CN114717432A - Zinc holmium alloy, method for the production thereof and use of a container - Google Patents

Zinc holmium alloy, method for the production thereof and use of a container Download PDF

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Publication number
CN114717432A
CN114717432A CN202210366225.3A CN202210366225A CN114717432A CN 114717432 A CN114717432 A CN 114717432A CN 202210366225 A CN202210366225 A CN 202210366225A CN 114717432 A CN114717432 A CN 114717432A
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Prior art keywords
holmium
zinc
alloy
content
metal
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Granted
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CN202210366225.3A
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CN114717432B (en
Inventor
刘玉宝
赵二雄
高日增
杨鹏飞
李园
张洋
吕卫东
黄海涛
张全军
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Baotou Rare Earth Research Institute
Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd
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Baotou Rare Earth Research Institute
Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd
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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
    • 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
    • C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The invention discloses a zinc-holmium alloy, a production method thereof and application of a container. The production method of the zinc-holmium alloy comprises the steps of smelting and refining raw materials consisting of metal holmium and metal zinc in a container; wherein at least a portion of the interior surface of the vessel is for contact with the feedstock, the at least a portion of the interior surface being formed from metallic tantalum. The production method can accurately control the content of holmium element in the zinc-holmium alloy.

Description

Zinc holmium alloy, method for the production thereof and use of a container
Technical Field
The invention relates to a zinc-holmium alloy and a production method thereof, and also relates to application of a container.
Background
The corrosion resistance and other performances of the zinc coating can be improved by adding a certain amount of rare earth elements into the zinc coating. The difference between the melting point of zinc and the melting point of rare earth elements is large, and the zinc and the rare earth elements are difficult to be smelted together. The rare earth elements are active in property and easy to oxidize to form a compound with a high melting point. These result in high impurity levels in the zinc rare earth alloy and difficult to control with precision in composition.
CN1105709A discloses a production process of rare earth zinc-copper alloy, which is to form copper and zinc into binary intermediate alloy liquid; forming a ternary intermediate alloy by the binary intermediate alloy liquid and the rare earth metal; and adding the zinc liquid into the ternary intermediate alloy, and then refining and casting to obtain the rare earth zinc-copper alloy. CN1405342A discloses a preparation process of an alloy, which comprises the steps of firstly melting zinc, then adding pure iron, and refining after the pure iron is completely melted; and adding mixed rare earth into the zinc-iron alloy liquid obtained after refining, and casting an alloy ingot when the alloy liquid reaches a specified temperature. CN1475592A discloses a preparation method of a 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 metal mold casts a tensile bar. Solution heat treatment is carried out in a box type electric furnace. The alloy obtained by the method contains a certain amount of other metal elements besides zinc and rare earth elements.
CN101100732A discloses a preparation method of a binary alloy plating material, which comprises the steps of adding Zn, RE and trace additive elements into a smelting furnace according to a proportion, smelting, stirring, refining, deslagging, and casting into an alloy ingot. CN111334688A discloses a preparation method of Zn-RE series zinc alloy, which comprises the step of mixing a mixture formed by pure zinc and non-radioactive rare earth element RE in CO2And SF6Under the protection of atmosphere, the mixture is placed in a jade crucible or a graphite crucible for smelting, and the Zn-RE series zinc alloy is obtained after casting and cooling. The content of the rare earth in the alloy obtained by the methods has larger deviation with the content of the rare earth in the original feeding materials, and the obtained alloy has more impurity content.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for producing a zinc-holmium alloy, which can accurately control the holmium element content in the zinc-holmium alloy and reduce the holmium element content deviation. Furthermore, the content of impurity elements in the zinc-holmium alloy is low. Another object of the present invention is to provide a zinc holmium alloy. It is a further object of the present invention to provide a use of the container.
The technical purpose is achieved through the following technical scheme.
In one aspect, the present invention provides a production method of a zinc-holmium alloy, comprising the steps of smelting and refining a raw material consisting of metal holmium and metal zinc in a vessel;
wherein at least a portion of the interior surface of the vessel is for contact with the feedstock, the at least a portion of the interior surface being formed from metallic tantalum.
According to the production method of the present invention, preferably, the entire inner surface of the container is formed of metallic tantalum.
According to the production method, the smelting temperature is preferably 600-1200 ℃, and the smelting pressure is preferably 0.005-0.07 MPa.
According to the production method of the present invention, preferably, the melting is performed under an inert atmosphere.
According to the production method of the present invention, preferably, the method further comprises the step of casting the alloy melt formed by melting and refining into a mold to form a zinc-holmium alloy; wherein the mold is a mold with a cooling water passage or a mold with a stirring function.
According to the production method of the present invention, preferably, the content of metal holmium in the raw material is 10 wt% or less.
According to the production method, the content deviation phi of holmium elements in the zinc-holmium alloy is preferably less than or equal to 0.006;
Φ＝|a/b-1|
wherein a represents the content of holmium element in the zinc-holmium alloy, and the unit is wt%; b represents the content of metal holmium in wt% of the raw materials for forming the zinc-holmium alloy.
In another aspect, the invention provides a zinc holmium alloy prepared by the above production method.
In another aspect, the invention provides a use of a container in reducing content deviation of holmium element in zinc-holmium alloy, wherein the content deviation Φ of holmium element in zinc-holmium alloy is calculated by adopting the following formula:
Φ＝|a/b-1|
wherein a represents the content of holmium element in the zinc-holmium alloy, and the unit is wt%; b represents the content of metal holmium in the raw materials for forming the zinc-holmium alloy, and the unit is weight percent;
wherein at least a portion of the interior surface of the vessel is for contact with the feedstock, the at least a portion of the interior surface being formed from metallic tantalum.
According to the use of the present invention, preferably, the content of holmium element in the zinc-holmium alloy is less than or equal to 10 wt%; phi is less than or equal to 0.006.
The production method can accurately control the holmium element content in the zinc-holmium alloy and reduce the holmium element content deviation. In addition, the zinc-holmium alloy prepared by the production method has low impurity content.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
< production method of Zinc-holmium alloy >
The production method of the zinc-holmium alloy comprises the steps of smelting and refining raw materials consisting of metal holmium and metal zinc in a container; the method can also comprise the step of casting the alloy melt formed by smelting and refining into a mould to form the zinc-holmium alloy. In certain embodiments, a step of pretreating raw material zinc to obtain metal zinc and/or a step of pretreating raw material holmium to obtain holmium can also be included. As described in detail below.
The invention carries out smelting and refining on raw materials consisting of metal holmium and metal zinc in a container to form alloy melt. The raw material of the invention can also comprise some inevitable impurity elements, such as oxygen element, phosphorus element, sulfur element and the like, besides holmium element and zinc element.
The metal holmium in the raw material is an essential raw material. The content of metal holmium in the raw materials is more than 0; preferably, the content of the metal holmium in the raw material is more than or equal to 0.02 wt%; more preferably, the content of metal holmium in the raw material is 3 wt% or more. The content of metal holmium in the raw materials is less than or equal to 10 wt%; preferably, the content of metal holmium in the raw material is less than or equal to 9 wt%; more preferably, the content of metal holmium in the raw material is 8 wt% or less.
The content of oxygen element in the metal holmium is less than or equal to 0.02 wt%; preferably, the content of oxygen element in the metal holmium is less than or equal to 0.008 wt%. The content of phosphorus element in the metal holmium is less than or equal to 0.03 wt%; preferably, the content of phosphorus element in the metal holmium is less than 0.01 wt%. The sulfur content in the metal holmium is less than or equal to 0.02 wt%; preferably, the sulphur content in the holmium metal is < 0.005 wt%.
The sum of the mass of the metal zinc and the metal holmium is 100 wt% of the mass of the raw materials. The content of metallic zinc in the raw material can be calculated by subtracting the content of metallic holmium in the raw material from 100 wt%. The content of metal zinc in the raw material is less than 100 wt%; preferably, the content of metallic zinc in the raw material is less than or equal to 99.8 wt%; more preferably, the content of metallic zinc in the raw material is 97 wt% or less. The content of metal zinc in the raw material is more than or equal to 90 wt%; preferably, the content of metallic zinc in the raw material is more than or equal to 91 wt%; more preferably, the content of metallic zinc in the raw material is 92 wt% or more.
The container is used for bearing raw materials in the processes of smelting, refining and the like. Examples of containers include, but are not limited to, crucibles. The portion of the vessel in contact with the feedstock is formed from metallic tantalum. Preferably, the inner surface of the raw material-containing receiving chamber of the container is formed of metallic tantalum. In certain embodiments, the container is formed from metallic tantalum. According to one embodiment of the invention, at least a portion of the inner surface of the vessel is adapted to be in contact with the feedstock, said at least a portion of the inner surface being formed of metallic tantalum. According to a preferred embodiment of the invention, the entire inner surface of the container is formed by metallic tantalum. Therefore, the content of the holmium element in the zinc-holmium alloy can be accurately controlled, and the content deviation of the holmium element is reduced.
And putting the container filled with the raw materials into a smelting furnace for smelting. The melting furnace may be a vacuum melting furnace. The smelting temperature can be 600-1200 ℃; preferably 700-1100 ℃; more preferably 800 to 1000 ℃. The smelting pressure can be 0.005-0.07 MPa; preferably 0.01 to 0.06 MPa; more preferably 0.02 to 0.04 MPa. 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.
Refining may be carried out in a smelting furnace. The melting furnace may be a vacuum melting furnace. Refining for more than 10 min; preferably, the refining time is 20-120 min; more preferably, the refining time is 30-60 min. Thus, the holmium and the zinc can be fully alloyed.
And (3) melting and refining the formed alloy solution into a mould to form the zinc-holmium alloy. The mold may be a mold having a cooling water passage or a mold with a stirring function. The mold may be formed of copper. According to one embodiment of the invention, the mould is a water-cooled copper ingot mould.
In certain embodiments, the invention may also include a step of pretreating the raw material zinc. The pretreatment is intended to remove impurities on the surface of the raw material zinc. For example, the surface of the raw material zinc is polished to obtain metallic zinc.
In certain embodiments, the invention may further comprise a step of pretreating the raw holmium material. The pretreatment aims to enable the content of each impurity in raw material holmium to meet the use requirement. For example, the surface of raw holmium is polished, and then melted and refined to obtain holmium metal.
< Zinc holmium alloy >
The zinc-holmium alloy is produced by the method. The zinc-holmium alloy consists of zinc element and holmium element. Of course, the zinc-holmium alloy may also contain some inevitable impurities, such as oxygen, phosphorus, sulfur, carbon, and the like.
The zinc-holmium alloy contains holmium element. The content of holmium element in the zinc-holmium alloy is more than 0; preferably, the content of holmium element in the zinc-holmium alloy is more than or equal to 0.02 wt%; more preferably, the content of holmium element in the zinc-holmium alloy is not less than 3 wt%. The content of holmium element in the zinc-holmium alloy is less than or equal to 10 wt%; preferably, the content of holmium element in the zinc-holmium alloy is less than or equal to 9 wt%; more preferably, the content of holmium element in the zinc-holmium alloy is less than or equal to 8 wt%.
The content of zinc element in the zinc-holmium alloy is less than 100 wt%; preferably, the content of zinc element in the zinc holmium alloy is less than or equal to 99.8 wt%; more preferably, the content of zinc element in the zinc holmium alloy is less than or equal to 97 wt%. The content of zinc element in the zinc-holmium alloy is more than or equal to 90 wt%; preferably, the content of zinc element in the zinc holmium alloy is more than or equal to 91 wt%; more preferably, the content of zinc element in the zinc holmium alloy is equal to or more than 92 wt%.
The content of oxygen element in the zinc holmium alloy is less than or equal to 0.002 wt%; preferably, the content of the oxygen element is 0.0013 wt% or less. The content of phosphorus element in the zinc holmium alloy is less than or equal to 0.01 wt%; preferably, the content of phosphorus element is less than 0.005 wt%. The content of sulfur element in the zinc holmium alloy is less than or equal to 0.01 wt%; preferably, the content of elemental sulphur is less than 0.005 wt%. The content of carbon element in the zinc holmium alloy is less than or equal to 0.006 wt%; preferably, the content of carbon element is 0.005 wt% or less.
The content deviation of holmium element in the zinc-holmium alloy can be expressed by phi. Phi is less than or equal to 0.006; preferably, phi is less than or equal to 0.003; more preferably, Φ ≦ 0.0017.
The content deviation phi of holmium element in the zinc-holmium alloy is calculated by adopting the following formula:
Φ＝|a/b-1|
wherein a represents the content of holmium element in the zinc-holmium alloy, and the unit is wt%; b represents the content of metal holmium in wt% of the raw materials for forming the zinc-holmium alloy.
< uses of the Container >
The container can reduce the content deviation of holmium element in the zinc-holmium alloy. The invention thus provides the use of a container for reducing the variation of the holmium element content of a zinc holmium alloy.
The content deviation of holmium element in the zinc-holmium alloy can be expressed by phi. Phi is less than or equal to 0.006; preferably, phi is less than or equal to 0.003; more preferably, Φ ≦ 0.0017.
The content deviation of holmium element in the zinc-holmium alloy is calculated by adopting the following formula:
Φ＝|a/b-1|
wherein phi represents the content deviation of holmium element in the zinc-holmium alloy; a represents the content of holmium element in the zinc-holmium alloy, and the unit is wt%; b represents the content of metal holmium in wt% of the raw materials for forming the zinc-holmium alloy.
The vessel is used for carrying raw materials in smelting and refining processes. Examples of containers include, but are not limited to, crucibles. The portion of the vessel in contact with the feedstock is formed from metallic tantalum. Preferably, the inner surface of the raw material-containing receiving chamber of the container is formed of metallic tantalum. In certain embodiments, the container is formed from metallic tantalum. According to one embodiment of the invention, at least a portion of the inner surface of the vessel is adapted to be in contact with the feedstock, said at least a portion of the inner surface being formed from metallic tantalum. According to a preferred embodiment of the invention, the entire inner surface of the container is formed of metallic tantalum. Therefore, the content of the holmium element in the zinc-holmium alloy can be accurately controlled, and the content deviation of the holmium element is reduced.
The zinc-holmium alloy contains holmium element. The content of holmium element in the zinc-holmium alloy is more than 0; preferably, the content of holmium element in the zinc-holmium alloy is more than or equal to 0.02 wt%; more preferably, the content of holmium element in the zinc-holmium alloy is not less than 3 wt%. The content of holmium element in the zinc-holmium alloy is less than or equal to 10 wt%; preferably, the content of holmium element in the zinc-holmium alloy is less than or equal to 9 wt%; more preferably, the content of holmium element in the zinc-holmium alloy is less than or equal to 8 wt%.
The content of zinc element in the zinc-holmium alloy is less than 100 wt%; preferably, the content of zinc element in the zinc holmium alloy is less than or equal to 99.8 wt%; more preferably, the content of zinc element in the zinc holmium alloy is less than or equal to 97 wt%. The content of zinc element in the zinc-holmium alloy is more than or equal to 90 wt%; preferably, the content of zinc element in the zinc holmium alloy is more than or equal to 91 wt%; more preferably, the content of zinc element in the zinc holmium alloy is equal to or more than 92 wt%.
The metal holmium in the raw material is an essential raw material. The content of metal holmium in the raw materials is more than 0; preferably, the content of the metal holmium in the raw material is more than or equal to 0.02 wt%; more preferably, the content of metal holmium in the raw material is 3 wt% or more. The content of metal holmium in the raw materials is less than or equal to 10 wt%; preferably, the content of metal holmium in the raw materials is less than or equal to 9 wt%; more preferably, the content of metal holmium in the raw material is 8 wt% or less.
The sum of the mass of the metal zinc and the metal holmium is 100 wt% of the mass of the raw materials. The content of metallic zinc in the raw material can be calculated by subtracting the content of metallic holmium in the raw material from 100 wt%. The content of metal zinc in the raw material is less than 100 wt%; preferably, the content of metallic zinc in the raw material is less than or equal to 99.8 wt%; more preferably, the content of metallic zinc in the raw material is 97 wt% or less. The content of metal zinc in the raw material is more than or equal to 90 wt%; preferably, the content of metallic zinc in the raw material is more than or equal to 91 wt%; more preferably, the content of metallic zinc in the raw material is 92 wt% or more.
The application of the invention can comprise the steps of smelting and refining raw materials consisting of metal holmium and metal zinc in a container, and can also comprise the step of casting alloy melt formed by smelting and refining to a mould to obtain the zinc holmium alloy. In certain embodiments, a step of pretreating raw material zinc to obtain metal zinc and/or a step of pretreating raw material holmium to obtain holmium can also be included. The selection of the raw materials and the specific operations of the steps are as described above, and are not described herein again.
The test method is described below:
the content of holmium element in the zinc-holmium alloy is as follows: and measuring by using an inductively coupled plasma emission spectrometer.
Carbon element content in the zinc holmium alloy: measured using an infrared carbon sulfur analyzer, model LECO-400, purchased from linco corporation, usa.
The content of sulfur element in the zinc holmium alloy is as follows: measured using an infrared carbon sulfur analyzer, model LECO-400, purchased from linco corporation, usa.
The content of phosphorus element in the zinc holmium alloy is as follows: the measurement was carried out using a spectrophotometer, model 722, purchased from precision instruments, Shanghai.
The content of oxygen element in the zinc holmium alloy is as follows: the oxygen, nitrogen and hydrogen analyzer with the model of ONH-2000 is adopted for determination.
The calculation method of the holmium element content deviation (phi) in the zinc-holmium alloy is as follows:
Φ＝|a/b-1|
wherein phi represents the content deviation of holmium element in the zinc-holmium alloy; a represents the content of holmium element in the zinc-holmium alloy, and the unit is wt%; b represents the content of metal holmium in the raw materials for forming the zinc-holmium alloy, and the unit is wt%.
Example 1
And (3) polishing the surface of the raw material holmium obtained by electrolysis, and then melting and refining in a vacuum melting furnace to obtain the metal holmium. The content of oxygen in the metal holmium is less than or equal to 0.008 wt%, the content of phosphorus is less than 0.01 wt%, and the content of sulfur is less than 0.0050 wt%.
And (4) polishing the surface of the raw material zinc to obtain the metal zinc.
Placing a raw material consisting of 6.6 parts by weight of holmium metal and 93.4 parts by weight of zinc metal in a tantalum-containing crucible (the inner wall of a receiving chamber for receiving the raw material is formed of tantalum metal); placing the tantalum-containing crucible in a smelting furnace, vacuumizing the pressure in the smelting furnace to be below 10Pa, and then filling argon into the smelting furnace until the pressure in the smelting furnace is 0.03 MPa; heating the temperature in the smelting furnace to 890 ℃, smelting the raw materials until the zinc is completely melted; then refining for 30min to obtain alloy melt.
And casting the alloy melt into a water-cooled copper ingot mold, and cooling to room temperature to obtain the zinc-holmium alloy.
The content of holmium element and the content of holmium element in the obtained zinc-holmium alloy are different, and the content of impurity elements is shown in table 1.
Comparative example 1
The procedure of example 1 was repeated, except that the tantalum-containing crucible was replaced with a magnesium oxide-containing crucible. The inner wall of the containing cavity of the crucible containing the magnesium oxide, which contains the raw material, is formed by magnesium oxide.
The content of holmium element and the content of holmium element in the obtained zinc-holmium alloy are different, and the content of impurity elements is shown in table 1.
TABLE 1
Figure BDA0003585956710000101
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 a zinc-holmium alloy is characterized by comprising the steps of smelting and refining raw materials consisting of metal holmium and metal zinc in a container;
wherein at least a portion of the interior surface of the vessel is for contact with the feedstock, the at least a portion of the interior surface being formed from metallic tantalum.
2. The production method according to claim 1, wherein the entire inner surface of the container is formed of metallic tantalum.
3. The production method according to claim 1, wherein the melting temperature is 600 to 1200 ℃ and the melting pressure is 0.005 to 0.07 MPa.
4. The production method according to claim 1, wherein the smelting is performed under an inert atmosphere.
5. The production method according to claim 1, further comprising a step of casting the alloy melt formed by melting and refining into a mold to form a zinc holmium alloy; wherein the mold is a mold with a cooling water passage or a mold with a stirring function.
6. The production method according to claim 1, wherein the content of metal holmium in the raw material is 10 wt% or less.
7. The production method according to claim 6, wherein the content deviation Φ of holmium element in the zinc-holmium alloy is less than or equal to 0.006;
Φ＝|a/b-1|
wherein a represents the content of holmium element in the zinc-holmium alloy, and the unit is wt%; b represents the content of metal holmium in wt% of the raw materials for forming the zinc-holmium alloy.
8. A zinc holmium alloy, characterized in that the zinc holmium alloy is prepared by the production method of any one of claims 1-7.
9. Use of a container for reducing the deviation of the content of holmium element in a zinc-holmium alloy, characterized in that:
the content deviation phi of holmium element in the zinc-holmium alloy is calculated by adopting the following formula:
Φ＝|a/b-1|
wherein a represents the content of holmium element in the zinc-holmium alloy, and the unit is wt%; b represents the content of metal holmium in raw materials for forming the zinc-holmium alloy, and the unit is wt%;
wherein at least a portion of the interior surface of the vessel is for contact with the feedstock, the at least a portion of the interior surface being formed from metallic tantalum.
10. The use according to claim 9, characterized in that the holmium element content of the zinc holmium alloy is less than or equal to 10 wt%; phi is less than or equal to 0.006.
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