CN114657421A - Ce-Zn alloy, method for producing same and use of smelting vessel - Google Patents
Ce-Zn alloy, method for producing same and use of smelting vessel Download PDFInfo
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- CN114657421A CN114657421A CN202210366224.9A CN202210366224A CN114657421A CN 114657421 A CN114657421 A CN 114657421A CN 202210366224 A CN202210366224 A CN 202210366224A CN 114657421 A CN114657421 A CN 114657421A
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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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention 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 metal cerium and metal zinc in a smelting vessel, and then refining to obtain an alloy melt; (2) casting the alloy melt to obtain a Ce-Zn alloy; wherein, the part of the smelting vessel contacted with 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 or equal to 10.0 wt% of the total weight of the metal cerium and the metal zinc and is more than 0. The preparation method can reduce the deviation of the content of cerium element in the prepared Ce-Zn alloy.
Description
Technical Field
The invention 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 easily oxidized in smelting. Therefore, the composition of the Ce — Zn alloy is difficult to control accurately. The ratio of the two materials to the content of the obtained alloy is deviated.
CN105441761A discloses a preparation process of Gd-Mg-Al-Zn alloy, which comprises the following steps: and smelting the Mg, Al, Zn and Mg-Gd intermediate alloy in a well-type crucible furnace, and protecting by using a covering agent during smelting to obtain an alloy melt. The alloy melt is cast in a metal ingot mold. The alloy contains elements such as Mg, Al and the like besides rare earth and Zn, and the content of Mg is relatively high.
CN1475592A discloses a preparation method of a high-zinc-aluminum rare earth magnesium alloy, which adopts a resistance crucible furnace to smelt pure magnesium, pure zinc, pure aluminum and rare earth intermediate alloy. The alloy obtained by the method also contains Mg and Al, and the specific gravity of Mg in the alloy is relatively large.
CN101100732A discloses a preparation method of a binary alloy plating material, which comprises the steps of smelting Zn, RE and trace elements in a smelting furnace, stirring, refining, deslagging, and casting into an alloy ingot. The deviation between the content of the rare earth in the alloy obtained by the method and the content of the rare earth in the original feeding materials is larger, and the content of impurities in the obtained alloy is higher.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for producing a Ce-Zn alloy, which can reduce variations in the content of cerium in the obtained Ce-Zn alloy. Furthermore, the Ce-Zn alloy obtained by the method has low impurity content. Another object of the present invention is to provide a Ce-Zn alloy. It is a further object of the present invention to provide a use of a smelting vessel that can reduce the deviation of the cerium content in a Ce-Zn alloy.
The technical purpose is realized by the following technical scheme.
In one aspect, the invention provides a method for producing a Ce-Zn alloy, comprising the steps of:
(1) smelting metal cerium and metal zinc in a smelting vessel, and then refining to obtain an alloy melt;
(2) casting the alloy melt to obtain a Ce-Zn alloy;
wherein, the part of the smelting vessel contacted with 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 or equal to 10.0 wt% of the total weight of the metal cerium and the metal zinc and is more than 0.
The production method according to the present invention preferably further comprises the steps of: polishing a cerium raw material, and then melting and refining to obtain metal cerium; and (4) polishing the zinc raw material to obtain the metal zinc.
According to the production method of the present invention, 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 invention, preferably, in the step (1), the refining time is 10min or more.
According to the production method of the present invention, 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.
In another aspect, the present invention provides a Ce-Zn alloy prepared by the above method.
According to the Ce-Zn alloy, the content of oxygen element in the Ce-Zn alloy is less than or equal to 0.002 wt%, the content of phosphorus element is less than or equal to 0.01 wt%, the content of sulfur element is less than or equal to 0.01 wt%, and the content of carbon element is less than or equal to 0.008 wt%.
According to the Ce-Zn alloy, preferably, the deviation of the content of the cerium element in the Ce-Zn alloy is less than or equal to 0.008; the deviation of the content of the 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 wt%;
wherein beta represents the content of cerium element in the Ce-Zn alloy, and the unit is wt%.
In a further aspect, the present invention provides a use of a smelting vessel for reducing the deviation of the Ce element content in a Ce-Zn alloy, wherein a part of the smelting vessel, which is in contact with metallic cerium and metallic zinc used for forming the Ce-Zn alloy, is formed by one or more of the following substances: tungsten, tantalum, cerium oxide;
the content of cerium element in the Ce-Zn alloy is more than zero and less than or equal to 10.0 wt%;
the deviation of the content of the 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 wt%;
wherein beta represents the content of cerium element in the Ce-Zn alloy, and the unit is wt%.
The use according to the invention preferably comprises the following steps:
(1) smelting metal cerium and metal zinc in a smelting vessel, and then refining to obtain an alloy melt;
(2) casting the alloy melt to obtain a Ce-Zn alloy;
wherein the content of the metal cerium is less than or equal to 10.0 wt% of the total weight of the metal cerium and the metal zinc and is more than 0.
The invention discovers that the part of the smelting vessel, which is in contact with the metal cerium and the metal zinc, is made of a specific material, so that the deviation of the content of the cerium element in the prepared Ce-Zn alloy can be reduced, and the content of the cerium element in the Ce-Zn alloy can be accurately controlled. Furthermore, the Ce-Zn alloy prepared by the method has low content of impurity elements.
Detailed Description
The present invention will be further described with reference to specific examples, but the scope of the present invention is not limited thereto.
The smelting vessel is a container for bearing the metal cerium and the 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 "inner surface of the smelting vessel" in the invention refers to the surface of the smelting vessel forming a containing cavity for containing the metal cerium and the metal zinc.
< 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
And smelting the metal cerium and the metal zinc in a smelting vessel, and refining to obtain the alloy melt. The smelting vessel only contains metal cerium and metal zinc. Of course, some unavoidable impurities, such as oxygen, phosphorus, sulfur, etc., may be contained.
The part of the smelting vessel, which is contacted 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 invention, the part of the smelting vessel that is in contact with the cerium metal and the zinc metal is formed from tungsten, tantalum or cerium oxide. Preferably, the part of the smelting vessel which is in contact with the metal cerium and the metal zinc is formed by cerium oxide. Tungsten is a simple substance of tungsten. Tantalum is a simple substance of tantalum. Preferably, the inner surface of the smelting vessel is formed from the above-mentioned substances. In certain embodiments, the entire smelting vessel is formed from the above-described materials. The application surprisingly finds that the deviation of the content of cerium in the formed Ce-Zn alloy can be reduced by adopting the smelting vessel to smelt and refine the metal cerium and the metal zinc.
In the smelting raw materials, the content of the metal cerium is less than 10.0 wt% 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 8.0 wt%; most preferably 2.0 to 7.0 wt%.
Polishing a 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 metal cerium is less than or equal to 0.02 wt%; preferably, the oxygen content is 0.008 wt.% or less. The content of phosphorus in the metal cerium is less than or equal to 0.03 wt%; preferably, the cerium metal has a phosphorus content of < 0.01 wt.%. The sulfur content in the metal cerium is less than or equal to 0.02 wt%; preferably, the sulfur content is < 0.0050 wt%.
The content of the metal zinc in the smelting raw materials is more than 90 wt% of the total weight of the metal cerium and the metal zinc and is less than 100 wt%; 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 metal zinc is 92-98.5 wt% of the total weight of the metal cerium and the metal zinc; most preferably, the content of the metal zinc is 93-98 wt% of the total weight of the metal cerium and the metal zinc.
And (4) polishing the zinc raw material to obtain the metal zinc. And (4) grinding can remove impurities on the surface of the metal zinc.
The smelting temperature of the metal cerium and the metal zinc can be 500-850 ℃; preferably 600-800 ℃; more preferably 650 to 750 ℃. The smelting time is based on the complete melting of zinc.
Smelting may be carried out in an inert atmosphere. Inert atmospheres include, but are not limited to, helium, neon, argon, and the like. According to one embodiment of the invention, the inert atmosphere is argon. The smelting pressure is 0.01-0.06 MPa; preferably 0.02-0.05 MPa; more preferably 0.03 to 0.04 MPa. Melting may be carried out in a vacuum melting furnace. According to one embodiment of the invention, the vacuum melting furnace is vacuumized to below 10Pa, and then inert gas is filled into the vacuum melting furnace to form a melting environment with the above pressure and inert atmosphere.
Refining time is more than 10 min; preferably, the refining time is 20-120 min; more preferably, the refining time is 30-60 min. This ensures sufficient alloying of cerium with zinc. The refining may be carried out in a vacuum melting furnace.
Step of forming Ce-Zn alloy
And 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, a step of cooling the cast alloy ingot may also be included.
< Ce-Zn alloy >
The Ce-Zn alloy is prepared by the method. The Ce-Zn alloy consists of cerium and zinc. Of course, the Ce-Zn alloy may include unavoidable impurities such as oxygen, phosphorus, sulfur, or carbon.
The content of oxygen element in the Ce-Zn alloy is less than or equal to 0.002 wt%; preferably, the content of the oxygen element is less than or equal to 0.0015 wt%; more preferably, the content of the oxygen element is less than or equal to 0.0012 wt%. The content of phosphorus element in the Ce-Zn alloy is less than or equal to 0.01 wt%; preferably, the content of the phosphorus element is less than or equal to 0.006 wt%; more preferably, the content of phosphorus element is < 0.0050 wt%. The content of sulfur element in the Ce-Zn alloy is less than or equal to 0.01 wt%; preferably, the content of the sulfur element is less than or equal to 0.006 wt%; more preferably, the content of elemental sulphur is < 0.0050 wt%. The content of carbon element in the Ce-Zn alloy is less than or equal to 0.008 wt%; preferably, the content of the carbon element is less than or equal to 0.007wt percent; more preferably, the content of carbon element is less than or equal to 0.0065 wt%.
The deviation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.008; preferably, the content deviation of the cerium element in the Ce-Zn alloy is less than or equal to 0.005; more preferably, the deviation of the content of the cerium element in the Ce-Zn alloy is less than or equal to 0.002; most preferably, the variation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.0000001. In certain embodiments, the deviation in the cerium content of the Ce-Zn alloy may be zero. The deviation of the cerium content 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 wt%;
wherein beta represents the content of cerium element in the Ce-Zn alloy, and the unit is wt%.
< use of melting vessel >
The application discovers that the part of the smelting vessel, which is in contact with the metal cerium and the metal zinc, is made of a specific material, so that the deviation of the content of cerium in the prepared Ce-Zn alloy can be reduced. Thus, the invention provides the use of a smelting vessel for reducing the deviation of the cerium content in a Ce-Zn alloy.
The part of the smelting vessel, which is contacted 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 invention, the part of the smelting vessel that is in contact with the cerium metal and the zinc metal is formed from tungsten, tantalum or cerium oxide. Preferably, the part of the smelting vessel which is in contact with the metal cerium and the metal zinc is formed by cerium oxide. Tungsten is a simple substance of tungsten. Tantalum is a simple substance of tantalum. Preferably, the inner surface of the smelting vessel is formed from the above-mentioned substances. In certain embodiments, the entire smelting vessel is formed from the above-described materials.
The content of cerium element in the Ce-Zn alloy is more than zero and less than or equal to 10.0 wt%; preferably 0.2 to 9.0 wt%; more preferably 1.5 to 8.0 wt%; most preferably 2.0 to 7.0 wt%.
The content of zinc element in the Ce-Zn alloy is less than 100 wt% and more than or equal to 90 wt%; preferably 91-99.8 wt%; more preferably 92-98.5 wt%; most preferably 93 to 98 wt%.
The deviation of the cerium content 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 wt%;
wherein beta represents the content of cerium element in the 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 content deviation of the cerium element in the Ce-Zn alloy is less than or equal to 0.005; more preferably, the deviation of the content of the cerium element in the Ce-Zn alloy is less than or equal to 0.002; most preferably, the variation of the content of cerium element in the Ce-Zn alloy is less than or equal to 0.0000001. In certain embodiments, the deviation in the cerium content of the Ce-Zn alloy may be zero.
Specifically, the method comprises the following steps: (1) smelting metal cerium and metal zinc in a smelting vessel, and then refining to obtain an alloy melt; (2) and casting the alloy melt to obtain the Ce-Zn alloy. The selection of the raw materials and the specific operations of the steps are as described above, and are not described herein again.
The following describes the test method of the content of each element in the Ce-Zn alloy:
cerium element: measuring by using an inductively coupled plasma emission spectrometer (ICP-OES);
carbon element (C): measuring with infrared carbon-sulfur analyzer (LECO-400, available from Like corporation, USA);
elemental sulfur: measuring with infrared carbon-sulfur analyzer (LECO-400, available from Like corporation, USA);
phosphorus element: measuring with spectrophotometer (model number 722, purchased from Shanghai precision instruments and factories);
oxygen element: measuring with oxygen nitrogen hydrogen analyzer (type ONH-2000).
The deviation of the cerium element in the 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 wt%;
wherein beta represents the content of cerium element in the Ce-Zn alloy, and the unit is wt%.
Example 1
And polishing the electrolyzed cerium raw material, and then melting and refining in a vacuum melting furnace to obtain the metal cerium. The content of oxygen element in the metal cerium is less than or equal to 0.008 wt%, the content of phosphorus element is less than 0.01 wt%, and the content of sulfur element is less than 0.0050 wt%.
And grinding the zinc raw material to obtain the metal zinc.
5.5 parts by weight of metallic cerium and 94.5 parts by weight of metallic zinc were placed in a crucible, the inner wall of which was formed of a simple substance of tungsten. And smelting the crucible in an argon atmosphere at the pressure of 0.03MPa and the temperature of 700 ℃ until the zinc is completely molten, and then refining for 30min to obtain the alloy melt.
And casting the alloy melt into a water-cooled copper ingot mold, and cooling to room temperature to obtain the Ce-Zn alloy.
The properties of the resulting alloy are shown in table 1.
Example 2
The same procedure as in example 1 was repeated, except that the inner wall of the crucible was formed of elemental tantalum. The properties of the resulting alloy are shown in table 1.
Example 3
The same procedure as in example 1 was repeated, except that the inner wall of the crucible was formed of cerium oxide. The properties of the resulting alloy are shown in table 1.
Comparative example 1
The same procedure as in example 1 was repeated, except that the inner wall of the crucible was made of magnesium oxide. The properties of the resulting alloy are shown in table 1.
TABLE 1
The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.
Claims (10)
1. A production method of Ce-Zn alloy is characterized by comprising the following steps:
(1) smelting metal cerium and metal zinc in a smelting vessel, and then refining to obtain an alloy melt;
(2) casting the alloy melt to obtain a Ce-Zn alloy;
wherein, the part of the smelting vessel contacted with 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 or equal to 10.0 wt% of the total weight of the metal cerium and the metal zinc and is more than 0.
2. The production method according to claim 1, further comprising the steps of:
polishing a cerium raw material, and then melting and refining to obtain metal cerium;
and (4) polishing the zinc raw material to obtain the metal zinc.
3. The production method according to claim 1, wherein the smelting conditions are as follows: the smelting temperature is 500-850 ℃, and the smelting pressure is 0.01-0.06 MPa.
4. The production method according to claim 1, wherein in the step (1), the refining time is 10min or more.
5. The production method according to claim 1, wherein 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.
6. The Ce-Zn alloy is characterized by being prepared by the production method of any one of claims 1 to 5.
7. The Ce-Zn alloy according to claim 6, wherein the Ce-Zn alloy contains 0.002 wt% or less of oxygen element, 0.01 wt% or less of phosphorus element, 0.01 wt% or less of sulfur element and 0.008 wt% or less of carbon element.
8. The Ce-Zn alloy according to claim 6, wherein the Ce-Zn alloy has a variation of cerium of 0.008 or less; the deviation of the content of the 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 wt%;
wherein beta represents the content of cerium element in the Ce-Zn alloy, and the unit is wt%.
9. Use of a smelting vessel for reducing the deviation of the Ce element content in a Ce-Zn alloy, characterized in that:
the part of the smelting vessel, which is contacted with the metal cerium and the metal zinc for forming the Ce-Zn alloy, is formed by one or more of the following substances: tungsten, tantalum, cerium oxide;
the content of cerium element in the Ce-Zn alloy is more than zero and less than or equal to 10.0 wt%;
the deviation of the content of the 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 wt%;
wherein beta represents the content of cerium element in the Ce-Zn alloy, and the unit is wt%.
10. Use according to claim 9, characterized in that it comprises the following steps:
(1) smelting metal cerium and metal zinc in a smelting vessel, and then refining to obtain an alloy melt;
(2) casting the alloy melt to obtain a Ce-Zn alloy;
wherein the content of the metal cerium is less than or equal to 10.0 wt% of the total weight of the metal cerium and the metal zinc and is more than 0.
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