CN105755540A - Method for preparing LaB6-VB2 eutectic composite material by adopting optical zone melting technology - Google Patents

Method for preparing LaB6-VB2 eutectic composite material by adopting optical zone melting technology Download PDF

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CN105755540A
CN105755540A CN201610316212.XA CN201610316212A CN105755540A CN 105755540 A CN105755540 A CN 105755540A CN 201610316212 A CN201610316212 A CN 201610316212A CN 105755540 A CN105755540 A CN 105755540A
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lab
eutectic
coupon
lab6
powder
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CN105755540B (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

The invention discloses a method for preparing an LaB6-VB2 eutectic composite material by adopting an optical zone melting technology. The method is characterized by comprising the following steps: firstly, performing spark plasma sintering to obtain an LaB6-VB2 eutectic perform; then, placing the LaB6-VB2 eutectic perform in an optical zone melting furnace, and directionally solidifying the LaB6-VB2 eutectic perform at the pulling speed of 1,000 mm/h in the atmosphere of argon by taking a xenon lamp as a heating source to prepare a high-quality LaB6-VB2 eutectic composite material. The LaB6-VB2 eutectic composite material prepared by the optical zone melting technology disclosed by the invention takes LaB6 as a substrate and takes VB2 as fibres; the spacing between the fibres is within the range of 0.56-6.51 [mu]m.

Description

A kind of employing optics zone-melting technique prepares LaB6-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 to utilize the eutectic during liquid-solid-phase changeable anti- Should so that LaB6Matrix and MeB2Fiber simultaneously symbiosis from melt separates out, it is to avoid boundary moisture and chemical reaction etc. are unfavorable Factor.The LaB formed6-MeB2Composite inherits the physical characteristic that eutectic is biphase, and can be by the tune of process of setting parameter Whole control MeB the most easily2Tissue morphology is to optimize material property.Research shows, directional solidification technique can make LaB6-MeB2MeB in eutectic composites2Uniform, the regular arrangement of fiber is in the base.The eutectic composites phase formed Ratio is in matrix LaB6There is relatively low work function, higher emission and higher anti-poisoning and hot cracking characteristics, these Characteristic makes this material can become the Novel hot emissive material of a new generation's high energy device.
Nineteen eighty-three, Ukraine S.S.Ordanyan et al. has primarily looked at LaB6-MeB2(Me=Zr, Cr, Hf, Mo) system, sends out Existing this kind of alloy biphase between mutually solid solution hardly, tissue can keep stably, aligning in wide temperature range simultaneously MeB2Can significantly improve matrix LaB6Mechanical property so that increase substantially the service life of whole material.? LaB6-MeB2In (Me=Zr, Ti, Hf, V, Cr, Ta) system, LaB6-VB2Work function minimum, highest current density.But At present about LaB6-VB2There is not been reported for the technology of preparing of eutectic composites and tissue characteristics, therefore in the urgent need to carrying out LaB6-VB2The preparation of eutectic composites and the research of performance.
Summary of the invention
The present invention proposes a kind of employing optics zone-melting technique and prepares LaB6-VB2The method of eutectic composites, it is intended to by accurately control Solidification Parameters processed, thus obtain high-quality LaB6-VB2Eutectic composites.
The present invention solves technical problem, adopts the following technical scheme that
The present invention uses optics zone-melting technique to prepare LaB6-VB2The method of eutectic composites, its feature is to include walking as follows Rapid:
Step one, preparation LaB6-VB2Eutectic precast body
The VB of 99.5% it is not less than with purity2Powder and purity are not less than the LaB of 99%6Powder is raw material, by eutectic phasor Mass percent dispensing, ball milling, be dried, it is thus achieved that LaB6-VB2Mixed-powder；
By described LaB6-VB2Mixed-powder puts into graphite jig pre-molding, is subsequently placed in the stove of discharge plasma sintering stove Intracavity, evacuation, the axial compressive force of applying 30MPa, it is warming up to 1600 DEG C, insulation 10min, last sample furnace cooling, Sample is taken out, it is thus achieved that LaB when furnace temperature is less than 50 DEG C6-VB2Eutectic precast body；
Step 2, Wire EDM LaB6-VB2Coupon
With WEDM by LaB6-VB2Eutectic precast body cuts into coupon, and it is clear that coupon is placed in ultrasound wave in ethanol 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 upper pumping rod and the lower pumping rod of optics zone melting furnace, adjust and make upper and lower coupon to suitably Position, then fills quartz ampoule, closes fire door；It is passed through argon, with the heating rate of no more than 80 DEG C/min in optics zone melting furnace Heating up, the end face making upper and lower coupon close to each other melts simultaneously；Directional solidification, growth rate is proceeded by after melting zone is stable For 1-1000mm/h, i.e. obtain LaB6-VB2Eutectic composites.
The invention have the advantages that
(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, Uniform solute field and temperature field that crystal growth needs can be obtained, thus the composite of even tissue can be obtained.
(2) low cost, efficiency height: optics zone melting furnace is furnished with CCD system, can be observed crystal growing process, and fit Time be adjusted, thus increase substantially high quality crystal growth success rate, reduce cost.
Accompanying drawing explanation
Fig. 1 is the LaB of preparation in the embodiment of the present invention 26-VB2Cross section tissue's pattern (withdrawing rate of eutectic composites For 200mm/h)；
Fig. 2 is the LaB of preparation in the embodiment of the present invention 26-VB2(withdrawing rate is in the longitudinal section tissue topography of eutectic composites 200mm/h)；
Detailed description of the invention
Embodiment 1
The present embodiment prepares LaB as follows6-VB2Eutectic composites:
Step one, preparation LaB6-VB2Eutectic precast body
The VB of 99.5% it is not less than with purity2Powder and purity are not less than the LaB of 99%6Powder is raw material, by eutectic phasor Mass percent dispensing, ball milling, be dried, it is thus achieved that LaB6-VB2Mixed-powder；
By LaB6-VB2Mixed-powder puts into graphite jig pre-molding, is subsequently placed in the furnace chamber of discharge plasma sintering stove In, evacuation, the axial compressive force of applying 30MPa, it is warming up to 1600 DEG C, insulation 10min, last sample furnace cooling, Sample is taken out, it is thus achieved that LaB when furnace temperature is less than 50 DEG C6-VB2Eutectic precast body；
Step 2, Wire EDM LaB6-VB2Coupon
LaB is cut with WEDM6-VB2Eutectic precast body, is placed in super by the coupon of a diameter of Ф 6mm cut out Sound wave is used alcohol washes 10min, then cleaned coupon 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 upper pumping rod and the lower pumping rod of optics zone melting furnace, adjust upper and lower coupon to suitable position Put, then fill quartz ampoule, close fire door；In optics zone melting furnace, it is passed through argon, heats up with the heating rate of 80 DEG C/min, make Upper and lower coupon end face close to each other melts simultaneously；Proceeding by directional solidification after melting zone is stable, growth rate is 1mm/h, I.e. obtain LaB6-VB2Eutectic composites.
Understand through characterizing, VB in products obtained therefrom2What fiber was the most regular is distributed on matrix, VB2Fiber spacing is 6.51 μm.
Embodiment 2
The present embodiment prepares LaB as follows6-VB2Eutectic composites:
Step one, preparation LaB6-VB2Eutectic precast body
The VB of 99.5% it is not less than with purity2Powder and purity are not less than the LaB of 99%6Powder is raw material, by eutectic phasor Mass percent dispensing, ball milling, be dried, it is thus achieved that LaB6-VB2Mixed-powder；
By LaB6-VB2Mixed-powder puts into graphite jig pre-molding, is subsequently placed in the furnace chamber of discharge plasma sintering stove In, evacuation, the axial compressive force of applying 30MPa, it is warming up to 1600 DEG C, insulation 10min, last sample furnace cooling, Sample is taken out, it is thus achieved that LaB when furnace temperature is less than 50 DEG C6-VB2Eutectic precast body；
Step 2, Wire EDM LaB6-VB2Coupon
LaB is cut with WEDM6-VB2Eutectic precast body, is placed in super by the coupon of a diameter of Ф 6mm cut out Sound wave is used alcohol washes 10min, then cleaned coupon 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 upper pumping rod and the lower pumping rod of optics zone melting furnace, adjust upper and lower coupon to suitable position Put, then fill quartz ampoule, close fire door；In optics zone melting furnace, it is passed through argon, heats up with the heating rate of 80 DEG C/min, make Upper and lower coupon end face close to each other melts simultaneously；Proceeding by directional solidification after melting zone is stable, growth rate is 200mm/h, I.e. obtain LaB6-VB2Eutectic composites.
The microstructure morphology of products obtained therefrom is as shown in Figure 1, 2, it can be seen that VB2What fiber was the most regular is distributed on matrix, VB2Fiber spacing is 1.29 μm.
Embodiment 3
The present embodiment prepares LaB as follows6-VB2Eutectic composites:
Step one, preparation LaB6-VB2Eutectic precast body
The VB of 99.5% it is not less than with purity2Powder and purity are not less than the LaB of 99%6Powder is raw material, by eutectic phasor Mass percent dispensing, ball milling, be dried, it is thus achieved that LaB6-VB2Mixed-powder；
By LaB6-VB2Mixed-powder puts into graphite jig pre-molding, is subsequently placed in the furnace chamber of discharge plasma sintering stove In, evacuation, the axial compressive force of applying 30MPa, it is warming up to 1600 DEG C, insulation 10min, last sample furnace cooling, Sample is taken out, it is thus achieved that LaB when furnace temperature is less than 50 DEG C6-VB2Eutectic precast body；
Step 2, Wire EDM LaB6-VB2Coupon
LaB is cut with WEDM6-VB2Eutectic precast body, is placed in super by the coupon of a diameter of Ф 6mm cut out Sound wave is used alcohol washes 10min, then cleaned coupon 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 upper pumping rod and the lower pumping rod of optics zone melting furnace, adjust upper and lower coupon to suitable position Put, then fill quartz ampoule, close fire door；In optics zone melting furnace, it is passed through argon, heats up with the heating rate of 80 DEG C/min, make Upper and lower coupon end face close to each other melts simultaneously；Proceeding by directional solidification after melting zone is stable, growth rate is 1000mm/h, i.e. obtains LaB6-VB2Eutectic composites.
Understand through characterizing, VB in products obtained therefrom2What fiber was the most regular is distributed on matrix, VB2Fiber spacing is 0.56 μm.

Claims (1)

1. one kind uses optics zone-melting technique to prepare LaB6-VB2The method of eutectic composites, it is characterised in that include as follows Step:
Step one, preparation LaB6-VB2Eutectic precast body
The VB of 99.5% it is not less than with purity2Powder and purity are not less than the LaB of 99%6Powder is raw material, by eutectic phasor Mass percent dispensing, ball milling, be dried, it is thus achieved that LaB6-VB2Mixed-powder；
By described LaB6-VB2Mixed-powder puts into graphite jig pre-molding, is subsequently placed in the stove of discharge plasma sintering stove Intracavity, evacuation, the axial compressive force of applying 30MPa, it is warming up to 1600 DEG C, insulation 10min, last sample furnace cooling, Sample is taken out, it is thus achieved that LaB when furnace temperature is less than 50 DEG C6-VB2Eutectic precast body；
Step 2, Wire EDM LaB6-VB2Coupon
With WEDM by LaB6-VB2Eutectic precast body cuts into coupon, and it is clear that coupon is placed in ultrasound wave in ethanol 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 upper pumping rod and the lower pumping rod of optics zone melting furnace, adjust and make upper and lower coupon suitably Position, then fills quartz ampoule, closes fire door；It is passed through argon, with the heating rate of no more than 80 DEG C/min in optics zone melting furnace Heating up, the end face making upper and lower coupon close to each other melts simultaneously；Directional solidification, growth rate is proceeded by after melting zone is stable For 1-1000mm/h, i.e. obtain LaB6-VB2Eutectic composites.
CN201610316212.XA 2016-05-11 2016-05-11 One kind prepares LaB using optics zone-melting technique6-VB2The method of eutectic composites Active CN105755540B (en)

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CN106882966A (en) * 2017-01-19 2017-06-23 合肥工业大学 One kind prepares SiC/LaB by optics zone-melting technique6The method of eutectic composites
CN109763170A (en) * 2019-03-25 2019-05-17 合肥工业大学 A kind of preparation method of high-performance Tetraheteropoly rare earth hexaboride-zirconium diboride composite material
CN115386778A (en) * 2022-08-12 2022-11-25 合肥工业大学 Lanthanum hexaboride eutectic composite material and preparation method thereof

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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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CN106882966A (en) * 2017-01-19 2017-06-23 合肥工业大学 One kind prepares SiC/LaB by optics zone-melting technique6The method of eutectic composites
CN109763170A (en) * 2019-03-25 2019-05-17 合肥工业大学 A kind of preparation method of high-performance Tetraheteropoly rare earth hexaboride-zirconium diboride 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
CN115386778A (en) * 2022-08-12 2022-11-25 合肥工业大学 Lanthanum hexaboride eutectic composite material and preparation method thereof

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