CN114657420B - Light rare earth-zinc alloy, preparation method and application thereof and application of smelting container - Google Patents
Light rare earth-zinc alloy, preparation method and application thereof and application of smelting container Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
- C23C2/06—Zinc or cadmium or alloys based thereon
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Abstract
The application discloses a light rare earth-zinc alloy, a preparation method and application thereof, and an application of a smelting container. The light rare earth-zinc alloy and the preparation method thereof comprise the following steps: smelting raw materials consisting of light rare earth metal and zinc in a smelting container, and then refining and casting to obtain a light rare earth-zinc alloy; wherein the light rare earth metal is selected from one or more of lanthanum, praseodymium or neodymium; the light rare earth metal is 0 to 10.0 weight percent of the total weight of the raw materials, but does not contain 0, and the balance is zinc; the contact part of the smelting container and the raw material is formed by tungsten. The preparation method can reduce the deviation of the content of the light rare earth elements in the light rare earth-zinc alloy.
Description
Technical Field
The application relates to a light rare earth-zinc alloy, a preparation method and application thereof, and also relates to application of a smelting container.
Background
The steel is easy to corrode in the use process, and serious economic loss is caused. Galvanization of steel surfaces is a relatively effective measure in preventing corrosion of steel. The addition of proper rare earth elements in zinc can improve the performance of the plating layer, reduce the thickness of the plating layer and increase the corrosion resistance of the plating layer. However, zinc has a low melting point (about 419.5 ℃) and rare earth metals have a high melting point (about 798-1663 ℃) and have extremely low solubility in zinc, and both are difficult to smelt together; and the rare earth metal has strong activity and is easy to oxidize in the smelting process. The traditional smelting method has the problems that the alloy components are difficult to control accurately, the impurity elements are difficult to control and the like.
CN101100732a discloses a method for preparing a binary alloy plating material, wherein the binary alloy consists of Zn and RE, and the material further comprises trace additive elements, and the total content of the trace additive elements is below 0.5%; adding the elements into a smelting furnace according to the alloy composition in proportion for smelting, stirring, refining, deslagging and casting into alloy ingots.
CN111334688A discloses a method for preparing Zn-RE series zinc alloy, which comprises mixing pure zinc and nonradioactive rare earth element RE to obtain a mixture; in CO 2 And SF (sulfur hexafluoride) 6 Under the protection of atmosphere, the mixture is placed in a jade crucible or a graphite crucible for smelting, and the Zn-RE zinc alloy is obtained after casting and cooling.
However, the alloy obtained by the method disclosed in the prior art 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
Accordingly, an object of the present application is to provide a method for preparing a light rare earth-zinc alloy, which has small deviation of the content of light rare earth elements in the light rare earth-zinc alloy. Further, the light rare earth-zinc alloy has lower impurity content.
It is another object of the present application to provide a light rare earth-zinc alloy.
It is a further object of the present application to provide the use of a light rare earth-zinc alloy.
It is a further object of the present application to provide the use of a smelting vessel that is capable of reducing the variation in the content of light rare earth elements in light rare earth-zinc alloys.
In one aspect, the application provides a method for preparing a light rare earth-zinc alloy, comprising the following steps:
smelting raw materials consisting of light rare earth metal and zinc in a smelting container, and then refining and casting to obtain a light rare earth-zinc alloy;
wherein the light rare earth metal is selected from one or more of lanthanum, praseodymium or neodymium; the light rare earth metal is 0 to 10.0 weight percent of the total weight of the raw materials, but does not contain 0, and the balance is zinc; the contact part of the smelting container and the raw material is formed by tungsten.
According to the preparation method of the present application, preferably, the light rare earth has an oxygen content of 0.02wt% or less, a phosphorus content of 0.03wt% or less, and a sulfur content of 0.02wt% or less.
According to the production method of the present application, preferably, the smelting is performed in an inert atmosphere; the smelting temperature is 460-800 ℃, and the smelting pressure is 0.01-0.06 MPa.
According to the preparation method of the application, preferably, the refined raw material is cast into a water-cooled ingot mould or an ingot mould with electromagnetic stirring function, so as to obtain the light rare earth-zinc alloy.
In another aspect, the present application provides a light rare earth-zinc alloy prepared by the above method.
According to the light rare earth-zinc alloy of the present application, preferably, the deviation of the content of the light rare earth element in the light rare earth-zinc alloy is not more than 0.004;
wherein, the deviation of the content of the light rare earth element in the light rare earth-zinc alloy is calculated by the following formula:
|X-I|/X；
wherein X represents the content of light rare earth metals in the raw materials, and the unit is weight percent;
i represents the content of light rare earth elements in the light rare earth-zinc alloy, and the unit is wt%.
In yet another aspect, the present application provides the use of the light rare earth-zinc alloy described above in the preparation of a rare earth zinc coating.
According to the use of the present application, preferably, the light rare earth-zinc alloy is added to a zinc bath, and a rare earth zinc plating layer is formed on the surface of an object to be plated by a hot dip plating method.
In a further aspect, the application provides the use of a smelting vessel formed from tungsten at a location in contact with a feedstock for forming a light rare earth-zinc alloy to reduce the bias in the content of light rare earth elements in the light rare earth-zinc alloy;
the light rare earth element in the light rare earth-zinc alloy is selected from one or more of lanthanum, praseodymium or neodymium; the light rare earth element content in the light rare earth-zinc alloy is 0-10.0 wt%, but does not contain 0, and the balance is zinc;
the deviation of the content of the light rare earth elements in the light rare earth-zinc alloy is calculated by adopting the following formula:
|X-I|/X；
wherein X represents the content of light rare earth metals in the raw materials, and the unit is weight percent;
i represents the content of light rare earth elements in the light rare earth-zinc alloy, and the unit is wt%.
The use according to the application preferably comprises the steps of: smelting raw materials consisting of light rare earth metal and zinc in a smelting container, and then refining and casting to obtain a light rare earth-zinc alloy;
wherein the light rare earth metal is selected from one or more of lanthanum, praseodymium or neodymium; the light rare earth metal is 0 to 10.0 weight percent of the total weight of the raw materials, but does not contain 0, and the balance is zinc.
The application reduces the deviation of the content of the light rare earth elements in the light rare earth-zinc alloy and solves the long-term problem that the components of the light rare earth-zinc alloy are difficult to accurately control by selecting the specific smelting container material contacted with the raw materials. The light rare earth-zinc alloy obtained by the preparation method has low impurity content.
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 deviation of the content of the light rare earth elements in the light rare earth-zinc alloy is calculated by the following formula: i X-I/X; wherein X represents the content of light rare earth metals in the raw materials, and the unit is weight percent; i represents the content of light rare earth elements in the light rare earth-zinc alloy, and the unit is wt%.
< preparation method of light rare-earth-Zinc alloy >
The preparation method of the light rare earth-zinc alloy comprises the following steps: smelting raw materials consisting of light rare earth metal and zinc in a smelting container, and then refining and casting to obtain the light rare earth-zinc alloy.
The raw materials of the application consist of light rare earth metals and zinc. Of course, the feedstock may include some unavoidable impurities such as oxygen, phosphorus, sulfur, and the like.
The light rare earth metal is selected from one of lanthanum, praseodymium and neodymium. In certain embodiments, the light rare earth metal is lanthanum or praseodymium. In other embodiments, the light rare earth metal is neodymium. The oxygen content in the light rare earth metal is less than or equal to 0.02wt%; preferably, the oxygen content in the light rare earth metal is less than or equal to 0.008wt%. The phosphorus content in the light rare earth metal is less than or equal to 0.03wt%; preferably, the phosphorus content in the light rare earth metal is < 0.01wt%. The sulfur content in the light rare earth metal is less than or equal to 0.02wt%; preferably, the sulfur content in the light rare earth metal is < 0.0050wt%. The light rare earth metal material may be subjected to a pretreatment to obtain a light rare earth metal that meets the above-mentioned oxygen, phosphorus, sulfur contents. The light rare earth metal material may be light rare earth metal obtained by electrolysis. The pretreatment step may include grinding, melting, refining, and the like.
Light rare earth metal is 0-10.0 wt% (excluding 0) of the total weight of the raw materials; preferably 0.2 to 5.0 wt.%; more preferably 0.5 to 4.0wt%; most preferably 1.0 to 3.0wt%.
The zinc may be zinc obtained by pretreating zinc metal. The pretreatment step may include sanding or the like. Zinc is 90-100 wt% (excluding 100%) of the total weight of the raw materials; preferably 95 to 99.8 wt.%; more preferably 96 to 99.5%; most preferably 97 to 99wt%.
The smelting vessel is a vessel for carrying raw materials in the processes of smelting, refining and the like. Such as a crucible, etc. The part of the smelting vessel in contact with the raw material is formed of tungsten. Tungsten is a simple metal. Preferably, the inner surface of the smelting vessel is formed from tungsten. The inner surface of the smelting vessel refers to the surface that forms the feed material containment cavity. Of course, the entire smelting vessel may be formed of tungsten. The application surprisingly finds that the deviation of the content of the light rare earth elements in the formed light rare earth-zinc alloy can be reduced by adopting the smelting container to smelt and refine raw materials.
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. The smelting pressure can be 0.01-0.06 MPa; preferably 0.02-0.05 MPa; more preferably 0.03 to 0.04MPa. The smelting temperature can be 460-800 ℃; preferably 550 to 750 ℃; more preferably 670 to 700 ℃. The smelting time is based on the complete melting of zinc. Smelting may be performed in a vacuum smelting furnace.
Refining time is longer than 10min; preferably, the refining time is 20-120 min; more preferably, the refining time is 30 to 60 minutes. Thus, the light rare earth and zinc can be fully alloyed. Refining may be performed in a vacuum melting furnace.
Casting the refined raw materials to obtain the light rare earth-zinc 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.
< light rare earth-zinc alloy and use thereof >
The light rare earth-zinc alloy is prepared by adopting the method. The deviation of the content of the light rare earth elements in the light rare earth-zinc alloy is less than or equal to 0.004; preferably, the deviation of the content of the light rare earth elements in the light rare earth-zinc alloy is less than or equal to 0.0035; more preferably, the deviation of the content of the light rare earth element in the light rare earth-zinc alloy is less than or equal to 0.0000001. In certain embodiments, the deviation in the light rare earth element content in the light rare earth-zinc alloy may be zero.
The light rare earth-zinc alloy can be applied to preparing rare earth zinc plating layers. The application also provides application of the light rare earth-zinc alloy in preparing rare earth zinc coating. Specifically, the method comprises the following steps:
adding the light rare earth-zinc alloy into zinc bath, and forming rare earth zinc coating on the surface of the to-be-plated object by adopting a hot dip plating method.
The light rare earth-zinc alloy may be added to the zinc bath through multiple addition points. The number of the adding points can be 5, 10 or 15, etc. The light rare earth-zinc alloy may be used in the form of a light rare earth-zinc alloy block. The weight of each light rare earth-zinc alloy is less than 100kg; preferably 5 to 30kg; more preferably 9 to 11kg. The temperature of the zinc bath can be 350-600 ℃; preferably 400-550 ℃; more preferably 450 to 500 ℃.
The article to be plated may be formed of steel. For example, it may be a steel plate.
< use of melting vessel >
The application discovers that the deviation of the content of the light rare earth elements in the light rare earth-zinc alloy can be reduced by putting the raw materials into a smelting container formed by specific materials for smelting, refining and the like. Thus, the present application provides the use of a smelting vessel for reducing the bias in the content of light rare earth elements in a light rare earth-zinc alloy.
The part of the smelting vessel in contact with the raw material is formed of tungsten. The smelting vessel is a vessel for carrying raw materials in the processes of smelting, refining and the like. Such as a crucible, etc. Preferably, the inner surface of the smelting vessel is formed from tungsten. The inner surface of the smelting vessel refers to the surface that forms the feed material containment cavity. Of course, the entire smelting vessel may be formed of tungsten.
The light rare earth element in the light rare earth-zinc alloy is selected from one or more of lanthanum, praseodymium or neodymium. In certain embodiments, the light rare earth element is selected from one of lanthanum, praseodymium. In other embodiments, the light rare earth element is neodymium. The content of the light rare earth element in the light rare earth-zinc alloy is 0 to 10.0wt% (excluding 0); preferably 0.2 to 5.0 wt.%; more preferably 0.5 to 4.0wt%; most preferably 1.0 to 3.0wt%.
The content of zinc element in the light rare earth-zinc alloy is 90-100 wt% (excluding 100%); preferably 95 to 99.8 wt.%; more preferably 96 to 99.5%; most preferably 97 to 99wt%.
The deviation of the content of the light rare earth elements in the light rare earth-zinc alloy is calculated by adopting the following formula:
|X-I|/X；
wherein X represents the content of light rare earth metals in the raw materials, and the unit is weight percent;
i represents the content of light rare earth elements in the light rare earth-zinc alloy, and the unit is wt%.
The deviation of the content of the light rare earth elements in the light rare earth-zinc alloy is less than or equal to 0.004; preferably, the deviation of the content of the light rare earth elements in the light rare earth-zinc alloy is less than or equal to 0.0035; more preferably, the deviation of the content of the light rare earth element in the light rare earth-zinc alloy is less than or equal to 0.0000001. In certain embodiments, the deviation in the light rare earth element content in the light rare earth-zinc alloy may be zero.
Specifically, the method comprises the following steps: smelting raw materials consisting of light rare earth metal and zinc in a smelting container until the zinc is molten, and then refining and casting to obtain the light rare earth-zinc 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 test method is described as follows:
the rare earth content in the light rare earth-zinc alloy is measured by an inductively coupled plasma emission spectrometer (ICP-OES);
the carbon and sulfur content of the light rare earth-zinc alloy was determined using an infrared carbon sulfur analyzer (model LECO-400, purchased from the american lacca company);
the phosphorus content in the light rare earth-zinc alloy is measured by a spectrophotometer (model 722, purchased from Shanghai precision instruments factory);
the oxygen content in the light rare earth-zinc alloy is measured by an oxygen-nitrogen-hydrogen analyzer (model number is ONH-2000).
Preparation example 1
And polishing the metal zinc to remove impurities on the surface of the metal zinc, thereby obtaining zinc.
Preparation example 2
Polishing the metal lanthanum obtained by electrolysis, and then melting and refining the polished metal lanthanum in a vacuum melting furnace to obtain lanthanum. The oxygen content in the obtained lanthanum 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%.
Preparation example 3
The metal praseodymium obtained by electrolysis was treated in the same manner as in preparation example 2 to obtain praseodymium. The oxygen content in the obtained praseodymium 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%.
Preparation example 4
The electrolytic neodymium metal was treated in the same manner as in preparation example 2 to obtain neodymium. The oxygen content in the obtained neodymium 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%.
Examples 1 to 3 and comparative examples 1 to 5
(1) Placing a raw material consisting of zinc and light rare earth metal obtained in preparation example 1 into a crucible; placing the crucible in a smelting furnace; vacuumizing the pressure in the smelting furnace to below 10Pa, and then filling argon into the smelting furnace to enable the pressure in the smelting furnace to be 0.03MPa; heating the temperature in the smelting furnace to the smelting temperature for smelting until the zinc is completely melted;
(2) Refining the smelted raw materials for 30min;
(3) Casting the refined raw materials into a water-cooled copper ingot mould, and cooling to room temperature to obtain the light rare earth-zinc alloy.
Specifically, the results are shown in Table 1. The contents of light rare earth elements and impurities in the obtained alloy are shown in Table 2.
TABLE 1
Note that: the inner wall of the crucible means the surface forming the raw material accommodating cavity.
TABLE 2
Note that: the deviation of the content of the light rare earth element is calculated by adopting the following formula: i X-I/X;
wherein X represents the content of light rare earth metals in the raw materials, and the unit is weight percent; i represents the content of light rare earth elements in the light rare earth-zinc alloy, and the unit is wt%.
Example 4
The plurality of light rare earth-zinc alloy blocks (10 kg/block) obtained in example 1 were added to a zinc bath at 10 addition points, the temperature of the zinc bath was controlled to 460 ℃, and a rare earth zinc plating layer was formed on the surface of a steel product (steel sheet) to be plated by a hot dip plating method.
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 (2)
1. Use of a smelting vessel for reducing deviations in the content of light rare earth elements in a light rare earth-zinc alloy, comprising the steps of:
placing raw materials consisting of light rare earth metal and zinc into a smelting container, smelting at 550-750 ℃, refining for 30-60 min, and casting into a water-cooled ingot mould to obtain light rare earth-zinc alloy; the water-cooled ingot mould is formed by copper;
wherein the light rare earth metal is selected from one or more of lanthanum, praseodymium or neodymium; the light rare earth metal is 1.0-3.0 wt% of the total weight of the raw materials, and the balance is zinc; the oxygen content in the light rare earth metal 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 inner surface of the smelting container is formed by tungsten, and the inner surface of the smelting container refers to the surface forming the raw material accommodating cavity;
wherein, the deviation of the content of the light rare earth element in the obtained light rare earth-zinc alloy is less than or equal to 0.0035;
the deviation of the content of the light rare earth elements in the light rare earth-zinc alloy is calculated by adopting the following formula:
|X-I|/X；
wherein X represents the content of light rare earth metals in the raw materials, and the unit is weight percent; i represents the content of light rare earth elements in the light rare earth-zinc alloy, and the unit is wt%.
2. The use according to claim 1, characterized in that the smelting is performed in an inert atmosphere; the smelting temperature is 670-700 ℃ and the smelting pressure is 0.01-0.06 MPa.
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| CN214120756U (en) * | 2020-12-22 | 2021-09-03 | 包头稀土研究院 | Furnace cover for rare earth alloy smelting furnace and smelting furnace |
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| AT15378U1 (en) * | 2016-02-05 | 2017-07-15 | Plansee Se | crucible |
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