Degassing method for tellurium copper smelting

Abstract

According to the degassing method for tellurium-copper smelting, oxygen, hydrogen and the like in a melt are removed through deoxidization of phosphorus-copper alloy, a degassing agent and inert gas are matched with the ultrasonic cavitation effect, then secondary cleaning is conducted through vacuum degassing, secondary ultrasonic treatment is conducted after pouring, cooling is matched, further exhausting is facilitated, and the quality of a formed cast ingot is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of materials, and particularly to a degassing method for tellurium copper smelting. Background Art

[0002] During the smelting process of copper alloys, there are many gases such as hydrogen and oxygen, which will greatly reduce the quality of ingots. To eliminate the gases in the melt, currently common methods such as adding master alloys to react with the corresponding gases, or adding degassing agents to adsorb or react with the gases, or introducing inert gases to exhaust gas, etc., but the effects are not good and need to be improved. Summary of the Invention

[0003] To solve the above at least one technical defect, the present invention provides the following technical solutions:

[0004] This application document discloses a degassing method for tellurium copper smelting, including the following steps:

[0005] S1. Add phosphor copper alloy to the melt formed by tellurium copper raw materials to remove oxygen;

[0006] S2. Introduce an inert gas containing a degassing agent into the melt after deoxidation treatment and perform ultrasonic treatment once;

[0007] S3. Perform vacuum degassing on the melt after ultrasonic treatment;

[0008] S4. Pour the melt after vacuum degassing, and perform secondary ultrasonic treatment on the melt after pouring. The ultrasonic treatment time is 60 - 100 s, and at the same time, cool the melt during ultrasonic treatment to the solidification of the melt through a refrigeration system.

[0009] In this solution, phosphor copper alloy is used to remove oxygen, and a degassing agent and an inert gas are combined with the ultrasonic cavitation effect to remove oxygen, hydrogen, etc. in the melt. Subsequently, vacuum degassing is used for secondary cleaning, and secondary ultrasonic treatment and cooling are performed after pouring to help further exhaust gas, improving the quality of the formed ingot.

[0010] Further, in step S1, the addition amount of the phosphor copper alloy is 1 - 3‰ of the melt mass, and the phosphorus content in the phosphor copper alloy is 10 - 15%. The addition of phosphor copper mainly removes oxygen through phosphorus, but inevitably some phosphorus remains in the melt. Limiting the addition amount of the phosphor copper alloy helps to improve the quality of the subsequent ingot.

[0011] Further, in step S2, the inert gas is introduced from the bottom of the furnace where the melt is located, and the ultrasonic probe extends into the melt from the top liquid surface. Through the ultrasonic cavitation effect, the inert gas bubbles are crushed and the degassing agent is more evenly distributed in the melt, which can adsorb more gases and discharge them. With the cooperation, the exhaust effect is excellent.

[0012] Further, the time for the first ultrasonic treatment is 60 - 150 s. Before the first ultrasonic treatment, it is necessary to cool down to 800 - 900 °C, and cooling can help exhaust gas.

[0013] Further, in step S4, the ultrasonic treatment time is 100 s. The output power in the first and second ultrasonic treatments is 2000 W, and the frequency is 20 KHz. Under the ultrasonic treatment with a limited time, etc., the exhaust gas effect is better.

[0014] Further, in step S2, the degassing agent includes graphite powder and sodium nitrate. By mass, the proportion of graphite powder is 30 - 50%. The exhaust gas is removed through the reactions, adsorption, etc. of graphite powder, and the degassing effect is excellent.

[0015] Further, by mass, the dosage of the degassing agent is 3 - 5‰ of the mass of the melt.

[0016] Further, the flow rate of the inert gas is 4 - 8 L / min, and the exhaust gas effect is better under the limited flow rate.

[0017] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0018] 1. The present invention comprehensively utilizes ultrasonic treatment, inert gas, degassing agent for exhaust gas, etc., and cooperates with ultrasonic treatment under the condition of cooling after casting, and the quality of the formed ingot is significantly improved, and the effect is excellent. Description of the Drawings

[0019] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following will briefly introduce the drawings required for the description of the embodiments. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0020] Figure 1 It is the microscopic structure diagram of the ingot in Example 1;

[0021] Figure 2 It is the microscopic structure diagram of the ingot in Comparative Example 2. Specific Embodiments

[0022] The following will further illustrate the present invention in combination with the drawings and specific embodiments.

[0023] In the following cases, by mass, the raw material ratio of tellurium copper is tellurium 0.6%, aluminum 0.04%, iron 0.03%, and the balance is copper.

[0024] Example 1

[0025] The degassing method for tellurium copper melting includes the following steps:

[0026] S1. Add tellurium copper raw materials into a furnace for smelting to form a melt, and add phosphor copper alloy into the melt formed by the tellurium copper raw materials to remove oxygen. The addition amount of the phosphor copper alloy is 1‰ of the mass of the melt, and the phosphorus content in the phosphor copper alloy is 14%.

[0027] S2. After the deoxidation treatment, introduce an inert gas containing a degassing agent into the melt and conduct ultrasonic treatment once. The inert gas is nitrogen. By mass, the addition amount of the degassing agent is 3‰ of the weight of the melt. Among them, the degassing agent: 50% graphite powder, 50% sodium nitrate. Nitrogen is introduced from the bottom of the furnace where the melt is located, and the gas flow rate is 5 L / min. The ultrasonic probe of the ultrasonic treatment mechanism extends from the liquid surface at the top of the melt to 50 mm below the liquid surface. The ultrasonic treatment time is 80 s, the ultrasonic power is 2000 W, and the frequency is 20 KHz. The melt is cooled to 860 °C before introducing nitrogen. Ultrasonic treatment is carried out 20 s after introducing nitrogen, and nitrogen input ends after the ultrasonic treatment ends.

[0028] S3. Adjust the temperature of the melt after ultrasonic treatment to carry out vacuum degassing. The vacuum degree is 100 Torr and the time is 10 min.

[0029] S4. Pour the melt after vacuum degassing, and conduct secondary ultrasonic treatment on the poured melt. The ultrasonic probe of the ultrasonic treatment mechanism extends from the top surface of the melt to 50 mm below the liquid surface. The ultrasonic treatment time is 100 s. While ultrasonic treatment is carried out, the bottom of the container where the poured melt is located is cooled by water until the melt solidifies.

[0030] After detection, compared with the initial melt, after ultrasonic treatment in step S4, the degassing efficiency is as high as 99.7%. As can be seen from the reference appendix Figure 1 The grains of the ingot are simultaneously refined well.

[0031] Example 2

[0032] A degassing method for tellurium copper smelting, including the following steps:

[0033] S1. Add tellurium copper raw materials into a furnace for smelting to form a melt, and add phosphor copper alloy into the melt formed by the tellurium copper raw materials to remove oxygen. The addition amount of the phosphor copper alloy is 2‰ of the mass of the melt, and the phosphorus content in the phosphor copper alloy is 12%.

[0034] S2. After the deoxidation treatment, an inert gas containing a degassing agent is introduced into the melt and ultrasonic treatment is carried out once. The inert gas is nitrogen. In terms of mass, the addition amount of the degassing agent is 4‰ of the weight of the melt. Among them, the degassing agent: 30% graphite powder, 70% sodium nitrate. Nitrogen is introduced from the bottom of the furnace where the melt is located, and the gas flow rate is 6 L / min. The ultrasonic probe of the ultrasonic treatment mechanism extends from the liquid surface at the top of the melt to 50 mm below the liquid surface. The ultrasonic treatment time is 100 s, the ultrasonic power is 2000 W, and the frequency is 20 KHz. Before introducing nitrogen, the melt is cooled to 820 °C. Ultrasonic treatment is carried out 20 s after introducing nitrogen, and nitrogen input ends after the ultrasonic treatment ends.

[0035] S3. The temperature of the melt after ultrasonic treatment is adjusted for vacuum degassing. The vacuum degree is 80 Torr and the time is 20 min.

[0036] S4. The melt after vacuum degassing is poured, and secondary ultrasonic treatment is carried out on the poured melt. The ultrasonic probe of the ultrasonic treatment mechanism extends from the top surface of the melt into the melt to 50 mm below the liquid surface. The ultrasonic treatment time is 90 s. While ultrasonic treatment is carried out, the bottom of the container where the poured melt is located is cooled by water until the melt solidifies.

[0037] After testing, compared with the original melt, after ultrasonic treatment in step S4, the degassing efficiency is as high as 99.6%.

[0038] Example 3

[0039] A degassing method for tellurium copper smelting, comprising the following steps:

[0040] S1. Add tellurium copper raw materials into the furnace for smelting to form a melt. Add phosphorus copper alloy to the melt formed by the tellurium copper raw materials for deoxidation. Among them, the addition amount of the phosphorus copper alloy is 3‰ of the mass of the melt, and the phosphorus content in the phosphorus copper alloy is 10%.

[0041] S2. After the deoxidation treatment, an inert gas containing a degassing agent is introduced into the melt and ultrasonic treatment is carried out once. The inert gas is nitrogen. In terms of mass, the addition amount of the degassing agent is 3.5‰ of the weight of the melt. Among them, the degassing agent: 60% graphite powder, 40% sodium nitrate. Nitrogen is introduced from the bottom of the furnace where the melt is located, and the gas flow rate is 7 L / min. The ultrasonic probe of the ultrasonic treatment mechanism extends from the liquid surface at the top of the melt to 50 mm below the liquid surface. The ultrasonic treatment time is 120 s, the ultrasonic power is 2000 W, and the frequency is 20 KHz. Before introducing nitrogen, the melt is cooled to 880 °C. Ultrasonic treatment is carried out 20 s after introducing nitrogen, and nitrogen input ends after the ultrasonic treatment ends.

[0042] S3. The temperature of the melt after ultrasonic treatment is adjusted for vacuum degassing. The vacuum degree is 100 Torr and the time is 15 min.

[0043] S4. The degassed melt is poured, and the poured melt is subjected to secondary ultrasonic treatment. The ultrasonic probe of the ultrasonic treatment mechanism penetrates from the top surface of the melt to 50 mm below the liquid surface. The ultrasonic treatment time is 100 s. While ultrasonic treatment is carried out, the bottom of the container where the poured melt is located is cooled by water until the melt solidifies.

[0044] After detection, compared with the initial melt, after ultrasonic treatment in step S4, the degassing efficiency is as high as 99.3%.

[0045] Comparative Example 1

[0046] Compared with Example 1, the difference is that there is no primary ultrasonic treatment in this example. After detection, compared with the initial melt, after ultrasonic treatment in step S4, the degassing efficiency is as high as 90.4%.

[0047] Comparative Example 2

[0048] Compared with Example 1, the difference is that there is no water cooling treatment during the secondary ultrasonic treatment in this example, and only natural cooling is used. After detection, compared with the initial melt, after ultrasonic treatment in step S4, the degassing efficiency is as high as 93.1%. Referring to the attached Figure 2 It can be seen that there are obvious large pores in the ingot.

[0049] In summary, it can be known that under the combined degassing of means such as phosphorus copper alloy, degassing agent, inert gas, and ultrasonic treatment, the quality of the ingot can be significantly improved.

[0050] The above is only the preferred embodiment of the present invention. The protection scope of the present invention is not limited to the above embodiments. All technical solutions falling within the idea of the present invention belong to the protection scope of the present invention. It should be pointed out that for those of ordinary skill in the art in this technical field, several improvements and refinements made without departing from the principle of the present invention should also be regarded as the protection scope of the present invention.

Claims

1. Degassing method for tellurium copper smelting, characterized in that, It includes the following steps: S1. Add phosphor copper alloy to the melt formed by tellurium copper raw materials to remove oxygen; S2. Pass an inert gas containing a degassing agent into the melt after deoxidation treatment and perform primary ultrasonic treatment; S3. Perform vacuum degassing on the melt after ultrasonic treatment; S4. Pour the melt after vacuum degassing, and perform secondary ultrasonic treatment on the melt after pouring. The ultrasonic treatment time is 60 - 100 s, and at the same time, cool down the melt during ultrasonic treatment to the solidification of the melt through a refrigeration system.

2. The degassing method for tellurium copper smelting according to claim 1, characterized in that: In step S1, the addition amount of phosphor copper alloy is 1 - 3‰ of the melt mass, and the phosphorus content in the phosphor copper alloy is 10 - 15%.

3. The degassing method for tellurium copper smelting according to claim 1, characterized in that: In step S2, the inert gas is introduced from the bottom of the furnace where the melt is located, and the ultrasonic probe extends into the melt from the top liquid level.

4. The degassing method for tellurium copper smelting according to claim 3, characterized in that: The primary ultrasonic treatment time is 60 - 150 s, and it is necessary to cool down to 800 - 900 °C before the primary ultrasonic treatment process.

5. The degassing method for tellurium copper smelting according to claim 1, characterized in that: In step S4, the ultrasonic treatment time is 100 s, and the output power in the primary ultrasonic treatment and the secondary ultrasonic treatment is 2000 W, and the frequency is 20 KHz.

6. The degassing method for tellurium copper smelting according to claim 1, characterized in that: In step S2, the degassing agent includes graphite powder and sodium nitrate. Among them, by mass, the proportion of graphite powder is 30 - 50%.

7. The degassing method for tellurium copper smelting according to claim 1, characterized in that: By mass, the dosage of the degassing agent is 3 - 5‰ of the melt mass.

8. The degassing method for tellurium copper smelting according to claim 1, characterized in that: The flow rate of the inert gas is 4 - 8 L / min.

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