CN107475773A - A kind of method for preparing La-Fe-Si systems complex phase symbiosis orientation bar - Google Patents

A kind of method for preparing La-Fe-Si systems complex phase symbiosis orientation bar Download PDF

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Publication number
CN107475773A
CN107475773A CN201710539776.4A CN201710539776A CN107475773A CN 107475773 A CN107475773 A CN 107475773A CN 201710539776 A CN201710539776 A CN 201710539776A CN 107475773 A CN107475773 A CN 107475773A
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Prior art keywords
complex phase
bar
orientation bar
melting
foundry alloy
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方跃
徐智帅
郑红星
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/52—Alloys
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/02—Heat treatment

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a kind of method for preparing La-Fe-Si systems complex phase symbiosis orientation bar, its step：(1) is equipped with lanthanum, iron, silicon material in proportion, using Medium frequency induction method of smelting melting La1+x Fe13‑y Si y Foundry alloy, a diameter of 8mm~10mm, a height of 100mm~120mm foundry alloy polycrystalline bar are poured into after melting in the original location；(2) uses zone refining directional freeze method to above-mentioned La1+x Fe13‑y Si y Foundry alloy polycrystalline bar carries out region remelting, and in crystal growing process, cavity internal pressure be 8~10bar, and protective gas is the argon gas of 99.99% purity, and zone refining temperature is 1853~1893K, and melting zone is highly 10~15mm, and pull rate is 10~200 μm/s；(3) the complex phase symbiosis orientation bar after remelting is placed in vacuum heat treatment furnace, 1 hour isothermal Water Quenching is carried out in 1373~1473K temperature ranges, La-Fe-Si systems complex phase symbiosis orientation bar is made.

Description

A kind of method for preparing La-Fe-Si systems complex phase symbiosis orientation bar
Technical field
The present invention relates to a kind of method for preparing La-Fe-Si systems complex phase symbiosis orientation bar, belong to field of magnetic refrigeration material.
Background technology
Compared to existing vapor compression refrigeration mode, room temperature magnetic refrigerating technology green high-efficient, energy-saving effect highly significant, by Increasing concern.At this stage in three big core technology of room temperature magnetic refrigerating, the design of heat-exchange system and rare-earth permanent magnet with Processing and manufacturing technology is comparatively ripe, and bottleneck problem is to seek the room temperature magnetic refrigerating material for manufacturing super performance low cost.It is existing The temperature that the magnetic entropy for having the magnetic refrigerating material in technology becomes peak value is not wide high, and refrigerating capacity is preferable not enough, during as refrigerating material It is influenced by temperature larger.La-Fe-Si systems alloy cost performance is the most excellent, it is considered to be the most room temperature of commercial application prospect One of magnetic refrigerating material, still, the intrinsic fragility of La-Fe-Si systems alloy strongly limit its high efficiency manufacture and application of being on active service, material Preparing must near-net forming as far as possible（Thin plate or bar）And there is certain mechanical property, prepare multiphase coexistence, La (Fe, Si)13Mutually height-oriented complex phase symbiosis orientation bar is one of effective way for lifting its mechanics and magnetics combination property.
The content of the invention
It is an object of the invention to provide a kind of method for preparing La-Fe-Si systems complex phase symbiosis orientation bar, prepared by this method Bar there is excellent refrigeration and mechanical property.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of method for preparing La-Fe-Si systems complex phase symbiosis orientation bar, it is characterised in that there is procedure below and step：
(1) is according to La1+x Fe13-y Si y Wherein 0≤x≤ 1,1≤y≤ 1.6 ratio is equipped with 120g~150g lanthanum, iron, silicon Raw material, using conventional Medium frequency induction method of smelting melting La1+x Fe13-y Si y Foundry alloy wherein 0≤x≤ 1,1≤y≤ 1.6 meltings Pour into a diameter of 8mm~10mm, a height of 100mm~120mm foundry alloy polycrystalline bar in the original location afterwards；
(2) uses the La that zone refining directional freeze method obtains to above-mentioned steps (1)1+x Fe13-y Si y Foundry alloy polycrystalline bar Carry out region remelting, in crystal growing process, cavity internal pressure be 8~10bar, protective gas for 99.99% purity argon gas, Zone refining temperature is 1853~1893K, and melting zone is highly 10~15mm, and pull rate is 10~200 μm/s；
(3) the complex phase symbiosis orientation bar after step (2) remelting is placed in vacuum heat treatment furnace by, in 1373~1473K temperature Section carries out 1 hour isothermal Water Quenching, and La-Fe-Si systems complex phase symbiosis orientation bar is made.
Compared with prior art, the present invention has the advantages of following prominent：
The inventive method preparation La-Fe-Si complex phases symbiosis orientation bar is simple to operate, and repeatability is strong, and required later stage height warms Processing time is shorter.
Embodiment
The present invention is described in further detail with reference to embodiments.
Embodiment 1
A kind of method for preparing La-Fe-Si systems complex phase symbiosis orientation bar, its step are as follows：
(1) is according to La1Fe11.6Si1.4Ratio be equipped with 150g lanthanum, iron, silicon material, using conventional Medium frequency induction melting Method melting La1Fe11.6Si1.4 , a diameter of 10mm, a height of 120mm are poured into after melting in the original location；
(2) uses the La that zone refining directional freeze method obtains to above-mentioned steps (1)1Fe11.6Si1.4Foundry alloy polycrystalline rod Material carries out region remelting, and in crystal growing process, cavity internal pressure 8bar, protective gas is 99.99% static high-purity argon gas, Zone refining temperature is 1853K, and melting zone is highly 10mm, and pull rate is 10 μm/s；
(3) is by the La after step (2) remelting1Fe11.6Si1.4Complex phase symbiosis orientation bar is placed in vacuum heat treatment furnace, in 1373K carries out 1 hour isothermal Water Quenching, and La is made1Fe11.6Si1.4It is complex phase symbiosis orientation bar.
Embodiment 2
(1) is according to La1.6Fe11.8Si1.2Ratio be equipped with 150g lanthanum, iron, silicon material, using conventional Medium frequency induction melting Method melting La1.6Fe11.8Si1.2, a diameter of 8mm, a height of 100mm are poured into after melting in the original location；
(2) uses the La that zone refining directional freeze method obtains to above-mentioned steps (1)1.6Fe11.8Si1.2Foundry alloy polycrystalline rod Material carries out region remelting, and in crystal growing process, cavity internal pressure 10bar, protective gas is 99.99% static high-purity argon gas, Zone refining temperature is 1873K, and melting zone is highly 12mm, and pull rate is 90 μm/s；
(3) is by the La after step (2) remelting1.6Fe11.8Si1.2Complex phase symbiosis orientation bar is placed in vacuum heat treatment furnace, in 1423K carries out 1 hour isothermal Water Quenching, and La is made1.6Fe11.8Si1.2It is complex phase symbiosis orientation bar.
Embodiment 3
(1) is according to La2Fe11.4Si1.6Ratio be equipped with 150g lanthanum, iron, silicon material, using conventional Medium frequency induction melting Method melting La2Fe11.4Si1.6, a diameter of 10mm, a height of 120mm are poured into after melting in the original location；
(2) uses the La that zone refining directional freeze method obtains to above-mentioned steps (1)2Fe11.4Si1.6Foundry alloy polycrystalline rod Material carries out region remelting, and in crystal growing process, cavity internal pressure 10bar, protective gas is 99.99% static high-purity argon gas, Zone refining temperature is 1893K, and melting zone is highly 10mm, and pull rate is 200 μm/s；
(3) is by the La after step (2) remelting2Fe11.4Si1.6Complex phase symbiosis orientation bar is placed in vacuum heat treatment furnace, in 1473K carries out 1 hour isothermal Water Quenching, and La is made2Fe11.4Si1.6It is complex phase symbiosis orientation bar.

Claims (1)

  1. A kind of 1. method for preparing La-Fe-Si systems complex phase symbiosis orientation bar, it is characterised in that this method has steps of：
    (1) is according to La1+x Fe13-y Si y Wherein 0≤x≤ 1,1≤yThe lanthanum, iron, silicon that≤1.6 ratio is equipped with 120g~150g are former Material, using conventional Medium frequency induction method of smelting melting La1+x Fe13-y Si y Foundry alloy wherein 0≤x≤ 1,1≤yAfter≤1.6 meltings A diameter of 8mm~10mm, a height of 100mm~120mm foundry alloy polycrystalline bar are poured into the original location；
    (2) uses the La that zone refining directional freeze method obtains to above-mentioned steps (1)1+x Fe13-y Si y Foundry alloy polycrystalline bar Carry out region remelting, in crystal growing process, cavity internal pressure be 8~10bar, protective gas for 99.99% purity argon gas, Zone refining temperature is 1853~1893K, and melting zone is highly 10~15mm, and pull rate is 10~20 μm/s；
    (3) the complex phase symbiosis orientation bar after step (2) remelting is placed in vacuum heat treatment furnace by, in 1373~1473K temperature Section carries out 1 hour isothermal Water Quenching, and La-Fe-Si systems complex phase symbiosis orientation bar is made.
CN201710539776.4A 2017-07-05 2017-07-05 A kind of method for preparing La-Fe-Si systems complex phase symbiosis orientation bar Pending CN107475773A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112797665A (en) * 2021-01-08 2021-05-14 哈尔滨工业大学 Heat accumulator shell of magnetic refrigerator with woven structure
CN112863846A (en) * 2021-01-08 2021-05-28 哈尔滨工业大学 Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system

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CN103757704A (en) * 2014-01-24 2014-04-30 南京理工大学 Preparation of nickel-base single-crystal high-temperature alloy through light floating zone melting directional solidification method
CN103993356A (en) * 2014-05-06 2014-08-20 上海大学 Method for high-pressure optical zone-melting growth of high-orientation crystal of easily volatile material
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CN103343238A (en) * 2013-07-22 2013-10-09 上海交通大学 Zone melting and directional solidifying method used for volatile element alloy
CN103757704A (en) * 2014-01-24 2014-04-30 南京理工大学 Preparation of nickel-base single-crystal high-temperature alloy through light floating zone melting directional solidification method
CN103993356A (en) * 2014-05-06 2014-08-20 上海大学 Method for high-pressure optical zone-melting growth of high-orientation crystal of easily volatile material
CN104694813A (en) * 2015-03-04 2015-06-10 中国科学院宁波材料技术与工程研究所 LaFeSi-based magnetic refrigeration material as well as preparation method and application thereof
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112797665A (en) * 2021-01-08 2021-05-14 哈尔滨工业大学 Heat accumulator shell of magnetic refrigerator with woven structure
CN112863846A (en) * 2021-01-08 2021-05-28 哈尔滨工业大学 Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system
CN112797665B (en) * 2021-01-08 2022-07-29 哈尔滨工业大学 Heat accumulator shell of magnetic refrigerator with woven structure

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