CN107245758A - A kind of multielement rare earth hexaboride（La0.6CexPr0.4‑x)B6The preparation method of monocrystal - Google Patents
A kind of multielement rare earth hexaboride（La0.6CexPr0.4‑x)B6The preparation method of monocrystal Download PDFInfo
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- CN107245758A CN107245758A CN201710441703.1A CN201710441703A CN107245758A CN 107245758 A CN107245758 A CN 107245758A CN 201710441703 A CN201710441703 A CN 201710441703A CN 107245758 A CN107245758 A CN 107245758A
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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
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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
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
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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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/02—Production of homogeneous polycrystalline material with defined structure directly from the solid state
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Abstract
The invention discloses a kind of multielement rare earth hexaboride (La0.6CexPr0.4‑x)B6The preparation method of monocrystal, is to prepare high-quality, high-performance, large-sized (La using plasma discharging burning technology combination optics zone-melting process0.6CexPr0.4‑x)B6Monocrystal.The gained single thing phase of sample of the invention, without impurity generation, and monocrystalline quality does not occur twinning well.
Description
Technical field
The invention belongs to rare-earth hexboride compound cathode material technical field, and in particular to multielement rare earth hexaboride monocrystal
Preparation method.
Background technology
LaB6And CeB6It is excellent hot cathode material, is widely used in military, civil area.But CeB6
And LaB6Negative electrode operating temperature is still higher, has influence on the life-span of device, therefore researcher wishes do not reducing the boronation of rare earth six
On the basis of thing emitting performance, the operating temperature of cathode material is reduced.Recent research result is proved in binary rare-earth hexaboride
The rare earth element of the middle other low work functions of doping, can effectively improve the emitting performance of cathode material, so that the negative electrode
Its emissivities can also meet the requirement of device to material at lower operating temperatures, the ternary hexaboride monocrystalline prepared at present
Such as：(La-Ce)B6、(La-Pr)B6、(Ce-Pr)B6Although their performances increase than binary rare-earth, but performance is still
Requirement is can not meet, therefore, in the urgent need to the preparation and the research of performance of development Tetraheteropoly rare earth hexaboride monocrystalline, but on
Large scale, high-quality, high-performance Tetraheteropoly rare earth hexaboride monocrystalline preparation have no report.
At present, the method for production of monocrystalline block mainly has：Al flux methods, fused salt electrolysis process, zone-melting process.Wherein, Al flux
Monocrystalline size that method is prepared is small, purity is low, it is impossible to realizes commercial Application demand, and is inevitably introduced in preparation process
Al impurity influences its emitting performance so as to reduce monocrystalline purity；And the cycle that fused salt electrolysis process prepares monocrystal is longer, obtain
To monocrystal easily contain other impurities, purity is relatively low, be only applicable to prepare be not very high small size list to purity requirement
Crystal.Zone-melting process be it is a kind of a small amount of material melted in relatively large Solid raw materials form stable melting zone, and melting zone is slowly led to
A kind of method of whole raw material is crossed, keeps stable during this, continuous melting zone is the necessary condition for preparing monocrystalline.With Al flux
Method is compared with fused salt electrolysis process, and zone-melting process can be used for preparing high-purity, large size single crystal.
The content of the invention
It is contemplated that overcome that existing single crystal preparation technology is present as monocrystalline size is small, the low defect of performance there is provided
A kind of high-quality, high-performance, large-sized multielement rare earth hexaboride (La0.6CexPr0.4-x)B6(0.1≤x≤0.3) monocrystal
Preparation method.
The present invention prepares high-quality, high-performance, big chi using discharge plasma sintering (SPS) technology combination optics zone-melting process
Very little multielement rare earth hexaboride (La0.6CexPr0.4-x)B6(0.1≤x≤0.3), is comprised the following steps that：
(1) according to 0.6：x：0.4-x mol ratio, 0.1≤x≤0.3, by LaB6、CeB6、PrB6Powder high-energy ball milling is equal
It is put into graphite jig, graphite jig is put into the cavity of discharge plasma sintering stove after even then, in vacuum 5-10Pa
Under be sintered, technological parameter is set to：1600-1700 DEG C of sintering temperature, sintering pressure 40-50MPa, soaking time 5min,
100-110 DEG C of heating rate/min；Cool to room temperature after the completion of sintering with the furnace, take out, obtain Polycrystalline；
(2) Polycrystalline is cut into polycrystalline rod, using two polycrystalline rods as loading rod and unloading rod, added
Carry out an area into optics zone melting furnace to melt, upper and lower charge bar is reversely rotated, velocity of rotation is 15-30rpm, the molten speed in an area
For 20-30mm/h；Whole crystal growing process is carried out in closed quartz ampoule, and argon stream is passed through in quartz ampoule；
(3) using the molten product in an area as loading rod, with LaB6Monocrystalline is added in optics zone melting furnace as unloading rod
Carry out secondary area to melt, upper and lower charge bar is reversely rotated, velocity of rotation is that to melt speed be 5-15mm/h for 15-30rpm, secondary area；Entirely
Crystal growing process is carried out in closed quartz ampoule, and argon stream is passed through in quartz ampoule；Obtained after secondary area is molten
(La0.6CexPr0.4-x)B6Monocrystal.
Further, LaB used in the above method6、CeB6、PrB6The purity of powder is not less than 99.9%, and granularity is
200-400 mesh.
Compared with existing single crystal preparation technology, the present invention has following beneficial effect：
Tetraheteropoly rare earth the hexaboride ((La that the inventive method is prepared0.6CexPr0.4-x)B6Monocrystal has size
Greatly, the advantages of quality is high, performance is good；Sample even thickness, surface are smooth it can be seen from the photo in kind of gained sample, say
Bright crystal growth is uniform；From the XRD spectrum and its single crystal X-ray diffraction collection of illustrative plates of gained sample, sample is monocrystalline and monocrystalline
Quality is good.
Brief description of the drawings
Fig. 1 is the (La that embodiment 1 is prepared0.6Ce0.1Pr0.3)B6The photo in kind of monocrystal；
Fig. 2 is the (La that embodiment 1 is prepared0.6Ce0.1Pr0.3)B6The XRD spectrum of monocrystal；
Fig. 3 is the (La that embodiment 1 is prepared0.6Ce0.1Pr0.3)B6The rocking curve collection of illustrative plates of monocrystal；
Fig. 4 is the (La that embodiment 1 is prepared0.6Ce0.1Pr0.3)B6The single crystal X-ray diffraction collection of illustrative plates of monocrystal；
Fig. 5 is the (La that embodiment 1 is prepared0.6Ce0.1Pr0.3)B6The VA characteristic curve of monocrystal.
Embodiment
With reference to specific embodiment, the present invention will be described.Following examples will be helpful to those skilled in the art
The present invention is further understood, but the invention is not limited in any way.It is any to be carried out on the premise of inventive concept is not changed
Any deformation and improvement, belong to protection scope of the present invention.
Discharge plasma sintering stove model LABOX-350 used in following embodiments；
Optics zone melting furnace model FZ-T-2000-X-I-VPO-PC used in following embodiments, is heated, often by four xenon lamps
Individual xenon lamp power is 5Kw, and maximum temperature is up to 3000 DEG C.
LaB used in following embodiments6、CeB6、PrB6The purity of powder is 99.9%, and granularity is 200-400 mesh.
Embodiment 1
The present embodiment prepares (La as follows0.6Ce0.1Pr0.3)B6Monocrystal：
(1) by LaB6、CeB6、PrB6Powder is according to 6:1:Be put into after 3 mol ratio high-energy ball milling is uniform internal diameter for 30mm,
Highly for 90mm graphite jig in, graphite jig is then put into the cavity of discharge plasma sintering stove (SPS), in vacuum
It is sintered under degree 5-10Pa, technological parameter is set to：1700 DEG C of sintering temperature, sintering pressure 40MPa, soaking time 5min,
100 DEG C/min of heating rate；Cool to room temperature after the completion of sintering with the furnace, take out, obtain Polycrystalline；
(2) Polycrystalline is cut into diameter of phi 6mm polycrystalline rods using Wire EDM equipment, by two polycrystalline rods point
Not as loading rod and unloading rod, it is added to area of progress in optics zone melting furnace and melts, to make melting zone more uniform, feeding, discharge
Rod is reversely rotated, and velocity of rotation is that to melt speed be 20mm/h for 15rpm, area；Whole crystal growing process is in closed quartz
Carried out in pipe, in order to effectively suppress to be passed through flowing argon gas in the volatilization and oxidation of La, Ce, Pr element in growth course, quartz ampoule；
(3) using the molten product in an area as loading rod, with LaB6Monocrystalline is added in optics zone melting furnace as unloading rod
Carry out secondary area to melt, upper and lower charge bar is reversely rotated, velocity of rotation is that to melt speed be 5mm/h for 15rpm, secondary area；Whole crystal life
Growth process is carried out in closed quartz ampoule, and flowing argon gas is passed through in quartz ampoule；Obtained after secondary area is molten
(La0.6Ce0.1Pr0.3)B6Monocrystal.
Fig. 1 is (La obtained by the present embodiment0.6Ce0.1Pr0.3)B6The photo in kind of monocrystal, it can be seen that
(La0.6Ce0.1Pr0.3)B6Monocrystal even thickness, surface are smooth, illustrate that crystal growth is uniform.Crystal diameter is about 6.1mm, long
Degree is about 22mm.
Fig. 2 is (La obtained by the present embodiment0.6Ce0.1Pr0.3)B6The XRD spectrum of monocrystal, it is single as a result to show crystal
Phase, without impurity generation, while collection of illustrative plates is shown as one group of parallel diffraction peak, meets the General Result of monocrystal XRD spectrum.
Fig. 3 is (La0.6Ce0.1Pr0.3)B6The rocking curve collection of illustrative plates of monocrystal, diffraction maximum is sharp, and symmetry is good, halfwidth
Only 0.148 °, show that monocrystalline crystalline quality is good.Fig. 4 is its single crystal X-ray diffraction collection of illustrative plates, as can be seen from the figure diffraction spot
Point is clear, separate, polycrystalline ring and splitting phenomena does not occur, can determine whether sample for monocrystalline and monocrystalline quality is good.
Fig. 5 is La obtained by the present embodiment0.6Ce0.1Pr0.3B6The VA characteristic curve of monocrystal, it is as can be seen from the figure outer
When making alive 1KV, 1600 DEG C of operating temperature, La0.6Ce0.1Pr0.3B6The heat emission current density of monocrystal is 51.06A/cm2, with
Binary rare-earth hexaboride monocrystalline is compared, and emission properties are obviously improved.
Embodiment 2
The present embodiment prepares (La by the identical mode of embodiment 10.6Ce0.2Pr0.2)B6Monocrystal, is differed only in：Step
(1) LaB in6、CeB6、PrB6The mol ratio of powder is 6:2:2nd, sintering temperature be 1600 DEG C, sintering pressure 50MPa, heating rate
For 110 DEG C/min；It is 25mm/h that speed is melted in an area in step (2)；It is 10mm/h that speed is melted in secondary area in step (3).
(the La obtained by the present embodiment it can be seen from photo in kind0.6Ce0.2Pr0.2)B6Monocrystal even thickness, surface light
It is sliding, illustrate that crystal growth is uniform.Crystal diameter is about 6.3mm, and length is 20mm.
From XRD spectrum and its single crystal X-ray diffraction collection of illustrative plates, sample obtained by the present embodiment is monocrystalline and monocrystalline quality is good
It is good.
Embodiment 3
The present embodiment prepares (La by the identical mode of embodiment 10.6Ce0.3Pr0.1)B6Monocrystal, is differed only in：Step
(1) LaB in6、CeB6、PrB6The mol ratio of powder is 6:3:1st, soaking time is 10min；Melt speed in an area in step (2)
For 30mm/h, charge bar rotates backward speed up and down is 30rpm；It is 15mm/h, up and down charge bar that speed is melted in secondary area in step (3)
Speed is rotated backward for 30rpm.
(the La obtained by the present embodiment it can be seen from photo in kind0.6Ce0.3Pr0.1)B6Monocrystal even thickness, surface light
It is sliding, illustrate that crystal growth is uniform.Crystal diameter is about 6mm, and length is 18mm.
From XRD spectrum and its single crystal X-ray diffraction collection of illustrative plates, sample obtained by the present embodiment is monocrystalline and monocrystalline quality is good
It is good.
These are only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Any modifications, equivalent substitutions and improvements made within principle etc., should be included in the scope of the protection.
Claims (2)
1. a kind of multielement rare earth hexaboride (La0.6CexPr0.4-x)B6The preparation method of monocrystal, it is characterised in that including following
Step：
(1) according to 0.6：x：0.4-x mol ratio, 0.1≤x≤0.3, by LaB6、CeB6、PrB6After powder high-energy ball milling is uniform
It is put into graphite jig, then graphite jig is put into the cavity of discharge plasma sintering stove, enters under vacuum 5-10Pa
Row sintering, technological parameter is set to：1600-1700 DEG C of sintering temperature, sintering pressure 40-50MPa, soaking time 5-10min rise
Warm 100-110 DEG C of speed/min；Cool to room temperature after the completion of sintering with the furnace, take out, obtain Polycrystalline；
(2) Polycrystalline is cut into polycrystalline rod, using two polycrystalline rods as loading rod and unloading rod, is added to light
Carry out area in the smelting furnace of school district to melt, upper and lower charge bar is reversely rotated, velocity of rotation is that to melt speed be 20- for 15-30rpm, an area
30mm/h；Whole crystal growing process is carried out in closed quartz ampoule, and argon stream is passed through in quartz ampoule；
(3) using the molten product in an area as loading rod, with LaB6Monocrystalline is added in optics zone melting furnace and carried out as unloading rod
Secondary area is melted, and upper and lower charge bar is reversely rotated, and velocity of rotation is that to melt speed be 5-15mm/h for 15-30rpm, secondary area；Whole crystal
Growth course is carried out in closed quartz ampoule, and argon stream is passed through in quartz ampoule；Obtained after secondary area is molten
(La0.6CexPr0.4-x)B6Monocrystal.
2. preparation method according to claim 1, it is characterised in that：LaB used6、CeB6、PrB6The purity of powder is equal
It is not less than 99.9%, granularity is 200-400 mesh.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108048907A (en) * | 2017-12-14 | 2018-05-18 | 合肥工业大学 | A kind of preparation method of large-size and high performance lanthanum hexaboride monocrystalline |
| 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 |
| 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 |
| CN114985737A (en) * | 2022-05-11 | 2022-09-02 | 合肥工业大学 | Multi-element hexaboride [100] monocrystal and preparation method thereof |
| CN115058775A (en) * | 2022-06-07 | 2022-09-16 | 合肥工业大学 | Large-size and high-performance ternary rare earth composite single crystal material and preparation method thereof |
| CN114985737B (en) * | 2022-05-11 | 2024-06-04 | 合肥工业大学 | Multi-element hexaboride [100] monocrystal and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102433587A (en) * | 2011-09-19 | 2012-05-02 | 北京工业大学 | Preparation method of multicomponent large-size rare earth boride LaxCe1-xB6 monocrystalline block cathode material |
| CN102808215A (en) * | 2012-06-28 | 2012-12-05 | 北京工业大学 | Preparation method of large-dimension multi-element rare earth boride (Ce0.9Pr0.1)B6 single crystal |
-
2017
- 2017-06-13 CN CN201710441703.1A patent/CN107245758B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102433587A (en) * | 2011-09-19 | 2012-05-02 | 北京工业大学 | Preparation method of multicomponent large-size rare earth boride LaxCe1-xB6 monocrystalline block cathode material |
| CN102808215A (en) * | 2012-06-28 | 2012-12-05 | 北京工业大学 | Preparation method of large-dimension multi-element rare earth boride (Ce0.9Pr0.1)B6 single crystal |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108048907A (en) * | 2017-12-14 | 2018-05-18 | 合肥工业大学 | A kind of preparation method of large-size and high performance lanthanum hexaboride monocrystalline |
| CN108048907B (en) * | 2017-12-14 | 2020-08-07 | 合肥工业大学 | Preparation method of large-size and high-performance lanthanum hexaboride single crystal |
| 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 |
| 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 |
| CN114985737A (en) * | 2022-05-11 | 2022-09-02 | 合肥工业大学 | Multi-element hexaboride [100] monocrystal and preparation method thereof |
| CN114985737B (en) * | 2022-05-11 | 2024-06-04 | 合肥工业大学 | Multi-element hexaboride [100] monocrystal and preparation method thereof |
| CN115058775A (en) * | 2022-06-07 | 2022-09-16 | 合肥工业大学 | Large-size and high-performance ternary rare earth composite single crystal material and preparation method thereof |
| CN115058775B (en) * | 2022-06-07 | 2024-03-19 | 合肥工业大学 | Large-size high-performance ternary rare earth composite single crystal material and preparation method thereof |
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