CN114657421B - Ce-Zn alloy, production method thereof and application of smelting vessel - Google Patents
Ce-Zn alloy, production method thereof and application of smelting vessel Download PDFInfo
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- CN114657421B CN114657421B CN202210366224.9A CN202210366224A CN114657421B CN 114657421 B CN114657421 B CN 114657421B CN 202210366224 A CN202210366224 A CN 202210366224A CN 114657421 B CN114657421 B CN 114657421B
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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
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Abstract
The application discloses a Ce-Zn alloy, a production method thereof and application of a smelting vessel. The production method of the Ce-Zn alloy comprises the following steps: (1) Smelting cerium metal and zinc metal in a smelting vessel, and refining to obtain an alloy melt; (2) casting the alloy melt to obtain Ce-Zn alloy; wherein, the contact part of the smelting vessel and the metal cerium and the metal zinc is formed by one or more of the following substances: tungsten, tantalum, cerium oxide; wherein the content of the metal cerium is less than 10.0wt% and more than 0 of the total weight of the metal cerium and the metal zinc. The preparation method can reduce the deviation of the content of cerium in the prepared Ce-Zn alloy.
Description
Technical Field
The application relates to a Ce-Zn alloy, a production method thereof and application of a smelting vessel.
Background
Zinc and cerium are not easily smelted together. The melting point of cerium metal is higher than that of zinc metal. The metal cerium has strong activity and is easy to oxidize in smelting. Therefore, the composition of the ce—zn alloy is difficult to control accurately. The feed ratio of the two materials often has a certain deviation from the content ratio of the obtained alloy.
CN105441761a discloses a preparation process of Gd-Mg-Al-Zn alloy: smelting Mg, al, zn and Mg-Gd intermediate alloy in a well-type crucible furnace, and protecting the intermediate alloy by adopting a covering agent during smelting to obtain an alloy melt. The alloy melt is cast in an ingot mold. The alloy contains rare earth, zn, mg, al and other elements, and the content of Mg is large.
CN1475592a discloses a preparation method of high zinc aluminum rare earth magnesium alloy, pure magnesium, pure zinc, pure aluminum and rare earth intermediate alloy are smelted by adopting a resistance crucible furnace. The alloy obtained by the method also contains Mg and Al, and the specific gravity of Mg in the alloy is larger.
CN101100732a discloses a preparation method of binary alloy plating material, zn, RE and microelements are smelted in a smelting furnace, and then stirred, refined and deslagged, and poured into alloy ingots. The alloy obtained by the method has larger deviation of the rare earth content from the rare earth content in the original batch, and the obtained alloy has more impurity content.
Disclosure of Invention
In view of the above, an object of the present application is to provide a method for producing a Ce-Zn alloy, which can reduce the variation in the content of cerium in the Ce-Zn alloy produced. Further, the Ce-Zn alloy obtained by the method has lower impurity content. Another object of the present application is to provide a Ce-Zn alloy. It is a further object of the present application to provide a use of a melting vessel capable of reducing the variation in the content of cerium in Ce-Zn alloy.
The technical aim is achieved through the following technical scheme.
In one aspect, the application provides a method for producing Ce-Zn alloy, comprising the following steps:
(1) Smelting cerium metal and zinc metal in a smelting vessel, and refining to obtain an alloy melt;
(2) Casting the alloy melt to obtain Ce-Zn alloy;
wherein, the contact part of the smelting vessel and the metal cerium and the metal zinc is formed by one or more of the following substances: tungsten, tantalum, cerium oxide;
wherein the content of the metal cerium is less than 10.0wt% and more than 0 of the total weight of the metal cerium and the metal zinc.
The production method according to the present application preferably further comprises the steps of: polishing a cerium raw material, and then melting and refining to obtain metal cerium; and polishing the zinc raw material to obtain the metallic zinc.
According to the production method of the present application, preferably, the smelting conditions are as follows: the smelting temperature is 500-850 ℃, and the smelting pressure is 0.01-0.06 MPa.
According to the production method of the present application, preferably, in the step (1), the refining time is 10 minutes or longer.
According to the production method of the present application, preferably, in the step (2), the alloy melt is cast into a water-cooled ingot mold or an ingot mold with an electromagnetic stirring function to obtain the ce—zn alloy.
On the other hand, the application provides a Ce-Zn alloy, which is prepared by the method.
According to the Ce-Zn alloy of the present application, preferably, the content of oxygen element in the Ce-Zn alloy is not more than 0.002wt%, the content of phosphorus element is not more than 0.01wt%, the content of sulfur element is not more than 0.01wt%, and the content of carbon element is not more than 0.008wt%.
According to the Ce-Zn alloy of the present application, preferably, the deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.008; the deviation of the content of cerium element in the Ce-Zn alloy is calculated by adopting the following formula:
|α-β|/α；
wherein, alpha represents the weight percentage of the metal cerium to the total weight of the metal cerium and the metal zinc, and the unit is weight percent;
wherein, beta represents the content of cerium element in Ce-Zn alloy, and the unit is wt%.
In a further aspect, the application provides the use of a smelting vessel for reducing the variance in the content of Ce element in a Ce-Zn alloy, the smelting vessel being formed from one or more of the following: tungsten, tantalum, cerium oxide;
the content of cerium element in the Ce-Zn alloy is more than zero and less than or equal to 10.0wt%;
the deviation of the content of cerium element in the Ce-Zn alloy is calculated by adopting the following formula:
|α-β|/α；
wherein, alpha represents the weight percentage of the metal cerium to the total weight of the metal cerium and the metal zinc, and the unit is weight percent;
wherein, beta represents the content of cerium element in Ce-Zn alloy, and the unit is wt%.
The use according to the application preferably comprises the steps of:
(1) Smelting cerium metal and zinc metal in a smelting vessel, and refining to obtain an alloy melt;
(2) Casting the alloy melt to obtain Ce-Zn alloy;
wherein the content of the metal cerium is less than 10.0wt% and more than 0 of the total weight of the metal cerium and the metal zinc.
The application discovers that the specific material is selected at the contact part of the smelting vessel, the metal cerium and the metal zinc, so that the deviation of the content of cerium in the prepared Ce-Zn alloy can be reduced, and the content of cerium in the Ce-Zn alloy can be controlled accurately. Further, the Ce-Zn alloy prepared by the method has low content of impurity elements.
Detailed Description
The present application will be further described with reference to specific examples, but the scope of the present application is not limited thereto.
The smelting vessel refers to a container for bearing metal cerium and metal zinc in the processes of smelting, refining and the like of the metal cerium and the metal zinc. Such as a crucible, etc.
The term "inner surface of the melting vessel" as used herein refers to the surface of the melting vessel that forms the receiving cavity for the cerium metal and zinc metal.
< method for producing Ce-Zn alloy >
The production method of the Ce-Zn alloy comprises the following steps: (1) a step of forming an alloy melt; (2) a step of forming a Ce-Zn alloy.
Step of forming alloy melt
Smelting cerium metal and zinc metal in a smelting vessel, and refining to obtain alloy melt. The smelting vessel of the present application contains only cerium metal and zinc metal. Of course, some unavoidable impurities such as oxygen, phosphorus, sulfur, etc. may be accommodated.
The contact part of the smelting vessel with the metal cerium and the metal zinc is formed by one or more of the following substances: tungsten, tantalum, cerium oxide. According to one embodiment of the application, the part of the smelting vessel that is in contact with the metal cerium and the metal zinc is formed of tungsten, tantalum or cerium oxide. Preferably, the smelting vessel is formed of cerium oxide at the location where the metal cerium and zinc are in contact. Tungsten is a simple substance of tungsten. Tantalum is a tantalum simple substance. Preferably, the inner surface of the smelting vessel is formed from the above-described materials. In certain embodiments, the entire smelting vessel is formed from the above-described materials. The application surprisingly discovers that the smelting vessel is used for smelting and refining metal cerium and metal zinc, so that the deviation of the content of cerium element in the formed Ce-Zn alloy can be reduced.
In the smelting raw material, the content of metal cerium is below 10.0wt% of the total weight of the metal cerium and the metal zinc and is more than 0; preferably 0.2 to 9.0 wt.%; more preferably 1.5 to 8.0wt%; most preferably from 2.0 to 7.0wt%.
Polishing the cerium raw material, and then melting and refining to obtain the metal cerium. The cerium raw material may be a metallic cerium raw material obtained by electrolysis.
The oxygen content in the cerium metal is less than or equal to 0.02wt%; preferably, the oxygen content is less than or equal to 0.008wt%. The phosphorus content in the cerium metal is less than or equal to 0.03wt%; preferably, the phosphorus content of the cerium metal is < 0.01wt%. The sulfur content in the cerium metal is less than or equal to 0.02wt%; preferably, the sulfur content is < 0.0050wt%.
The content of the metal zinc in the smelting raw material is more than 90 weight percent and less than 100 weight percent of the total weight of the metal cerium and the metal zinc; preferably, the content of the metal zinc is 91-99.8 wt% of the total weight of the metal cerium and the metal zinc; more preferably, the content of the metallic zinc is 92 to 98.5wt% of the total weight of the metallic cerium and the metallic zinc; most preferably, the content of the metallic zinc is 93 to 98wt% of the total weight of the metallic cerium and the metallic zinc.
And polishing the zinc raw material to obtain the metallic zinc. Polishing can remove impurities on the surface of the metallic zinc.
The smelting temperature of the metal cerium and the metal zinc can be 500-850 ℃; preferably 600 to 800 ℃; more preferably 650 to 750 ℃. The smelting time is based on the complete melting of zinc.
Smelting may be performed in an inert atmosphere. Inert atmospheres include, but are not limited to, helium, neon, argon, and the like. According to one embodiment of the application, the inert atmosphere is argon. Smelting pressure is 0.01-0.06 MPa; preferably 0.02-0.05 MPa; more preferably 0.03 to 0.04MPa. Smelting may be performed in a vacuum smelting furnace. According to one embodiment of the application, the vacuum melting furnace is evacuated to below 10Pa, and then inert gas is charged into the vacuum melting furnace to form a melting environment having the above-described pressure and inert atmosphere.
Refining time is longer than 10min; preferably, the refining time is 20-120 min; more preferably, the refining time is 30 to 60 minutes. This ensures that the cerium is fully alloyed with the zinc. Refining may be performed in a vacuum melting furnace.
Step of Forming Ce-Zn alloy
Casting the alloy melt to obtain the Ce-Zn alloy.
The mould used for casting can be a water-cooled ingot mould or an ingot mould with stirring function. The mold may be formed of copper. In certain embodiments, the method may further comprise the step of cooling the cast alloy ingot.
< Ce-Zn alloy >
The Ce-Zn alloy is prepared by adopting the method. The Ce-Zn alloy consists of cerium element and zinc element. Of course, unavoidable impurities such as oxygen, phosphorus, sulfur, or carbon may be included in the ce—zn alloy.
The content of oxygen element in the Ce-Zn alloy is less than or equal to 0.002wt%; preferably, the content of oxygen element is less than or equal to 0.0015wt%; more preferably, the content of oxygen element is 0.0012wt% or less. The content of phosphorus element in Ce-Zn alloy is less than or equal to 0.01wt%; preferably, the content of phosphorus element is less than or equal to 0.006wt%; more preferably, the content of phosphorus element is < 0.0050wt%. The content of sulfur element in Ce-Zn alloy is less than or equal to 0.01wt%; preferably, the content of sulfur element is less than or equal to 0.006wt%; more preferably, the content of elemental sulphur is < 0.0050wt%. The content of carbon element in Ce-Zn alloy is less than or equal to 0.008wt%; preferably, the content of carbon element is less than or equal to 0.007wt%; more preferably, the content of the carbon element is 0.0065wt% or less.
The deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.008; preferably, the deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.005; more preferably, the deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.002; most preferably, the deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.0000001. In certain embodiments, the variance in the content of cerium in the Ce-Zn alloy may be zero. The deviation of the content of cerium element in the Ce-Zn alloy is calculated by adopting the following formula:
|α-β|/α；
wherein, alpha represents the weight percentage of the metal cerium to the total weight of the metal cerium and the metal zinc, and the unit is weight percent;
wherein, beta represents the content of cerium element in Ce-Zn alloy, and the unit is wt%.
< use of melting vessel >
According to the application, the specific material is selected at the contact part of the smelting vessel with the metal cerium and the metal zinc, so that the deviation of the content of cerium in the prepared Ce-Zn alloy can be reduced. Thus, the application provides the use of a smelting vessel for reducing the deviation of the content of cerium in a Ce-Zn alloy.
The contact part of the smelting vessel with the metal cerium and the metal zinc is formed by one or more of the following substances: tungsten, tantalum, cerium oxide. According to one embodiment of the application, the part of the smelting vessel that is in contact with the metal cerium and the metal zinc is formed of tungsten, tantalum or cerium oxide. Preferably, the smelting vessel is formed of cerium oxide at the location where the metal cerium and zinc are in contact. Tungsten is a simple substance of tungsten. Tantalum is a tantalum simple substance. Preferably, the inner surface of the smelting vessel is formed from the above-described materials. In certain embodiments, the entire smelting vessel is formed from the above-described materials.
The content of cerium element in Ce-Zn alloy is more than zero and less than or equal to 10.0wt%; preferably 0.2 to 9.0 wt.%; more preferably 1.5 to 8.0wt%; most preferably from 2.0 to 7.0wt%.
The content of zinc element in Ce-Zn alloy is less than 100wt% and more than or equal to 90wt%; preferably 91 to 99.8 wt.%; more preferably 92 to 98.5wt%; most preferably 93 to 98wt%.
The deviation of the content of cerium element in the Ce-Zn alloy is calculated by adopting the following formula:
|α-β|/α；
wherein, alpha represents the weight percentage of the metal cerium to the total weight of the metal cerium and the metal zinc, and the unit is weight percent;
wherein, beta represents the content of cerium element in Ce-Zn alloy, and the unit is wt%.
The deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.008; preferably, the deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.005; more preferably, the deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.002; most preferably, the deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.0000001. In certain embodiments, the variance in the content of cerium in the Ce-Zn alloy may be zero.
Specifically, the method comprises the following steps: (1) Smelting cerium metal and zinc metal in a smelting vessel, and refining to obtain an alloy melt; and (2) casting the alloy melt to obtain the Ce-Zn alloy. The selection of each raw material and the specific operation of each step are as described above, and are not described in detail herein.
The following describes the method for testing the content of each element in Ce-Zn alloy:
cerium element: measuring by using an inductively coupled plasma emission spectrometer (ICP-OES);
carbon element: measured using an infrared carbon sulfur analyzer (model LECO-400, purchased from the american LECO company);
elemental sulfur: measured using an infrared carbon sulfur analyzer (model LECO-400, purchased from the american LECO company);
phosphorus element: measuring with spectrophotometer (model 722, purchased from Shanghai precision instruments factory);
oxygen element: the measurement was carried out by using an oxygen-nitrogen-hydrogen analyzer (model number ONH-2000).
The deviation of cerium element in Ce-Zn alloy is calculated by the following formula:
|α-β|/α；
wherein, alpha represents the weight percentage of the metal cerium to the total weight of the metal cerium and the metal zinc, and the unit is weight percent;
wherein, beta represents the content of cerium element in Ce-Zn alloy, and the unit is wt%.
Example 1
Polishing the cerium raw material obtained by electrolysis, and then melting and refining in a vacuum melting furnace to obtain metal cerium. The content of oxygen element in the metal cerium is less than or equal to 0.008wt%, the content of phosphorus element is less than 0.01wt%, and the content of sulfur element is less than 0.0050wt%.
And polishing the zinc raw material to obtain the metallic zinc.
5.5 parts by weight of metallic cerium and 94.5 parts by weight of metallic zinc were placed in a crucible whose inner wall was formed of elemental tungsten. And smelting the crucible in argon atmosphere at the temperature of 700 ℃ under the pressure of 0.03MPa until zinc is completely melted, and refining for 30min to obtain alloy melt.
Casting the alloy melt into a water-cooled copper ingot mould, and cooling to room temperature to obtain the Ce-Zn alloy.
The properties of the resulting alloy are shown in table 1.
Example 2
Example 1 was repeated except that the inner wall of the crucible was formed of tantalum simple substance. The properties of the resulting alloy are shown in table 1.
Example 3
Example 1 was repeated except that the inner wall of the crucible was made of cerium oxide. The properties of the resulting alloy are shown in table 1.
Comparative example 1
Example 1 was repeated except that the inner wall of the crucible was formed of magnesium oxide. The properties of the resulting alloy are shown in table 1.
TABLE 1
The present application is not limited to the above-described embodiments, and any modifications, improvements, substitutions, and the like, which may occur to those skilled in the art, fall within the scope of the present application without departing from the spirit of the application.
Claims (4)
1. A use of a smelting vessel for reducing the deviation of the content of Ce element in Ce-Zn alloy is characterized in that,
(1) Smelting cerium metal and zinc metal in a smelting vessel, and refining for 20-120 min to obtain alloy melt; the smelting temperature is 650-750 ℃;
(2) Casting the alloy melt in a water-cooled ingot mould formed by copper to obtain Ce-Zn alloy;
wherein, the contact part of the smelting vessel with the metal cerium and the metal zinc is formed by cerium oxide;
wherein the content of the metal cerium is 1.5 to 8.0 weight percent of the total weight of the metal cerium and the metal zinc; in the metal cerium, the oxygen content is less than or equal to 0.008wt%, the phosphorus content is less than 0.01wt%, and the sulfur content is less than 0.0050wt%;
wherein, the deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.0000001; the deviation of the content of cerium element in the Ce-Zn alloy is calculated by adopting the following formula:
|α-β|/α；
wherein, alpha represents the weight percentage of the metal cerium to the total weight of the metal cerium and the metal zinc, and the unit is weight percent;
wherein, beta represents the content of cerium element in Ce-Zn alloy, and the unit is wt%.
2. The use according to claim 1, further comprising the steps of:
polishing a cerium raw material, and then melting and refining to obtain metal cerium;
and polishing the zinc raw material to obtain the metallic zinc.
3. Use according to claim 1, characterized in that the smelting pressure is 0.01-0.06 MPa.
4. The use according to claim 1, wherein the content of oxygen element in the Ce-Zn alloy is less than or equal to 0.002wt%, the content of phosphorus element is less than or equal to 0.01wt%, the content of sulfur element is less than or equal to 0.01wt%, and the content of carbon element is less than or equal to 0.008wt%.
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