CN105755540B - One kind prepares LaB using optics zone-melting technique6-VB2The method of eutectic composites - Google Patents

One kind prepares LaB using optics zone-melting technique6-VB2The method of eutectic composites Download PDF

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CN105755540B
CN105755540B CN201610316212.XA CN201610316212A CN105755540B CN 105755540 B CN105755540 B CN 105755540B CN 201610316212 A CN201610316212 A CN 201610316212A CN 105755540 B CN105755540 B CN 105755540B
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lab
eutectic
coupon
powder
melting
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CN105755540A (en
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杨新宇
王盼
张久兴
胡可
李志�
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Hefei University of Technology
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Hefei University of 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
    • 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

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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)
  • Ceramic Products (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Powder Metallurgy (AREA)

Abstract

LaB is prepared using optics zone-melting technique the invention discloses one kind6‑VB2The method of eutectic composites, it is characterised in that：LaB is obtained by discharge plasma sintering first6‑VB2Eutectic precast body, then by LaB6‑VB2Eutectic precast body is placed in optics zone melting furnace, using xenon lamp as heating source, with the drawing velocity directional solidification of 1 1000mm/h, the LaB of obtained high quality under argon atmosphere6‑VB2Eutectic composites.The LaB that the present invention is prepared by optics zone-melting technique6‑VB2Eutectic composites, with LaB6For matrix, with VB2For fiber, fiber spacing is in 0.56 6.51 μ ms.

Description

One kind prepares LaB using optics zone-melting technique6-VB2The method of eutectic composites
Technical field
The present invention relates to a kind of LaB6-VB2The preparation method of eutectic composites, belongs to technical field of new material preparation.
Background technology
Directional solidification LaB6-MeB2(Me=Zr, Cr, Hf, Mo) eutectic composites, are using during liquid-solid-phase changeable Eutectic reaction so that LaB6Matrix and MeB2Fiber symbiosis at the same time from melt separates out, and avoids boundary moisture and chemical reaction etc. Unfavorable factor.The LaB of formation6-MeB2Composite material inherits the physical characteristic of eutectic two-phase, and can pass through process of setting parameter Adjustment more easily control MeB2Tissue morphology is to optimize material property.Research shows that directional solidification technique can make LaB6-MeB2MeB in eutectic composites2Uniform, the regular arrangement of fiber is in the base.The eutectic composites phase of formation Than in matrix LaB6With relatively low work function, higher emission and higher anti-poisoning and hot cracking characteristics, this A little characteristics cause the material to become the new heat emission material of high energy device of new generation.
Nineteen eighty-three, Ukraine S.S.Ordanyan et al. has primarily looked at LaB6-MeB2(Me=Zr, Cr, Hf, Mo) system, It was found that hardly mutually solid solution, tissue can keep stablizing in wide temperature range, orient at the same time between the two-phase of this kind of alloy The MeB of arrangement2Matrix LaB can significantly be improved6Mechanical property so that the service life of whole material increases substantially. In LaB6-MeB2In (Me=Zr, Ti, Hf, V, Cr, Ta) system, LaB6-VB2Work function it is minimum, highest current density.So And at present on LaB6-VB2There is not been reported for the technology of preparing and tissue characteristics of eutectic composites, therefore there is an urgent need to carry out LaB6-VB2The preparation of eutectic composites and the research of performance.
The content of the invention
The present invention proposes a kind of using optics zone-melting technique preparation LaB6-VB2The method of eutectic composites, it is intended to pass through Accurate control Solidification Parameters, so as to obtain the LaB of high quality6-VB2Eutectic composites.
The present invention solves technical problem, adopts the following technical scheme that：
The present invention prepares LaB using optics zone-melting technique6-VB2The method of eutectic composites, its feature are to include such as Lower step：
Step 1: prepare LaB6-VB2Eutectic precast body
It is not less than 99.5% VB with purity2Powder and purity are not less than 99% LaB6Powder is raw material, by eutectic phase The mass percent dispensing of figure, ball milling, drying, obtain LaB6-VB2Mixed-powder；
By the LaB6-VB2Mixed-powder is put into graphite jig and pre-molding, is subsequently placed in discharge plasma sintering In the furnace chamber of stove, the axial compressive force of 30MPa is vacuumized, applied, is warming up to 1600 DEG C, keeps the temperature 10min, last sample is with furnace cooling But, sample is taken out when furnace temperature is less than 50 DEG C, obtains LaB6-VB2Eutectic precast body；
Step 2: Wire EDM LaB6-VB2Coupon
With electric spark wire cutting machine by LaB6-VB2Eutectic precast body cuts into coupon, and coupon is placed in ultrasound in alcohol Ripple cleans, and then coupon after cleaning is placed in electric vacunm drying case, 100 DEG C of dry 10h；
Step 3: LaB6-VB2Coupon directional solidification
Two coupons are respectively placed on the upper pumping rod and lower pumping rod of optics zone melting furnace, adjustment makes upper and lower coupon extremely Suitable position, then fills quartz ampoule, closes fire door；Argon gas is passed through into optics zone melting furnace, with the liter no more than 80 DEG C/min Warm speed heating, the end face for making upper and lower coupon close to each other is melted at the same time；Directional solidification is proceeded by after melting zone is stablized, it is raw Long speed is 1-1000mm/h, that is, obtains LaB6-VB2Eutectic composites.
The present invention has the following advantages：
(1) even tissue：Optics zone-melting process is by four equally distributed high power xenon lamp heating, in conjunction with the rotation of charge bar Turn, uniform solute field and the temperature field of crystal growth needs can be obtained, so as to obtain the composite material of even tissue.
(2) cost is low, efficient：Optics zone melting furnace is furnished with CCD systems, and crystal growing process can be observed, and fits When be adjusted so that increase substantially high quality crystal growth success rate, reduce cost.
Brief description of the drawings
Fig. 1 is the LaB prepared in the embodiment of the present invention 26-VB2Cross section tissue's pattern (pull speed of eutectic composites Rate is 200mm/h)；
Fig. 2 is the LaB prepared in the embodiment of the present invention 26-VB2Longitudinal section tissue topography (the pull speed of eutectic composites Rate is 200mm/h)；
Embodiment
Embodiment 1
The present embodiment prepares LaB as follows6-VB2Eutectic composites：
Step 1: prepare LaB6-VB2Eutectic precast body
It is not less than 99.5% VB with purity2Powder and purity are not less than 99% LaB6Powder is raw material, by eutectic phase The mass percent dispensing of figure, ball milling, drying, obtain LaB6-VB2Mixed-powder；
By LaB6-VB2Mixed-powder is put into graphite jig and pre-molding, is subsequently placed in discharge plasma sintering stove The axial compressive force of 30MPa in furnace chamber, is vacuumized, applied, is warming up to 1600 DEG C, keeps the temperature 10min, last sample furnace cooling, Furnace temperature takes out sample when being less than 50 DEG C, obtain LaB6-VB2Eutectic precast body；
Step 2: Wire EDM LaB6-VB2Coupon
LaB is cut with electric spark wire cutting machine6-VB2Eutectic precast body, the coupon of a diameter of Ф 6mm cut out is placed in Alcohol washes 10min is used in ultrasonic wave, then the coupon cleaned is placed in electric vacunm drying case, 100 DEG C of dry 10h.
Step 3: LaB6-VB2Coupon directional solidification
Two coupons are respectively placed on the upper pumping rod and lower pumping rod of optics zone melting furnace, adjust upper and lower coupon to conjunction Suitable position, then fills quartz ampoule, closes fire door；Argon gas is passed through into optics zone melting furnace, with the heating rate liter of 80 DEG C/min Temperature, the end face for making upper and lower coupon close to each other are melted at the same time；Directional solidification is proceeded by after melting zone is stablized, growth rate is 1mm/h, that is, obtain LaB6-VB2Eutectic composites.
Understood through characterization, VB in products obtained therefrom2Fiber is uniformly regular to be distributed on matrix, VB2Fiber spacing is 6.51 μ m。
Embodiment 2
The present embodiment prepares LaB as follows6-VB2Eutectic composites：
Step 1: prepare LaB6-VB2Eutectic precast body
It is not less than 99.5% VB with purity2Powder and purity are not less than 99% LaB6Powder is raw material, by eutectic phase The mass percent dispensing of figure, ball milling, drying, obtain LaB6-VB2Mixed-powder；
By LaB6-VB2Mixed-powder is put into graphite jig and pre-molding, is subsequently placed in discharge plasma sintering stove The axial compressive force of 30MPa in furnace chamber, is vacuumized, applied, is warming up to 1600 DEG C, keeps the temperature 10min, last sample furnace cooling, Furnace temperature takes out sample when being less than 50 DEG C, obtain LaB6-VB2Eutectic precast body；
Step 2: Wire EDM LaB6-VB2Coupon
LaB is cut with electric spark wire cutting machine6-VB2Eutectic precast body, the coupon of a diameter of Ф 6mm cut out is placed in Alcohol washes 10min is used in ultrasonic wave, then the coupon cleaned is placed in electric vacunm drying case, 100 DEG C of dry 10h.
Step 3: LaB6-VB2Coupon directional solidification
Two coupons are respectively placed on the upper pumping rod and lower pumping rod of optics zone melting furnace, adjust upper and lower coupon to conjunction Suitable position, then fills quartz ampoule, closes fire door；Argon gas is passed through into optics zone melting furnace, with the heating rate liter of 80 DEG C/min Temperature, the end face for making upper and lower coupon close to each other are melted at the same time；Directional solidification is proceeded by after melting zone is stablized, growth rate is 200mm/h, that is, obtain LaB6-VB2Eutectic composites.
The microstructure morphology of products obtained therefrom is as shown in Figure 1, 2, it can be seen that VB2Fiber is uniformly regular to be distributed in matrix On, VB2Fiber spacing is 1.29 μm.
Embodiment 3
The present embodiment prepares LaB as follows6-VB2Eutectic composites：
Step 1: prepare LaB6-VB2Eutectic precast body
It is not less than 99.5% VB with purity2Powder and purity are not less than 99% LaB6Powder is raw material, by eutectic phase The mass percent dispensing of figure, ball milling, drying, obtain LaB6-VB2Mixed-powder；
By LaB6-VB2Mixed-powder is put into graphite jig and pre-molding, is subsequently placed in discharge plasma sintering stove The axial compressive force of 30MPa in furnace chamber, is vacuumized, applied, is warming up to 1600 DEG C, keeps the temperature 10min, last sample furnace cooling, Furnace temperature takes out sample when being less than 50 DEG C, obtain LaB6-VB2Eutectic precast body；
Step 2: Wire EDM LaB6-VB2Coupon
LaB is cut with electric spark wire cutting machine6-VB2Eutectic precast body, the coupon of a diameter of Ф 6mm cut out is placed in Alcohol washes 10min is used in ultrasonic wave, then the coupon cleaned is placed in electric vacunm drying case, 100 DEG C of dry 10h.
Step 3: LaB6-VB2Coupon directional solidification
Two coupons are respectively placed on the upper pumping rod and lower pumping rod of optics zone melting furnace, adjust upper and lower coupon to conjunction Suitable position, then fills quartz ampoule, closes fire door；Argon gas is passed through into optics zone melting furnace, with the heating rate liter of 80 DEG C/min Temperature, the end face for making upper and lower coupon close to each other are melted at the same time；Directional solidification is proceeded by after melting zone is stablized, growth rate is 1000mm/h, that is, obtain LaB6-VB2Eutectic composites.
Understood through characterization, VB in products obtained therefrom2Fiber is uniformly regular to be distributed on matrix, VB2Fiber spacing is 0.56 μ m。

Claims (1)

1. one kind prepares LaB using optics zone-melting technique6-VB2The method of eutectic composites, it is characterised in that including following step Suddenly：
Step 1: prepare LaB6-VB2Eutectic precast body
It is not less than 99.5% VB with purity2Powder and purity are not less than 99% LaB6Powder is raw material, by eutectic phasor Mass percent dispensing, ball milling, drying, obtain LaB6-VB2Mixed-powder；
By the LaB6-VB2Mixed-powder is put into graphite jig and pre-molding, is subsequently placed in discharge plasma sintering stove The axial compressive force of 30MPa in furnace chamber, is vacuumized, applied, is warming up to 1600 DEG C, keeps the temperature 10min, last sample furnace cooling, Furnace temperature takes out sample when being less than 50 DEG C, obtain LaB6-VB2Eutectic precast body；
Step 2: Wire EDM LaB6-VB2Coupon
With electric spark wire cutting machine by LaB6-VB2Eutectic precast body cuts into coupon, and it is clear that coupon is placed in ultrasonic wave in alcohol Wash, then coupon after cleaning is placed in electric vacunm drying case, 100 DEG C of dry 10h；
Step 3: LaB6-VB2Coupon directional solidification
Two coupons are respectively placed on the upper pumping rod and lower pumping rod of optics zone melting furnace, adjustment makes upper and lower coupon suitable Position, then fill quartz ampoule, close fire door；Argon gas is passed through into optics zone melting furnace, with the heating speed no more than 80 DEG C/min Rate heats up, and the end face for making upper and lower coupon close to each other is melted at the same time；Directional solidification, growth speed are proceeded by after melting zone is stablized Rate is 1-1000mm/h, that is, obtains LaB6-VB2Eutectic composites.
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CN106882966B (en) * 2017-01-19 2020-06-26 合肥工业大学 Preparation of SiC/LaB by optical zone melting technology6Method for eutectic composite material
CN109763170B (en) * 2019-03-25 2021-03-09 合肥工业大学 Preparation method of high-performance quaternary rare earth hexaboride-zirconium diboride composite material
CN115386778B (en) * 2022-08-12 2023-06-06 合肥工业大学 Lanthanum hexaboride eutectic composite material and preparation method thereof

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JPH05319991A (en) * 1992-05-19 1993-12-03 Natl Inst For Res In Inorg Mater Method for growing lanthanum hexaboride single crystal
CN1680215A (en) * 2005-01-14 2005-10-12 李根法 Eutectic composite powdery-sintering assistant for manufacturing structural ceramic and production thereof
CN101381085B (en) * 2008-10-24 2010-07-21 北京工业大学 Rapid preparation method of LaB6 polycrystalline bulk cathode material
CN102433587B (en) * 2011-09-19 2014-11-26 北京工业大学 Preparation method of multicomponent large-size rare earth boride LaxCe1-xB6 monocrystalline block cathode material
CN103205801B (en) * 2013-03-23 2015-11-18 北京工业大学 A kind of large scale rare-earth boride SmB 6the preparation method of single crystal
CN103523792B (en) * 2013-10-18 2015-05-06 湖南稀土金属材料研究院 LaB6 polycrystal and preparation method thereof, and LaB6 cathode comprising LaB6 polycrystal

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109133993A (en) * 2018-08-09 2019-01-04 合肥工业大学 A kind of LaB6-(Zr,V)B2The preparation method of eutectic composites
CN109133993B (en) * 2018-08-09 2021-12-14 合肥工业大学 LaB6-(Zr,V)B2Preparation method of eutectic composite material

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