CN112414126A - Method for melting hundred kilogram grade oxide and metal powder mixture at ultrahigh temperature - Google Patents

Method for melting hundred kilogram grade oxide and metal powder mixture at ultrahigh temperature Download PDF

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Publication number
CN112414126A
CN112414126A CN202011250209.5A CN202011250209A CN112414126A CN 112414126 A CN112414126 A CN 112414126A CN 202011250209 A CN202011250209 A CN 202011250209A CN 112414126 A CN112414126 A CN 112414126A
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Prior art keywords
mixture
melting
metal powder
metal
oxide
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CN202011250209.5A
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Chinese (zh)
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陈波
梁田
刘奎
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Priority to CN202011250209.5A priority Critical patent/CN112414126A/en
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00Crucible or pot furnaces
    • F27B14/08Details peculiar to crucible or pot furnaces
    • F27B14/14Arrangements of heating devices
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00Crucible or pot furnaces
    • F27B14/08Details peculiar to crucible or pot furnaces
    • F27B14/10Crucibles
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D1/00Casings; Linings; Walls; Roofs
    • F27D1/12Casings; Linings; Walls; Roofs incorporating cooling arrangements

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a method for melting a mixture of hundred kilogram-level oxides and metal powder at ultrahigh temperature, belonging to the technical field of high-temperature metallurgy of materials. A split water-cooled copper crucible is adopted, a mixture of oxides and metal powder (or small particles) in the crucible is heated by electromagnetic induction, a small metal ring is embedded in the mixture in advance, and the materials are smelted in an inert atmosphere. Because the oxide is a dielectric body at room temperature, the mixture of the oxide and the metal can not be heated to be molten by an electromagnetic field, the embedded small metal ring is heated by the electromagnetic field until the small metal ring is molten, the oxide and the metal mixture around the metal ring can absorb the energy of the electromagnetic field after being heated to a certain temperature by the metal ring, the mixture around the small metal ring is gradually heated and molten by a high-frequency electromagnetic field, finally, a molten pool is gradually expanded to all crucible materials, and the mixture is kept warm for a certain time to ensure that the mixture is completely molten.

Description

Method for melting hundred kilogram grade oxide and metal powder mixture at ultrahigh temperature
Technical Field
The invention relates to the technical field of high-temperature metallurgy of materials, in particular to a method for melting a mixture of hundred kilograms of oxides and metal powder at ultrahigh temperature.
Background
When the nuclear power plant has serious core melting accident, the UO is used under the condition of cooling water loss2The cracking heat causes the temperature of the reactor core to rise sharply, the fuel pellets and the nearby Zr cladding and tube plate are melted, and the molten UO2、Zr、ZrO2(reaction of zirconium with Water to form ZrO)2And H2) And the mixture of stainless steel and the like falls to the lower end enclosure. Discovery of UO2、ZrO2The mixing of (A) and (B) is relatively sufficient to form an intermediate oxide layer, and Zr metal reduces part UO2Heavy metal uranium is placed at the bottom of the melting pool to form a heavy metal layer, Fe and Zr at the top of the melting pool form a light metal layer, and the melting pool is of a three-layer structure by analyzing the layering mechanism of the melting pool, so that the method has important significance for improving the nuclear accident analysis accuracy and the success rate of in-pile melt mitigation measures.
Disclosure of Invention
The invention aims to provide a method for melting hundred kilograms of oxide and metal powder mixture at ultrahigh temperature, which adopts a water-cooled copper crucible to melt 50-100 kilograms of oxide and metal powder mixture in an induction manner, and the melt temperature is higher than 2800 ℃ after melting.
The technical scheme adopted by the invention is as follows:
a method for melting kilogram-grade oxide and metal powder mixture at ultrahigh temperature adopts a water-cooled copper crucible to inductively melt 50-100 kilograms of oxide and metal powder mixture, and the temperature of the melt obtained after melting is more than 2800 ℃. The method specifically comprises the following steps:
(1) uniformly mixing an oxide to be smelted and metal powder (or metal small particles) to form a mixture, wherein the weight of the metal powder (or metal small particles) accounts for 5-40% of the total weight of the mixture;
(2) adding the mixture into a water-cooled copper crucible, and embedding a small metal ring in the mixture in advance;
(3) under an inert atmosphere, heating and smelting the mixture in the crucible by adopting electromagnetic induction, wherein the electromagnetic heating power is 100-150KW, the power supply heating frequency is 100-200KHz (preferably-150 KHz), and the mixture is electromagnetically heated until the small metal ring is melted; and then the temperature is maintained for 10 to 120 minutes under the power condition of 250 and 350KW, and in the heat preservation process, the small metal ring fuses the mixture of the surrounding oxide and the metal powder until all the mixture in the crucible is melted and the metal layer and the oxide are well layered.
The oxide is ZrO with a melting point higher than 2700 DEG C2Powder, CaO powder and UO2One or more of the powders, the metalThe powder is one or more of pure iron powder, stainless steel powder, 508-III steel and zirconium powder.
In the step (2), the water-cooled copper crucible is a split water-cooled copper crucible, gaps among crucible halves are smaller than 2mm, and the gaps of the crucible are tightly filled with oxides to be melted.
In the step (2), the weight of the small metal rings embedded in the mixture is 100-1000 g.
In the step (3), the material of the small metal ring is the same as that of the metal powder.
The design principle and the beneficial effects of the invention are as follows:
when the mixture containing the metal rings is heated by electromagnetic induction, because the oxide is a dielectric body at room temperature, the mixture of the oxide and the metal powder cannot be heated to be molten by an electromagnetic field, the embedded small metal rings are heated by the electromagnetic field until the small metal rings are molten, the mixture of the oxide and the metal powder around the metal rings can absorb the energy of the electromagnetic field after being heated to a certain temperature by the metal rings, the mixture around the small metal rings is gradually heated and molten by a high-frequency electromagnetic field, finally, a molten pool is gradually expanded to all materials in the crucible, the temperature is kept for a certain time to ensure that the mixture is completely molten, and the metal layer and the oxide form good layers.
Drawings
FIG. 1 is an external view and a top view of a split water-cooled copper crucible used in the present invention.
FIG. 2 shows ZrO in the crucible after melting in example 12And a metallic Zr mixture.
FIG. 3 shows the melted ZrO after tapping in example 12And a metallic Zr mixture ingot.
Detailed Description
For a further understanding of the present invention, the following description is given in conjunction with the examples which are set forth to illustrate, but are not to be construed to limit the present invention, features and advantages.
The water-cooled copper crucible used in the following examples was a split water-cooled copper crucible, as shown in fig. 1, the gaps between the crucible halves were less than 2mm, and the gaps were tightly filled with the oxide to be melted.
Example 1:
ZrO weighed 69.7kg2The mixture of powder and metallic Zr pellets (wherein the weight of the metallic Zr pellets was 10kg) was placed in a split water-cooled copper crucible having an inner diameter of 240mm and a depth of 920mm (FIG. 1). A stainless steel ring with the inner diameter of 130mm, the outer diameter of 140mm and the weight of 800g is pre-embedded in the mixture. The charging sequence in the crucible is as follows: half of the mixture was filled in the crucible and then a stainless steel ring was placed in the mixture. Then the remaining half of the mixture was added again and finally tamped with an iron rod.
And placing the water-cooled copper crucible in an electromagnetic induction furnace, vacuumizing the furnace to below 10Pa, introducing high-purity argon, repeating the vacuumizing and argon introducing process for 3 times, and finally introducing argon to the pressure of-0.08 MPa.
After the power is gradually increased to 112KW for heating for 12 minutes, the current reading is reduced, which indicates that the metal ring and the mixture begin to melt, at the moment, the power supply heating frequency is 132KHz, the power is increased to 300-310KW for heat preservation for 60 minutes, and the power is cut off for cooling.
After the mixture was completely cooled, radial cracks were observed on the upper surface of the mixture inside the water-cooled crucible (fig. 2), and the mixture was taken out of the furnace to confirm that the mixture ingot was completely melted (fig. 3).

Claims (6)

1. A method for melting a mixture of hundred kilograms of oxides and metal powder at ultrahigh temperature is characterized by comprising the following steps: the method adopts a water-cooled copper crucible to perform induction melting on a mixture of 50-150 kg of oxide and metal powder, and the temperature of the melt obtained after melting is more than 2800 ℃.
2. The ultra-high temperature melting method for the mixture of the oxides and the metal powder in the hundred kilogram scale according to the claim 1 is characterized in that: the method comprises the following steps:
(1) uniformly mixing an oxide to be smelted and metal powder (or metal small particles) to form a mixture, wherein the weight of the metal powder (or metal small particles) accounts for 5-40% of the total weight of the mixture;
(2) adding the mixture into a water-cooled copper crucible, and embedding a small metal ring in the mixture in advance;
(3) under an inert atmosphere, heating and smelting the mixture in the crucible by adopting electromagnetic induction, gradually increasing the power to 100-; and then the temperature is maintained for 10 to 120 minutes under the power condition of 250 and 350KW, and in the process of temperature maintenance, the small metal ring is used for guiding and melting the mixture of the oxide and the metal powder around the small metal ring until all the mixture in the crucible is melted.
3. The ultra-high temperature melting method for the mixture of the oxides and the metal powder in the hundred kilogram level according to the claim 1 or 2 is characterized in that: the oxide is ZrO with a melting point higher than 2700 DEG C2Powder, CaO powder and UO2The metal powder is one or more of pure iron powder, stainless steel powder, 508-III steel, zirconium powder and the like.
4. The ultra-high temperature melting method for the mixture of the oxides and the metal powder in the hundred kilogram level according to the claim 2 is characterized in that: in the step (2), the water-cooled copper crucible is a split water-cooled copper crucible, gaps among crucible halves are smaller than 2mm, and the gaps of the crucible are tightly filled with oxides to be melted.
5. The method for melting kilogram-grade oxide and metal powder mixture under ultra-high temperature according to claim 2, is characterized in that: in the step (2), the weight of the small metal rings embedded in the mixture is 100-1000 g.
6. The method for melting kilogram-grade oxide and metal powder mixture under ultra-high temperature according to claim 1 or 2, is characterized in that: in the step (3), the material of the small metal ring is the same as that of the metal powder.
CN202011250209.5A 2020-11-11 2020-11-11 Method for melting hundred kilogram grade oxide and metal powder mixture at ultrahigh temperature Pending CN112414126A (en)

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CN202011250209.5A CN112414126A (en) 2020-11-11 2020-11-11 Method for melting hundred kilogram grade oxide and metal powder mixture at ultrahigh temperature

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313447A (en) * 2011-10-25 2012-01-11 沈阳师范大学 Medium-frequency induction heating furnace for smelting nonmetallic high-melting-point oxide
CN102997661A (en) * 2012-11-26 2013-03-27 睿为科技(天津)有限公司 Start melting device and method for preparing high-purity metallic oxide by using cold crucible
CN105283563A (en) * 2013-04-26 2016-01-27 原子能与替代能源委员会 Electromagnetic induction furnace and use of the furnace for melting a mixture of metal(s) and oxide(s), said mixture representing a corium
CN106643147A (en) * 2016-11-30 2017-05-10 昆明铂生金属材料加工有限公司 Melting starting device and method for high-frequency cold crucible to smelt metal oxide
CN111741550A (en) * 2020-06-24 2020-10-02 中国科学院金属研究所 Method for heating tungsten tube by electromagnetic induction to fuse oxide and metal mixture
CN111811275A (en) * 2020-06-24 2020-10-23 中国科学院金属研究所 Method for melting and melting high-melting-point mixture by utilizing sandwich material distribution mode and electromagnetic induction

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313447A (en) * 2011-10-25 2012-01-11 沈阳师范大学 Medium-frequency induction heating furnace for smelting nonmetallic high-melting-point oxide
CN102997661A (en) * 2012-11-26 2013-03-27 睿为科技(天津)有限公司 Start melting device and method for preparing high-purity metallic oxide by using cold crucible
CN105283563A (en) * 2013-04-26 2016-01-27 原子能与替代能源委员会 Electromagnetic induction furnace and use of the furnace for melting a mixture of metal(s) and oxide(s), said mixture representing a corium
CN106643147A (en) * 2016-11-30 2017-05-10 昆明铂生金属材料加工有限公司 Melting starting device and method for high-frequency cold crucible to smelt metal oxide
CN111741550A (en) * 2020-06-24 2020-10-02 中国科学院金属研究所 Method for heating tungsten tube by electromagnetic induction to fuse oxide and metal mixture
CN111811275A (en) * 2020-06-24 2020-10-23 中国科学院金属研究所 Method for melting and melting high-melting-point mixture by utilizing sandwich material distribution mode and electromagnetic induction

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Application publication date: 20210226