CN106007727A - Method for preparing LaB6/ZrB2 eutectic composites in rapid sintering mode - Google Patents

Method for preparing LaB6/ZrB2 eutectic composites in rapid sintering mode Download PDF

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CN106007727A
CN106007727A CN201610316167.8A CN201610316167A CN106007727A CN 106007727 A CN106007727 A CN 106007727A CN 201610316167 A CN201610316167 A CN 201610316167A CN 106007727 A CN106007727 A CN 106007727A
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powder
zrb
lab
mixed
sintering
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张久兴
王翔
杨新宇
胡可
李志�
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Hefei University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3804—Borides
    • C04B2235/3813—Refractory metal borides

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  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a method for preparing LaB6/ZrB2 eutectic composites in a rapid sintering mode. The method is characterized by including the steps that ZrB2 power and LaB6 powder are mixed with a high-energy ball mill, screened, subjected to prepressing forming and finally sintered in a discharging plasma sintering furnace, and the LaB6/ZrB2 eutectic composites are obtained. The LaB6/ZrB2 eutectic composites prepared with the discharging plasma sintering technology have high density which can be 98.43%.

Description

A kind of Fast Sintering prepares LaB6/ZrB2The method of eutectic composites
Technical field
The present invention relates to one and prepare LaB6/ZrB2The method of eutectic composites, belongs to technical field of new material preparation.
Background technology
Zirconium diboride (ZrB2) owing to unique metal is strong, covalent bond, ionic bond interact, thus have high-melting-point (3040 DEG C), The characteristics such as high rigidity and excellent conduction, heat conduction, are the high-temperature ceramic materials of a kind of excellent performance, the most at aviation, metallurgy Well applied Deng high-temperature field.LaB6The advantage such as high-melting-point, low work function, low evaporation rate and longer service life, Can be as the hot cathode material with high emission electric current density.LaB6/ZrB2Eutectic composites inherit ZrB2Excellent mechanical is special Property and LaB6Good heat emission characteristic, is therefore a kind of composite integrating function and structure.
At present, only LaB is prepared by traditional hot pressing sintering method6/ZrB2The report of eutectic composites.
Document " Ordan'yan S S, Paderno Y B, Khoroshilova I K, et al.Interaction in the LaB6-ZrB2 System [J] .Powder Metallurgy and Metal Ceramics, 1983,22 (11): 946-948. " disclose one to prepare LaB6/ZrB2The method of system.The technology preparation i.e. using traditional hot pressed sintering has different ZrB2The LaB of content6/ZrB2 System, the document mainly have studied different ZrB2The LaB of content6/ZrB2The fusing point of system, lattice parameter and microhardness.
Conventional thermocompression sintering technology generally uses the nano raw material powder of high cost, adds the sintering aid of the low melting points such as Ni in the powder To improve sintered density, but low melting point sintering aid forms glass phase when cooling, has had a strong impact on the high-temperature behavior of material, Make deformation increase, intensity decline, and owing to sintering temperature is higher, sintering time is long, its high energy consumption, inefficient shortcoming are very big Limit the industrial applications that this material is following.
Therefore, it is badly in need of researching and developing the preparation LaB of a kind of high efficiency, low cost without adding sintering aid at present6/ZrB2Eutectic composite wood The method of material.
Summary of the invention
The present invention is for avoiding the weak point existing for above-mentioned prior art, it is provided that a kind of Fast Sintering prepares LaB6/ZrB2Altogether The method of crystal composite material, it is intended to use discharge plasma sintering technique, by accurately controlling the rate of heat addition, sintering temperature and guarantor The temperature time, thus obtain the LaB of high-compactness6/ZrB2Eutectic composites.
The present invention solves technical problem, adopts the following technical scheme that
Fast Sintering of the present invention prepares LaB6/ZrB2The method of eutectic composites, its feature is to comprise the steps:
Step one, join powder
It is not less than 99%ZrB with purity2Powder and purity are not less than the LaB of 99%6Powder is raw material, by 21wt.% ZrB2-79wt.%LaB6The mass percent of eutectic phasor, carries out joining powder in glove box；
Step 2, ball milling
Powder step one prepared loads in ball grinder, is passed through argon atmosphere, after evacuation then on planetary ball mill Carry out high-energy ball milling, it is thus achieved that LaB6/ZrB2Mixed-powder；By described LaB6/ZrB2Mixed-powder is placed in electric vacunm drying case Being dried, drying condition is preferably temperature 100 DEG C, time 24h；
Step 3, sieve powder
In mechanical milling process, temperature is higher, the easy overheated caking of powder, is unfavorable for sintering, in order to solve the caking of powder after ball milling Agglomeration, uses the sieve of 300 mesh to described LaB on vibration-type screen(ing) machine6/ZrB2Mixed-powder screens, it is thus achieved that sieve LaB after choosing6/ZrB2Mixed-powder；
Step 4, precompressed
LaB after screening6/ZrB2Mixed-powder puts into graphite jig, by the adjustment of mold and punching head so that powder is in stone In the middle of ink mould, then graphite jig being placed in pre-molding on hand press, the pressure of precompressed is preferably 10MPa；
Step 5, discharge plasma sintering
Graphite jig after precompressed is placed in the furnace chamber of discharge plasma sintering stove, evacuation, apply 30MPa axial compressive force, Heating rate is set；Start sintering after, electric current is gradually increased with special speed, when mold temperature reach set sintering temperature 1600～ When 1900 DEG C, start insulation；Insulation 3～15min, cuts off electric current, sample furnace cooling, takes out examination when furnace temperature is less than 50 DEG C Sample, i.e. obtains LaB6/ZrB2Eutectic composites.
The speed heated up in step 5 is not higher than 100 DEG C/min.
Compared with prior art, the invention have the advantages that
(1) present invention prepares LaB by discharge plasma sintering technique6/ZrB2Eutectic composites, method is simple, it is not necessary to add Add sintering aid；And products obtained therefrom has higher consistency, reach 98.43%.
(2) raw material range is wide: plasma sintering technique can particle surface moment produce high temperature (more than 2000 DEG C), thus Particle surface causes evaporation and melts, desorption and oxide-film, makes particle surface activate, can make other conventional sintering skill The material that art can not sinter realizes sintering.
(3) Fast Sintering: due to pulse current moment, interrupted, the high frequency of plasma sintering technique generation, connect at powder particle Contact portion position produces Joule heat, is producing heat discharge not in contact with position, and electric field diffusion effect enhances the atom of powder particle greatly Diffusion velocity (more much bigger than traditional sintering techniques), thus realize the Fast Sintering of powder.
(4) uniformly heating: the pulse current that plasma sintering technique produces, can make grain contact point produce plasma discharging, from And the consistent heat generation of each granule in realizing precast body, the thermal efficiency is high, and performance is good.
(5) sintering temperature is low: powder is acted on by pulse current and vertical uniaxial pressure, produces the strongest diffusion field (thermal efficiency High) so that in the case of lower than conventional sintering temperature 200-500 DEG C of sintering temperature, it is achieved sintering.
Accompanying drawing explanation
Fig. 1 is the LaB prepared by the embodiment of the present invention 16/ZrB2The tissue topography of eutectic composites (sintering temperature is 1600 DEG C, Temperature retention time 5min)；
Fig. 2 is the LaB prepared by the embodiment of the present invention 26/ZrB2The tissue topography of eutectic composites (sintering temperature is 1800 DEG C, Temperature retention time 5min)；
Fig. 3 is the LaB prepared by the embodiment of the present invention 36/ZrB2The tissue topography of eutectic composites (sintering temperature is 1900 DEG C, Temperature retention time 5min).
Detailed description of the invention
Embodiment 1
The present embodiment prepares LaB as follows6/ZrB2Eutectic composites:
Step one, join powder
With purity be 99%, particle diameter be about the ZrB of 2 μm2Powder and purity are 99%, particle diameter is about the LaB of 45 μm6Powder For raw material, by 21wt.%ZrB2-79wt.%LaB6The mass percent of eutectic phasor, carries out joining powder in glove box；
Step 2, ball milling
Powder step one prepared loads in ball grinder, is passed through argon atmosphere, after evacuation then on planetary ball mill After carrying out high-energy ball milling 4h, it is thus achieved that LaB6/ZrB2Mixed-powder；By LaB6/ZrB2Mixed-powder is placed in electric vacunm drying case In, 100 DEG C of dry 24h；
Step 3, sieve powder
In mechanical milling process, temperature is higher, the easy overheated caking of powder, is unfavorable for sintering, in order to solve the caking of powder after ball milling Agglomeration, uses the sieve of 300 mesh to LaB on vibration-type screen(ing) machine6/ZrB2Mixed-powder screens, remove 50 μm with On big agglomerated powder granules, it is thus achieved that LaB after screening6/ZrB2Mixed-powder；
Step 4, precompressed
LaB after screening6/ZrB2Mixed-powder puts into the graphite jig that internal diameter is 20.4mm, by the adjustment of mold and punching head, Making powder be in the middle of graphite jig, then graphite jig is placed in pre-molding on hand press, the pressure of precompressed is 10MPa；
Step 5, discharge plasma sintering
Graphite jig after precompressed is placed in the furnace chamber of discharge plasma sintering stove, evacuation, apply 30MPa axial compressive force, Arranging heating rate is 100 DEG C/min；After starting sintering, electric current is gradually increased with special speed, burns when mold temperature reaches to set During junction temperature 1600 DEG C, start insulation；Insulation 5min, cuts off electric current, sample furnace cooling, takes when furnace temperature is less than 50 DEG C Go out sample, i.e. obtain LaB6/ZrB2Eutectic composites.
The microstructure of the present embodiment gained sample is as shown in Figure 1, it can be seen that at ZrB2Porous occurs on matrix；After tested, The consistency of the present embodiment gained sample is 79.49%.
Embodiment 2
The present embodiment prepares LaB as follows6/ZrB2Eutectic composites:
Step one, join powder
With purity be 99%, particle diameter be about the ZrB of 2 μm2Powder and purity are 99%, particle diameter is about the LaB of 45 μm6Powder For raw material, by 21wt.%ZrB2-79wt.%LaB6The mass percent of eutectic phasor, carries out joining powder in glove box；
Step 2, ball milling
Powder step one prepared loads in ball grinder, is passed through argon atmosphere, after evacuation then on planetary ball mill After carrying out high-energy ball milling 4h, it is thus achieved that LaB6/ZrB2Mixed-powder；By described LaB6/ZrB2Mixed-powder is placed in electrothermal vacuum and does In dry case, 100 DEG C of dry 24h；
Step 3, sieve powder
In mechanical milling process, temperature is higher, the easy overheated caking of powder, is unfavorable for sintering, in order to solve the caking of powder after ball milling Agglomeration, uses the sieve of 300 mesh to LaB on vibration-type screen(ing) machine6/ZrB2Mixed-powder screens, remove 50 μm with On big agglomerated powder granules, it is thus achieved that LaB after screening6/ZrB2Mixed-powder；
Step 4, precompressed
LaB after screening6/ZrB2Mixed-powder puts into the graphite jig that internal diameter is 20.4mm, by the adjustment of mold and punching head, Making powder be in the middle of graphite jig, then graphite jig is placed in pre-molding on hand press, the pressure of precompressed is 10MPa；
Step 5, discharge plasma sintering
Graphite jig after precompressed is placed in the furnace chamber of discharge plasma sintering stove, evacuation, apply 30MPa axial compressive force, Arranging heating rate is 100 DEG C/min；After starting sintering, electric current is gradually increased with special speed, burns when mold temperature reaches to set During junction temperature 1800 DEG C, start insulation；Insulation 5min, cuts off electric current, sample furnace cooling, takes when furnace temperature is less than 50 DEG C Go out sample, i.e. obtain LaB6/ZrB2Eutectic composites.
The microstructure of the present embodiment gained sample is as shown in Figure 2, it can be seen that ZrB2Matrix and LaB6Strengthen and combine more preferably, And space significantly reduces on matrix；After tested, the consistency of the present embodiment gained sample is 98.27%.
Embodiment 3
The present embodiment prepares LaB as follows6/ZrB2Eutectic composites:
Step one, join powder
With purity be 99%, particle diameter be about the ZrB of 2 μm2Powder and purity are 99%, particle diameter is about the LaB of 45 μm6Powder For raw material, by 21wt.%ZrB2-79wt.%LaB6The mass percent of eutectic phasor, carries out joining powder in glove box；
Step 2, ball milling
Powder step one prepared loads in ball grinder, is passed through argon atmosphere, after evacuation then on planetary ball mill After carrying out high-energy ball milling 4h, it is thus achieved that LaB6/ZrB2Mixed-powder；By described LaB6/ZrB2Mixed-powder is placed in electrothermal vacuum and does In dry case, 100 DEG C of dry 24h；
Step 3, sieve powder
In mechanical milling process, temperature is higher, the easy overheated caking of powder, is unfavorable for sintering, in order to solve the caking of powder after ball milling Agglomeration, uses the sieve of 300 mesh to screen powder on vibration-type screen(ing) machine, removes the big reunion of more than 50 μm Powder particle, it is thus achieved that LaB after screening6/ZrB2Mixed-powder；
Step 4, precompressed
LaB after screening6/ZrB2Mixed-powder puts into the graphite jig that internal diameter is 20.4mm, by the adjustment of mold and punching head, Making powder be in the middle of graphite jig, then graphite jig is placed in pre-molding on hand press, the pressure of precompressed is 10MPa；
Step 5, discharge plasma sintering
Graphite jig after precompressed is placed in the furnace chamber of discharge plasma sintering stove, evacuation, apply 30MPa axial compressive force, Arranging heating rate is 100 DEG C/min；After starting sintering, electric current is gradually increased with special speed, burns when mold temperature reaches to set During junction temperature 1900 DEG C, start insulation；Insulation 5min, cuts off electric current, sample furnace cooling, takes when furnace temperature is less than 50 DEG C Go out sample, i.e. obtain LaB6/ZrB2Eutectic composites.
As it is shown on figure 3, after tested, the consistency of the present embodiment gained sample is the microstructure of the present embodiment gained sample 98.43%.

Claims (4)

1. a Fast Sintering prepares LaB6/ZrB2The method of eutectic composites, it is characterised in that comprise the steps:
Step one, join powder
The ZrB of 99% it is not less than with purity2Powder and purity are not less than the LaB of 99%6Powder is raw material, by 21wt.% ZrB2-79wt.%LaB6The mass percent of eutectic phasor, carries out joining powder in glove box；
Step 2, ball milling
Powder step one prepared loads in ball grinder, is passed through argon atmosphere, after evacuation then on planetary ball mill Carry out high-energy ball milling, it is thus achieved that LaB6/ZrB2Mixed-powder；By described LaB6/ZrB2Mixed-powder is placed in electric vacunm drying case It is dried；
Step 3, sieve powder
Use the sieve of 300 mesh to described LaB on vibration-type screen(ing) machine6/ZrB2Mixed-powder screens, it is thus achieved that after screening LaB6/ZrB2Mixed-powder；
Step 4, precompressed
LaB after screening6/ZrB2Mixed-powder puts into graphite jig, by the adjustment of mold and punching head so that powder is in graphite In the middle of mould, then graphite jig is placed in pre-molding on hand press；
Step 5, discharge plasma sintering
Graphite jig after precompressed is placed in the furnace chamber of discharge plasma sintering stove, evacuation, apply 30MPa axial compressive force, Being warming up to 1600～1900 DEG C, be incubated 3～15min, sample furnace cooling, when furnace temperature is less than 50 DEG C, taking-up sample, i.e. obtains Obtain LaB6/ZrB2Eutectic composites.
Method the most according to claim 1, it is characterised in that: the baking temperature in step 2 is 100 DEG C, drying time For 24h.
Method the most according to claim 1, it is characterised in that: in step 4, the pressure of pre-molding is 10MPa.
Method the most according to claim 1, it is characterised in that: the speed heated up in step 5 is not higher than 100 DEG C/min.
CN201610316167.8A 2016-05-11 2016-05-11 Method for preparing LaB6/ZrB2 eutectic composites in rapid sintering mode Pending CN106007727A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
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
CN111825463A (en) * 2020-06-29 2020-10-27 井冈山大学 LaB6-CrB2Composite cathode material and preparation method thereof
CN112872360A (en) * 2021-01-13 2021-06-01 太原理工大学 Mixed forming method of iron-based wear-resistant material
CN114590816A (en) * 2022-03-10 2022-06-07 合肥工业大学 Preparation method of strontium hexaboride powder
CN114920560A (en) * 2022-05-05 2022-08-19 兰州理工大学 LaB 6 Powder and method for producing sintered body thereof
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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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN111825463A (en) * 2020-06-29 2020-10-27 井冈山大学 LaB6-CrB2Composite cathode material and preparation method thereof
CN112872360A (en) * 2021-01-13 2021-06-01 太原理工大学 Mixed forming method of iron-based wear-resistant material
CN112872360B (en) * 2021-01-13 2024-01-02 山西盛世永恒工程咨询有限公司 Mixed forming method of iron-based wear-resistant material
CN114590816A (en) * 2022-03-10 2022-06-07 合肥工业大学 Preparation method of strontium hexaboride powder
CN114920560A (en) * 2022-05-05 2022-08-19 兰州理工大学 LaB 6 Powder and method for producing sintered body thereof
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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