilization loss of the silver is increased. Silver, when melted in air, absorbs 21 times its own volume of oxygen, which is released as "silver rain" when the molten silver liquid condenses, causing a splash loss of fine-grained silver beads. Oxygen can affect the resistivity and subsequent processing performance of the pure silver melt material, so that the oxygen content in the silver ingot casting process is controlled, the low-oxygen high-purity silver ingot preparation process is developed, and the method has important significance for processing the precise pure silver melt material.
Disclosure of Invention
The technical scheme of the invention is as follows: a fusion casting preparation method of a low-oxygen pure silver melt material comprises the following specific steps:
1) putting a silver ingot into a graphite crucible, putting activated carbon powder into a hopper, putting a graphite mold into a casting mold station of a vacuum furnace, closing a vacuum furnace cover, and heating for primary vacuum melting;
2) after the silver ingot is completely melted into silver solution, pouring the activated carbon powder into a graphite crucible, preserving heat, standing for 15-30min, and beginning to cast to obtain a cast ingot;
3) after the cast ingot is cooled, opening a furnace cover, taking out the cast ingot from the mold, and cutting off a riser part to obtain a primary cast ingot;
4) and carrying out secondary vacuum melting on the primary cast ingot, cooling, taking out, and cutting off a riser again to obtain a secondary cast ingot, thus completing the preparation.
Further optimizing, the graphite crucible in the step 1) is a crucible with high purity, high strength and high compactness, and the casting mold is made of graphite with high purity, high strength and high compactness.
Further optimizing, the aperture of the graphite mould in the step 1) is 100mm, and the height of the graphite mould is 260 mm.
Further optimizing, the size of a riser cut by the primary ingot in the step 3) is one tenth of the length of the whole ingot.
Further preferably, the oxygen content value measured in the step 4) is 10.4-10.6 ppm.
Further optimizing, the heating temperature of the primary vacuum melting in the step 1) and the secondary vacuum melting in the step 4) is 900-
-3Pa, introducing high-purity argon after the silver ingot begins to sweat until the vacuum degree is 0.1-0.5Pa, and smelting at the smelting temperature of 950-1030 ℃.
The invention has the beneficial effects that:
the method has the advantages that a vacuum smelting process is adopted, oxygen in the atmosphere is prevented from being absorbed in the silver ingot smelting process, a crucible and a casting mold adopted in the smelting process are both made of high-purity, high-strength and high-density graphite, pollution of other impurity elements to the silver ingot can be avoided, and the graphite can be used for deoxidation;
secondly, adding activated carbon powder during smelting, so that the contact area of oxygen and carbon in the silver solution is increased, the oxygen and the carbon in the silver solution can fully react to generate carbon dioxide and carbon monoxide, and the carbon dioxide and the carbon monoxide volatilize from the silver solution, so that full deoxidation can be realized, and the low-oxygen high-purity silver ingot is obtained;
and thirdly, cutting off a dead head of the obtained primary ingot, removing the part containing more impurities at the dead head in the silver ingot, and in addition, carrying out secondary vacuum melting on the obtained ingot, deoxidizing again and cutting off the dead head, thereby realizing the effect of secondary refining, effectively reducing the oxygen content in the silver ingot and finally obtaining the low-oxygen high-purity silver ingot.
Detailed Description
The technical solutions in the embodiments of the present invention will be described in detail below, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all 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
Selecting a vacuum smelting furnace with the capacity of 25kg, putting a silver ingot with the oxygen content of 186ppm and the weight of 24kg into a graphite crucible, putting 500g of activated carbon powder into a hopper in the vacuum furnace, putting a graphite mold with the aperture of 100mm and the height of 260mm into a casting mold station of the vacuum furnace, placing the graphite crucible in the vacuum furnace, closing a vacuum furnace cover, setting the smelting temperature to be 900 ℃ and the vacuum degree to be 5.0 multiplied by 10
-3Pa, starting a power supply to start heating, and carrying out primary vacuum melting and primary deoxidation; after the silver ingot is sweated, high-purity argon is introduced until the vacuum degree is 0.1Pa, and heating is continued. After the silver ingot is completely melted into silver solution, starting a feeding button, pouring activated carbon powder into a crucible, preserving heat, standing for 20min, then casting to obtain an ingot, after the ingot is cooled, opening a furnace cover, taking out the ingot from a mold, cutting off a feeder head part with the length of 23mm, effectively removing most impurities to obtain a primary ingot, putting the primary ingot into the graphite crucible again, setting the melting temperature to be 900 ℃ and the vacuum degree to be 5.0 multiplied by 10
-3Pa; heating, introducing high-purity argon after the silver ingot is sweated until the vacuum degree is 0.1Pa, continuing heating, adding activated carbon powder after the silver ingot is completely melted, and performing secondary vacuum melting and secondary deoxidation at the melting temperature of 980 ℃ and the vacuum degree of 0.1 Pa; and cutting off a dead head of the ingot obtained by secondary vacuum melting, testing the oxygen content, and measuring the oxygen content value to be 10.4ppm to obtain the low-oxygen high-purity silver ingot meeting the requirement.
Example 2
Selecting a vacuum smelting furnace with the capacity of 25kg, putting a silver ingot with the oxygen content of 186ppm and the weight of 24kg into a graphite crucible, putting 500g of activated carbon powder into a hopper in the vacuum furnace, putting a graphite mold with the aperture of 100mm and the height of 260mm into a casting mold station of the vacuum furnace, placing the graphite crucible in the vacuum furnace, closing a vacuum furnace cover, setting the smelting temperature to be 910 ℃ and the vacuum degree to be 5.0 multiplied by 10
-3Pa, starting a power supply to start heating, and carrying out primary vacuum melting and primary deoxidation; after the silver ingot is sweated, high-purity argon is introduced until the vacuum degree is 0.2Pa, and heating is continued. After the silver ingot is completely melted into silver solution, starting a feeding button, pouring activated carbon powder into a crucible, keeping the temperature and standing for 25min, and then starting castingObtaining an ingot, opening a furnace cover after the ingot is cooled, taking the ingot out of the mold, cutting off a riser part with the length of 23mm to obtain a primary ingot, adding the primary ingot into a graphite crucible, setting the melting temperature to be 910 ℃ and the vacuum degree to be 5.0 multiplied by 10
-3Pa; heating, introducing high-purity argon after the silver ingot is sweated until the vacuum degree is 0.2Pa, and continuing heating. (ii) a After the mixture is completely melted, adding activated carbon powder to carry out secondary vacuum melting and secondary deoxidation; and cutting off a dead head of the ingot obtained by secondary vacuum melting, testing the oxygen content, and measuring the oxygen content value to be 11.6ppm to obtain the low-oxygen high-purity silver ingot meeting the requirement.
Example 3
Selecting a vacuum smelting furnace with the capacity of 25kg, putting a silver ingot with the oxygen content of 186ppm and the weight of 24kg into a graphite crucible, putting 500g of activated carbon powder into a hopper in the vacuum furnace, putting a graphite mold with the aperture of 100mm and the height of 260mm into a casting mold station of the vacuum furnace, placing the graphite crucible in the vacuum furnace, closing a vacuum furnace cover, setting the smelting temperature to 930 ℃ and the vacuum degree to 5.0 multiplied by 10
-3Pa, starting a power supply to start heating, and carrying out primary vacuum melting and primary deoxidation; after the silver ingot is sweated, introducing high-purity argon until the vacuum degree is 0.5Pa, and continuing heating; after the silver ingot is completely melted into silver solution, starting a feeding button, pouring activated carbon powder into a crucible, preserving heat, standing for 30min, then casting to obtain an ingot, after the ingot is cooled, opening a furnace cover, taking out the ingot from a mold, cutting off a feeder head part with the length of 23mm to obtain a primary ingot, adding the primary ingot into a graphite crucible, setting the melting temperature to be 930 ℃ and the vacuum degree to be 5.0 multiplied by 10
-3Pa; heating, introducing high-purity argon after the silver ingot is sweated until the vacuum degree is 0.5Pa, and continuing heating. After the mixture is completely melted, adding activated carbon powder to carry out secondary vacuum melting and secondary deoxidation; and cutting off a dead head of the ingot obtained by secondary vacuum melting, testing the oxygen content, and measuring the oxygen content value to be 10.4ppm to obtain the low-oxygen high-purity silver ingot meeting the requirement.
The foregoing illustrates and describes the principal features, utilities, and principles of the invention, as well as advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made in the invention without departing from the spirit and scope of the invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A fusion casting preparation method of a low-oxygen pure silver melt material is characterized by comprising the following specific steps:
1) putting a silver ingot into a graphite crucible, putting activated carbon powder into a hopper, putting a graphite mold into a casting mold station of a vacuum furnace, closing a vacuum furnace cover, and heating for primary vacuum melting;
2) after the silver ingot is completely melted into silver solution, pouring the activated carbon powder into a graphite crucible, preserving heat, standing for 15-30min, and beginning to cast to obtain a cast ingot;
3) after the cast ingot is cooled, opening a furnace cover, taking out the cast ingot from the mold, and cutting off a riser part to obtain a primary cast ingot;
4) and carrying out secondary vacuum melting on the primary cast ingot, cooling, taking out, and cutting off a riser again to obtain a secondary cast ingot, thus completing the preparation.
2. The method for preparing low-oxygen pure silver melt material by fusion casting according to claim 1, wherein the graphite crucible in step 1) is a high-purity, high-strength and high-density crucible, and the casting mold is made of high-purity, high-strength and high-density graphite.
3. The fusion casting method of claim 1, wherein the graphite mold in step 1) has a diameter of 100mm and a height of 260 mm.
4. The fusion casting method of claim 1, wherein the size of the riser of the single ingot in step 3) is one tenth of the entire length of the ingot.
5. The fusion casting method of claim 1, wherein the melting temperature of the first vacuum melting in step 1) and the second vacuum melting in step 4) is 950-
-3Pa, introducing high-purity argon after the silver ingot begins to sweat until the vacuum degree is 0.1-0.5Pa, and smelting again at the smelting temperature of 950-1030 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910992898.8A CN110777263A (en) | 2019-10-18 | 2019-10-18 | Fusion casting preparation method of low-oxygen pure silver melt material |
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| CN201910992898.8A CN110777263A (en) | 2019-10-18 | 2019-10-18 | Fusion casting preparation method of low-oxygen pure silver melt material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114395749A (en) * | 2021-11-13 | 2022-04-26 | 洛阳高新四丰电子材料有限公司 | Preparation method of large-size multi-element Ag-based alloy sputtering target material |
| CN114921656A (en) * | 2022-05-17 | 2022-08-19 | 有研亿金新材料有限公司 | Method for reducing carbon content of high-purity gold |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756075A (en) * | 2016-12-06 | 2017-05-31 | 西安诺博尔稀贵金属材料有限公司 | A kind of degasification method of smelting of big specification fine silver ingot casting |
| CN108504879A (en) * | 2018-06-22 | 2018-09-07 | 昆明冶金研究院 | A kind of the electron-beam smelting method and its device of hypoxemia high purity titanium ingot |
| CN207850043U (en) * | 2017-12-15 | 2018-09-11 | 郑州机械研究所有限公司 | A kind of fine silver melt material vacuum melting device |
-
2019
- 2019-10-18 CN CN201910992898.8A patent/CN110777263A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756075A (en) * | 2016-12-06 | 2017-05-31 | 西安诺博尔稀贵金属材料有限公司 | A kind of degasification method of smelting of big specification fine silver ingot casting |
| CN207850043U (en) * | 2017-12-15 | 2018-09-11 | 郑州机械研究所有限公司 | A kind of fine silver melt material vacuum melting device |
| CN108504879A (en) * | 2018-06-22 | 2018-09-07 | 昆明冶金研究院 | A kind of the electron-beam smelting method and its device of hypoxemia high purity titanium ingot |
Non-Patent Citations (2)
| Title |
|---|
| 周瑞发，韩雅芳，李树索编著: "《高温结构材料》", 30 April 2006, 北京：国防工业出版社 * |
| 姜不居主编: "《实用熔模铸造技术》", 31 March 2008, 沈阳：辽宁科学技术出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114395749A (en) * | 2021-11-13 | 2022-04-26 | 洛阳高新四丰电子材料有限公司 | Preparation method of large-size multi-element Ag-based alloy sputtering target material |
| CN114395749B (en) * | 2021-11-13 | 2023-06-02 | 丰联科光电(洛阳)股份有限公司 | Preparation method of large-size and multi-element Ag-based alloy sputtering target material |
| CN114921656A (en) * | 2022-05-17 | 2022-08-19 | 有研亿金新材料有限公司 | Method for reducing carbon content of high-purity gold |
| CN114921656B (en) * | 2022-05-17 | 2024-01-26 | 有研亿金新材料有限公司 | Method for reducing high-purity gold carbon content |
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Application publication date: 20200211 |
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