CN108940125A - It is a kind of to prepare Al13Fe3The method of single crystal grain - Google Patents
It is a kind of to prepare Al13Fe3The method of single crystal grain Download PDFInfo
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- CN108940125A CN108940125A CN201810608643.2A CN201810608643A CN108940125A CN 108940125 A CN108940125 A CN 108940125A CN 201810608643 A CN201810608643 A CN 201810608643A CN 108940125 A CN108940125 A CN 108940125A
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/08—Application of shock waves for chemical reactions or for modifying the crystal structure of substances
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Abstract
It is a kind of to prepare Al13Fe3The method of single crystal grain, its atom ratio for mainly pressing Al and Fe are as follows: Al 75-80%, Fe 20-25%, high-purity Al powder, Fe powder are fully ground after being uniformly mixed and are fitted into sintered-carbide die, preparation block is made in the pressure maintaining 5min under hydraulic tablet press machine 2-4MPa pressure；Preparation block is fitted into boron nitride crucible and assembles the tubular graphene furnace body of prebake, boron nitride crucible, boron nitride piece and graphite flake, it is put into cubic hinge press, pressure is controlled in static pressure such as 3-6GPa, and temperature is first heated between 1200-1250 DEG C, heat-insulation pressure keeping 30-60min；Then temperature is down to 1050-1100 DEG C, heat-insulation pressure keeping 1-3h.Present invention process is simple, low energy consumption, high-efficient, settles at one go from raw material to monocrystalline, need to can be only widely applied using conventional equipment.
Description
Technical field
The invention belongs to technical field of metal material, in particular to a kind of preparation method of single crystal grain.
Background technique
Metastable metal material itself has novel structure and excellent performance, the structure and property of the metastable metal material of high pressure
Further investigation can be equally worth.Al-Fe alloy system has complicated phasor and numerous intermetallic compounds.Many documents once from
The features such as it is big that different aspect introduces Al-Fe bianry alloy hardness, wear-resisting, corrosion-resistant and lightweight, while two kinds of aluminium, iron elements are on ground
Content in shell is very high, therefore alfer has very extensive application in terms of aviation components are with other.
Novel high-pressure metastable phase Al in the system13Fe3Appearance not only further enrich phasor content, but also to studying the system phase
Change process and high pressure metastable phase itself are of great significance.
The method that metal single crystal particle mainly uses high melt quickly to solidify was prepared in the past obtains monocrystalline phase, this high temperature
Melting method needs to consume more raw materials and process time compared to our high temperature and high pressure method, and this method is generally adopted
Raw material is block alloy, and the high purity powdered form compared to us is sintered, and the crystals that such method is prepared contain miscellaneous
Matter is more, brings many troubles to the dependence test in later period.And the method that this rapid cooling prepares single crystal grain is difficult to control
It forming core processed and is not easy to grow up, and there are many defects in crystal, generally require the solid phase-solid phase equilibration crystal growth in later period
The techniques such as annealing eliminate defect grown crystal, and the manufacturing cycle of monocrystalline greatly prolongs since then and preparation process is complicated.
Summary of the invention
Single crystal grain is prepared in order to simple and convenient, it is an object of that present invention to provide a kind of simple processes, at low cost, high-efficient
Preparation Al13Fe3The method of single crystal grain.
The present invention mainly uses high-pressure process, directly acts on pressure and uniformly mixes and be in heating melting state
On Al, Fe mixed raw material, the single crystal grain of single-phase micron order scale is directly made in starting cubic hinge press.The present invention has
The advantages that simple process, operating method is practical, and experimental facilities is relatively conventional, the method that powder directly generates are very suitable for
Al13Fe3Single crystal grain generates.
The method of the present invention is as follows:
(1)Al13Fe3The atom ratio of the chemical component of monocrystalline are as follows: Al 75-80%, Fe 20-25%, described Al, Fe are
High pure metal powder；
(2) high-purity Al powder, Fe powder are fully ground after being uniformly mixed and are fitted into sintered-carbide die, in hydraulic tablet press machine
Preparation block is made in pressure maintaining 5min under 2-4MPa pressure；
(3) graphite furnace tubulose furnace body both ends boron nitride piece is sealed, is set with boron nitride crucible, crucible both ends in graphite furnace
It is sealed with boron nitride piece, while graphite furnace both ends use graphite flake as package and conduction, then by above described tubular graphite furnace body, nitrogen
Change pyrophillite square that boron crucible, boron nitride piece and graphite flake are used together with cubic hinge press and conducting steel ring is put in temperature
Degree is spare to dry 2-5 hours in 150-200 DEG C of drying box.
(4) the preparation block of step (2) is fitted into boron nitride crucible and by the tubular graphene furnace of step (3) prebake
Body, boron nitride crucible, boron nitride piece and graphite flake assembling are put into cubic hinge press, and pressure control is in the static pressure such as 3-6GPa, temperature
Degree is first heated between 1200-1250 DEG C, heat-insulation pressure keeping 30-60min；Then temperature is down to 1050-1100 DEG C, heat-insulation pressure keeping 1-
3h。
The invention has the following advantages over the prior art:
1, simple process, low energy consumption, high-efficient, solve the complicated processes of other method feedstock processings, reduce the time,
It reduces costs, improves the preparation efficiency of monocrystalline, and influence of the pressure to crystal growth mechanism can be studied.
2, conventional equipment need to be only used, is a kind of efficient one-step synthesis, can be widely applied.
Detailed description of the invention
Fig. 1 is Al prepared by the embodiment of the present invention 113Fe3The EDS of monocrystalline schemes.
Fig. 2 is Al prepared by the embodiment of the present invention 113Fe3The SEM of monocrystalline schemes.
Fig. 3 is Al prepared by the embodiment of the present invention 213Fe3The EDS of monocrystalline schemes.
Fig. 4 is Al prepared by the embodiment of the present invention 213Fe3The SEM of monocrystalline schemes.
Fig. 5 is Al prepared by the embodiment of the present invention 1,2,3,413Fe3Crystal structure figure.
Specific embodiment
Embodiment 1
(1) high-purity Al powder (0.3201g) and Fe powder (0.2203g) are weighed by atom ratio (Al:Fe=75:25), it will
Two kinds of powder are fitted into after mixing in the sintered-carbide die of internal diameter Φ 5mm, the pressure maintaining under hydraulic tablet press machine 2MPa pressure
The prefabricated block of diameter of phi 5mm high 7.9mm is made in 5min.
(2) graphite furnace is the tubulose furnace body of high 15mm outer diameter Φ 8mm internal diameter Φ 6mm, is set with boron nitride crucible in graphite furnace,
Diameter of phi 5mm thickness 0.75mm boron nitride piece, diameter are successively used in the high 8mm outer diameter Φ 6mm internal diameter Φ 5mm of crucible, both ends from inside to outside
Φ 5mm thickness 2mm zirconium oxide piece and the sealing of Φ 5mm thickness 0.75mm boron nitride piece, graphite furnace periphery is also set with boron nitride crucible, crucible
High 15mm outer diameter Φ 10mm internal diameter Φ 8mm, peripheral boron nitride crucible is again by 15mm outer diameter Φ 14mm internal diameter Φ 10mm one high
Zirconium oxide crucible suit, while graphite furnace both ends package and conduction are diameter of phi 14mm thickness 1.6mm with graphite flake specification.Will more than
The pyrophillite square and conducting steel ring that material is used together with cubic hinge press are put in the drying box that temperature is 180 DEG C and dry 3
Hour is spare.
(3) prefabricated block prepared in step (1) is put into step (2) in the boron nitride crucible of prebake, will be nitrogenized
Boron crucible, tubular graphene furnace, oxidation zirconium crucible, graphite flake, boron nitride piece and zirconium oxide piece assemble be placed on six in certain sequence
In the high pressure apparatus of face, pressure is set as 5GPa, and peak temperature is controlled at 1230 DEG C, keeps the temperature 30min；Heat preservation when temperature is down to 1080 DEG C
2h, then direct turn-off current stops heating.
(4) take out and block and carry out surface cleaning, then broken into pieces, selected under ultramicroscopic observation specification 50~
150 μm of crystal grain is sticked on thin glass tube using glue and places progress single crystal diffraction test on four circular single crystal diffractometers,
Obtain the diffraction data of single crystal grain, it is determined that Al13Fe3Crystal structure, as shown in Figure 5.
Then it carries out EDS and SEM to sample to test, as depicted in figs. 1 and 2, from synthesis known to ingredient
Al81.05Fe18.95, atomic ratio and Al13Fe3Substantially it is consistent.It can determine whether Al by three of the above means of testing13Fe3Success is made
It is standby.
Embodiment 2
(1) high-purity Al powder (0.3308g) and Fe powder (0.2282g) are weighed by atom ratio (Al:Fe=75:25), it will
Two kinds of powder are fitted into after mixing in the sintered-carbide die of internal diameter Φ 5mm, the pressure maintaining under hydraulic tablet press machine 3MPa pressure
The prefabricated block of diameter of phi 5mm high 7.9mm is made in 5min.
(2) graphite furnace is the tubulose furnace body of high 15mm outer diameter Φ 8mm internal diameter Φ 6mm, is set with boron nitride crucible in graphite furnace,
Diameter of phi 5mm thickness 0.75mm boron nitride piece, diameter are successively used in the high 8mm outer diameter Φ 6mm internal diameter Φ 5mm of crucible, both ends from inside to outside
Φ 5mm thickness 2mm zirconium oxide piece and the sealing of Φ 5mm thickness 0.75mm boron nitride piece, graphite furnace periphery is also set with boron nitride crucible, crucible
High 15mm outer diameter Φ 10mm internal diameter Φ 8mm, peripheral boron nitride crucible is again by 15mm outer diameter Φ 14mm internal diameter Φ 10mm one high
Zirconium oxide crucible suit, while graphite furnace both ends package and conduction are diameter of phi 14mm thickness 1.6mm with graphite flake specification.Will more than
The pyrophillite square and conducting steel ring that material is used together with cubic hinge press are put in the drying box that temperature is 150 DEG C and dry 5
Hour is spare.
(3) prefabricated block prepared in step (1) is put into step (2) in the boron nitride crucible of prebake, will be nitrogenized
Boron crucible, tubular graphene furnace, oxidation zirconium crucible, graphite flake, boron nitride piece and zirconium oxide piece assemble be placed on six in certain sequence
In the high pressure apparatus of face, pressure is set as 4GPa, and peak temperature is controlled at 1220 DEG C, keeps the temperature 40min；Heat preservation when temperature is down to 1070 DEG C
1.5h, then direct turn-off current stops heating, and Al is made13Fe3Monocrystalline.
(4) it takes out block and carries out surface cleaning, obtained after being broken into pieces and largely contain Al13Fe3The block of single crystal grain, so
The crystal grain for selecting 50~150 μm under high magnification microscope afterwards, is sticked on thin glass tube using glue and places four circular single crystals
Single crystal diffraction test is carried out on diffractometer, obtains the diffraction data of single crystal grain, it is determined that Al13Fe3Crystal structure, such as Fig. 5 institute
Show.
EDS and SEM test is carried out to sample, determines ingredient, as shown in Figure 3, Figure 4.From synthesis known to ingredient
Al80.47Fe19.53, atomic ratio and Al13Fe3Substantially it is consistent.It can determine whether to be successfully prepared by three of the above means of testing
Al13Fe3Single crystal grain.
Embodiment 3
(1) high-purity Al powder (0.4213g) and Fe powder (0.2180g) are weighed by atom ratio (Al:Fe=80:20), it will
Two kinds of powder are fitted into after mixing in the sintered-carbide die of internal diameter Φ 5mm, the pressure maintaining under hydraulic tablet press machine 4MPa pressure
The prefabricated block of diameter of phi 5mm high 7.9mm is made in 5min.
(2) graphite furnace is the tubulose furnace body of high 15mm outer diameter Φ 8mm internal diameter Φ 6mm, is set with boron nitride crucible in graphite furnace,
Diameter of phi 5mm thickness 0.75mm boron nitride piece, diameter are successively used in the high 8mm outer diameter Φ 6mm internal diameter Φ 5mm of crucible, both ends from inside to outside
Φ 5mm thickness 2mm zirconium oxide piece and the sealing of Φ 5mm thickness 0.75mm boron nitride piece, graphite furnace periphery is also set with boron nitride crucible, crucible
High 15mm outer diameter Φ 10mm internal diameter Φ 8mm, peripheral boron nitride crucible is again by 15mm outer diameter Φ 14mm internal diameter Φ 10mm one high
Zirconium oxide crucible suit, while graphite furnace both ends package and conduction are diameter of phi 14mm thickness 1.6mm with graphite flake specification.Will more than
The pyrophillite square and conducting steel ring that material is used together with cubic hinge press are put in the drying box that temperature is 200 DEG C and dry 2
Hour is spare.
(3) prefabricated block prepared in step (1) is put into step (2) in the boron nitride crucible of prebake, will be nitrogenized
Boron crucible, tubular graphene furnace, oxidation zirconium crucible, graphite flake, boron nitride piece and zirconium oxide piece assemble be placed on six in certain sequence
In the high pressure apparatus of face, pressure is set as 3GPa, and peak temperature is controlled at 1200 DEG C, keeps the temperature 60min；Heat preservation when temperature is down to 1050 DEG C
2h, then direct turn-off current stops heating, and Al is made13Fe3Crystal.
(4) take out and block and carry out surface cleaning, then broken into pieces, selected under ultramicroscopic observation specification 50~
150 μm of crystal grain is sticked on thin glass tube using glue and places progress single crystal diffraction test on four circular single crystal diffractometers,
Obtain the diffraction data of single crystal grain, it is determined that Al13Fe3Crystal structure, as shown in Figure 5.
Embodiment 4
(1) high-purity Al powder (0.3451g) and Fe powder (0.1786g) are weighed by atom ratio (Al:Fe=75:25), it will
Two kinds of powder are fitted into after mixing in the sintered-carbide die of internal diameter Φ 5mm, the pressure maintaining under hydraulic tablet press machine 4MPa pressure
The prefabricated block of diameter of phi 5mm high 7.9mm is made in 5min.
(2) graphite furnace is the tubulose furnace body of high 15mm outer diameter Φ 8mm internal diameter Φ 6mm, is set with boron nitride crucible in graphite furnace,
Diameter of phi 5mm thickness 0.75mm boron nitride piece, diameter are successively used in the high 8mm outer diameter Φ 6mm internal diameter Φ 5mm of crucible, both ends from inside to outside
Φ 5mm thickness 2mm zirconium oxide piece and the sealing of Φ 5mm thickness 0.75mm boron nitride piece, graphite furnace periphery is also set with boron nitride crucible, crucible
High 15mm outer diameter Φ 10mm internal diameter Φ 8mm, peripheral boron nitride crucible is again by 15mm outer diameter Φ 14mm internal diameter Φ 10mm one high
Zirconium oxide crucible suit, while graphite furnace both ends package and conduction are diameter of phi 14mm thickness 1.6mm with graphite flake specification.Will more than
The pyrophillite square and conducting steel ring that material is used together with cubic hinge press are put in the drying box that temperature is 170 DEG C and dry 4
Hour is spare.
(3) prefabricated block prepared in step (1) is put into step (2) in the boron nitride crucible of prebake, will be nitrogenized
Boron crucible, tubular graphene furnace, oxidation zirconium crucible, graphite flake, boron nitride piece and zirconium oxide piece assemble be placed on six in certain sequence
In the high pressure apparatus of face, pressure is set as 6GPa, and peak temperature is controlled at 1250 DEG C, keeps the temperature 50min；Heat preservation when temperature is down to 1100 DEG C
3h, then direct turn-off current stops heating, and Al is made13Fe3Crystal.
(4) take out and block and carry out surface cleaning, then broken into pieces, selected under ultramicroscopic observation specification 50~
150 μm of crystal grain is sticked on thin glass tube using glue and places progress single crystal diffraction test on four circular single crystal diffractometers,
Obtain the diffraction data of single crystal grain, it is determined that Al13Fe3Crystal structure, as shown in Figure 5.
Claims (2)
1. a kind of prepare Al13Fe3The method of single crystal grain, it is characterised in that: it includes the following steps:
(1)Al3The atom ratio of the chemical component of Fe monocrystalline are as follows: Al 75-80%, Fe 20-25%；
(2) Al powder, Fe powder are fully ground after being uniformly mixed and are fitted into sintered-carbide die, pressed in hydraulic tablet press machine 2-4MPa
Preparation block is made in pressure maintaining 5min under power；
(3) graphite furnace tubulose furnace body both ends boron nitride piece is sealed, is set with boron nitride crucible, crucible both ends nitrogen in graphite furnace
Change the sealing of boron piece, while graphite furnace both ends use graphite flake as package and conduction, then by above described tubular graphite furnace body, boron nitride
The pyrophillite square and conducting steel ring that crucible, boron nitride piece and graphite flake are used together with cubic hinge press are put in temperature and are
Dried in 150-200 DEG C of drying box 2-5 hours it is spare.
(4) the preparation block of step (2) is fitted into boron nitride crucible and by tubular graphene furnace body, the nitrogen of step (3) prebake
Change boron crucible, boron nitride piece and graphite flake assembling, be put into cubic hinge press, in static pressure such as 3-6GPa, temperature is first for pressure control
It is heated between 1200-1250 DEG C, heat-insulation pressure keeping 30-60min；Then temperature is down to 1050-1100 DEG C, heat-insulation pressure keeping 1-3h.
2. preparing Al according to claim 113Fe3The method of single crystal grain, it is characterised in that: the Al and Fe is high-purity
The metal powder of degree.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2101903B1 (en) * | 2006-12-13 | 2012-03-14 | Diamond Innovations, Inc. | Abrasive compacts with improved machinability |
| CN102600768A (en) * | 2012-03-30 | 2012-07-25 | 常熟市怡华金刚石有限公司 | Indirect heating-type synthesis assembly for high-temperature and high-pressure artificial single crystal synthesis by using cubic press |
| CN106399732A (en) * | 2016-09-27 | 2017-02-15 | 华南理工大学 | Method for preparing Al-Sn based bearing bush alloy by powder sintering |
| CN106784703A (en) * | 2016-12-27 | 2017-05-31 | 天津先众新能源科技股份有限公司 | A kind of preparation method with high compacted density monocrystalline positive electrode |
| CN107185459A (en) * | 2017-07-27 | 2017-09-22 | 燕山大学 | A kind of preparation method of Al4Cu9 single crystal grains |
-
2018
- 2018-06-13 CN CN201810608643.2A patent/CN108940125A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2101903B1 (en) * | 2006-12-13 | 2012-03-14 | Diamond Innovations, Inc. | Abrasive compacts with improved machinability |
| CN102600768A (en) * | 2012-03-30 | 2012-07-25 | 常熟市怡华金刚石有限公司 | Indirect heating-type synthesis assembly for high-temperature and high-pressure artificial single crystal synthesis by using cubic press |
| CN106399732A (en) * | 2016-09-27 | 2017-02-15 | 华南理工大学 | Method for preparing Al-Sn based bearing bush alloy by powder sintering |
| CN106784703A (en) * | 2016-12-27 | 2017-05-31 | 天津先众新能源科技股份有限公司 | A kind of preparation method with high compacted density monocrystalline positive electrode |
| CN107185459A (en) * | 2017-07-27 | 2017-09-22 | 燕山大学 | A kind of preparation method of Al4Cu9 single crystal grains |
Non-Patent Citations (1)
| Title |
|---|
| ZHENG XIA ET AL: "《Al13Fe3》", 《IUCRDATA》 * |
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