CN107185459A - A kind of preparation method of Al4Cu9 single crystal grains - Google Patents
A kind of preparation method of Al4Cu9 single crystal grains Download PDFInfo
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- CN107185459A CN107185459A CN201710622158.6A CN201710622158A CN107185459A CN 107185459 A CN107185459 A CN 107185459A CN 201710622158 A CN201710622158 A CN 201710622158A CN 107185459 A CN107185459 A CN 107185459A
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- boron nitride
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- 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
- B01J3/062—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
Abstract
A kind of Al4Cu9The preparation method of single crystal grain, Al4Cu9The atom ratio of the chemical composition of monocrystalline is：Al 28 31%, Cu 69 72%；Its preparation method is put into sintered-carbide die after mainly high-purity Al powder is well mixed with Cu powder, is applied 3MPa pressure using powder compressing machine and is kept about 180s to obtain prefabricated block；Obtained prefabricated block is put into boron nitride crucible, it is placed in after boron nitride crucible, tubular graphene stove, graphite flake, boron nitride piece are assembled in order in cubic hinge press, pressure is arranged between 3 5GPa, and peak temperature is controlled at 1100 DEG C 1150 DEG C, is incubated 30min；Temperature is incubated 1 2h when being down to 800 DEG C 950 DEG C.The present invention has technique simple, and operating method is truly feasible, the advantages of experimental facilities is relatively conventional, and generation monocrystalline quality is preferable.
Description
Technical field
The invention belongs to technical field of metal material, more particularly to a kind of preparation method of single crystal grain.
Background technology
Science and technology today's society with rapid changepl. never-ending changes and improvements finds innumerable with the material synthesized.Made of Al-Cu alloy is a kind of typical
Alloy system, such as Al is compared with many alloys2Cu、AlCu3And Al4Cu9Etc., function admirable is widely used.Material
Application determined by its performance, and structures shape performance, when us it should be appreciated that not only needing to do performance survey during a kind of material
Examination, should also start with from structure.And a kind of structure of material is measured, monocrystalline will be provided and greatly helped.The existing monocrystalline of preparing
Method is a lot, but all more complicated cumbersome.
The content of the invention
Monocrystalline is prepared in order to simple and convenient, a kind of technique of the object of the invention offer is simple, generation single crystal grain quality is preferable
Al4Cu9The preparation method of single crystal grain.The present invention mainly prepares Al to net income with high-pressure process4Cu9Single crystalline uniform mixes it
Afterwards Al is prepared using high-pressure process4Cu9Monocrystalline.
Technical scheme is as follows：
(1)Al4Cu9The atom ratio of the chemical composition of monocrystalline is：Al 28-31%, Cu 69-72%；
(2) high-purity Al powder and Cu powder are well mixed, apply 2-3MPa pressure with powder compressing machine and keep about 180s,
Prefabricated block is made；
(3) by graphite furnace tubulose body of heater two ends boron nitride piece covering, boron nitride crucible, crucible two ends are set with graphite furnace
Sealed with boron nitride piece, while graphite furnace two ends graphite flake is as parcel and conduction, then by above described tubular graphite body of heater, nitrogen
Pyrophillite square and conductive steel that change boron crucible, boron nitride piece, pyrophillite piece and graphite flake are used together with cubic hinge press
It is standby to dry 3 hours in 180 DEG C of drying baker that circle is put in temperature；
(4) prefabricated block prepared in step (2) is put into the boron nitride crucible of step (3) prebake, by boron nitride
Crucible, tubular graphene stove, graphite flake, boron nitride piece are placed in cubic hinge press after assembling in order, and pressure is set to 3-5GPa,
Peak temperature is controlled at 1100 DEG C -1150 DEG C, is incubated 30min；Temperature is incubated 1-2h when being down to 800 DEG C -950 DEG C.
The present invention has advantages below compared with prior art：
Technique is simple, and operating method is truly feasible, it is not necessary to complicated equipment, without the need for the excessive place of raw material
Reason just directly can carry out synthetic single crystal phase using raw material, and generation single crystal grain quality preferably, and can meet a variety of monocrystalline
The preparation of phase constituent.
Brief description of the drawings
Fig. 1 is Al prepared by the embodiment of the present invention 14Cu9The EDS figures of single crystal grain.
Fig. 2 is Al prepared by the embodiment of the present invention 14Cu9The SEM figures of single crystal grain.
Fig. 3 is Al prepared by the embodiment of the present invention 24Cu9The SEM figures of single crystal grain.
Fig. 4 is Al prepared by the embodiment of the present invention 34Cu9The SEM figures of single crystal grain.
Embodiment
Embodiment 1
(1) atom ratio (Al is pressed:Cu=30:70) the high-purity Al powder of 0.56422g and 3.00850g Cu powder are weighed, by two
Is fitted into after kind of powder is well mixed in internal diameter Φ 9.6mm sintered-carbide die, with powder compressing machine pressurization 3MPa and keeps
180s, obtains the high 10mm of diameter of phi 9.6mm prefabricated block；
(2) graphite furnace is high 16.6mm external diameters Φ 14mm internal diameters Φ 12mm tubulose bodies of heater, two ends Φ 12mm thickness 3.3mm nitrogen
Change in the sealing of boron piece, graphite furnace and be set with boron nitride crucible, the high 10mm external diameters Φ 12mm internal diameters Φ 9.6mm of crucible, two ends diameter
Φ 9.6mm thickness 1.2mm boron nitride piece is sealed, while graphite furnace two ends parcel and conduction are that diameter of phi 14 is thick with graphite flake specification
1.6mm, by graphite furnace, boron nitride crucible, boron nitride piece, the pyrophillite square and conducting steel ring used together with cubic hinge press
It is standby to dry 3 hours in 180 DEG C of drying baker to be put in temperature；
(3) prefabricated block for preparing step (1) is put into step (2) in the boron nitride crucible of prebake, by boron nitride
Crucible, tubular graphene stove, graphite flake, boron nitride piece are placed in cubic hinge press after assembling in order, and pressure is set to 5GPa, peak
It is worth temperature control at 1150 DEG C, is incubated 30min；Temperature is incubated 2h when being down to 950 DEG C.Then direct turn-off current stops heating；
(4) take out block and carry out surface cleaning, obtain and contain Al4Cu9The block of single crystal grain.
To Al4Cu9Single crystal grain block carries out EDS tests, determines composition, as shown in figure 1, understanding to close from the compositions of Spot 2
Into Al30.89Cu69.11, its atomic ratio and Al4Cu9It is consistent, thus can determine whether Al4Cu9Monocrystalline is mutually successfully prepared.
Then single crystal diffraction test is carried out, Al is determined4Cu9Mono-crystalline structures, as shown in Figure 2.
Embodiment 2
(1) atom ratio (Al is pressed:Cu=28:72) the high-purity Al powder of 0.50738g and 3.09259g Cu powder are weighed, by two
Is fitted into after kind of powder is well mixed in internal diameter Φ 9.6mm sintered-carbide die, with powder compressing machine pressurization 3MPa and keeps
180s, obtains the high 10mm of diameter of phi 9.6mm prefabricated block；
(2) graphite furnace is high 16.6mm external diameters Φ 14mm internal diameters Φ 12mm tubulose bodies of heater, two ends Φ 12mm thickness 3.3mm nitrogen
Change in the sealing of boron piece, graphite furnace and be set with boron nitride crucible, the high 10mm external diameters Φ 12mm internal diameters Φ 9.6mm of crucible, two ends diameter
Φ 9.6mm thickness 1.2mm boron nitride piece is sealed, while graphite furnace two ends parcel and conduction are that diameter of phi 14 is thick with graphite flake specification
1.6mm.By graphite furnace, boron nitride crucible, boron nitride piece, the pyrophillite square and conducting steel ring used together with cubic hinge press
It is standby to dry 3 hours in 180 DEG C of drying baker to be put in temperature；
(3) prefabricated block for preparing step (1) is put into step (2) in the boron nitride crucible of prebake, by boron nitride
Crucible, tubular graphene stove, graphite flake, boron nitride piece are placed in cubic hinge press after assembling in order, and pressure is set to 4GPa, peak
It is worth temperature control at 1100 DEG C, is incubated 30min；Temperature is incubated 2h when being down to 800 DEG C, then direct turn-off current stops heating；
(4) take out block and carry out surface cleaning, obtain and contain Al4Cu9The block of single crystal grain.
As shown in figure 3, to Al4Cu9The block of single crystal grain carries out SEM tests, finds and the sample identical group of embodiment 1
Knit, it is known that also successfully prepare Al4Cu9Single crystal grain.
Embodiment 3
(1) atom ratio (Al is pressed:Cu=31:69) the high-purity Al powder of 0.55768g and 2.94231g Cu powder are weighed, by two
Is fitted into after kind of powder is well mixed in internal diameter Φ 9.6mm sintered-carbide die, with powder compressing machine pressurization 3MPa and keeps
180s, obtains the high 10mm of diameter of phi 9.6mm prefabricated block；
(2) graphite furnace is high 16.6mm external diameters Φ 14mm internal diameters Φ 12mm tubulose bodies of heater, two ends Φ 12mm thickness 3.3mm nitrogen
Change in the sealing of boron piece, graphite furnace and be set with boron nitride crucible, the high 10mm external diameters Φ 12mm internal diameters Φ 9.6mm of crucible, two ends diameter
Φ 9.6mm thickness 1.2mm boron nitride piece is sealed, while graphite furnace two ends parcel and conduction are that diameter of phi 14 is thick with graphite flake specification
1.6mm, by graphite furnace, boron nitride crucible, boron nitride piece, the pyrophillite square and conducting steel ring used together with cubic hinge press
It is standby to dry 3 hours in 180 DEG C of drying baker to be put in temperature.
(3) prefabricated block for preparing step (1) is put into step (2) in the boron nitride crucible of prebake, by boron nitride
Crucible, tubular graphene stove, graphite flake, boron nitride piece are placed in cubic hinge press after assembling in order, and pressure is set to 3GPa, peak
It is worth temperature control at 1150 DEG C, is incubated 30min；Temperature is incubated 1h when being down to 900 DEG C, then direct turn-off current stops heating；
(4) take out block and carry out surface cleaning, obtain and contain Al4Cu9The block of single crystal grain.
As shown in figure 4, to Al4Cu9The block of single crystal grain carries out SEM tests, and tissue topography is identical with example 1 and example 2, by
This understands that example 3 has also prepared Al4Cu9Single crystal grain.
Claims (1)
1. a kind of Al4Cu9The preparation method of single crystal grain, it is characterised in that：
(1)Al4Cu9The atom ratio of the chemical composition of monocrystalline is：Al 28-31%, Cu 69-72%；
(2) high-purity Al powder and Cu powder are well mixed, apply 2-3MPa pressure with powder compressing machine and keep about 180s, be made
Prefabricated block；
(3) by graphite furnace tubulose body of heater two ends boron nitride piece covering, boron nitride crucible, crucible two ends nitrogen are set with graphite furnace
Change in boron piece and seal, while graphite furnace two ends graphite flake is as parcel and conduction, then by above described tubular graphite body of heater, boron nitride
The pyrophillite square and conducting steel ring that crucible, boron nitride piece, pyrophillite piece and graphite flake are used together with cubic hinge press are put
It is standby for drying in 180 DEG C of drying baker 3 hours in temperature；
(4) prefabricated block prepared in step (2) is put into the boron nitride crucible of step (3) prebake, by boron nitride crucible,
Tubular graphene stove, graphite flake, boron nitride piece are placed in cubic hinge press after assembling in order, and pressure is set to 3-5GPa, peak value
Temperature control is incubated 30min at 1100 DEG C -1150 DEG C；Temperature is incubated 1-2h when being down to 800 DEG C -950 DEG C.
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| CN201710622158.6A CN107185459B (en) | 2017-07-27 | 2017-07-27 | Preparation method of Al4Cu9 single crystal particles |
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| CN201710622158.6A CN107185459B (en) | 2017-07-27 | 2017-07-27 | Preparation method of Al4Cu9 single crystal particles |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108866632A (en) * | 2018-06-13 | 2018-11-23 | 燕山大学 | It is a kind of to prepare Al2The method of Cu two-phase single crystal grain |
| CN108930064A (en) * | 2018-06-13 | 2018-12-04 | 燕山大学 | A kind of Al45Cr7The preparation method of single crystal grain |
| CN108940125A (en) * | 2018-06-13 | 2018-12-07 | 燕山大学 | It is a kind of to prepare Al13Fe3The method of single crystal grain |
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| US20010048887A1 (en) * | 1997-11-25 | 2001-12-06 | Rustum Roy | Process for sintering powder metal components |
| CN105568023A (en) * | 2016-01-07 | 2016-05-11 | 燕山大学 | Preparation method for Al6Mn quasicrystal |
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2017
- 2017-07-27 CN CN201710622158.6A patent/CN107185459B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010048887A1 (en) * | 1997-11-25 | 2001-12-06 | Rustum Roy | Process for sintering powder metal components |
| CN105568023A (en) * | 2016-01-07 | 2016-05-11 | 燕山大学 | Preparation method for Al6Mn quasicrystal |
Non-Patent Citations (2)
| Title |
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| 周静: "《近代材料科学研究技术进展》", 31 December 2012, 武汉理工大学出版社 * |
| 蒋淑英等: "Al /Cu 系金属间化合物价电子结构计算与界面反应预测", 《材料热处理学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108866632A (en) * | 2018-06-13 | 2018-11-23 | 燕山大学 | It is a kind of to prepare Al2The method of Cu two-phase single crystal grain |
| CN108930064A (en) * | 2018-06-13 | 2018-12-04 | 燕山大学 | A kind of Al45Cr7The preparation method of single crystal grain |
| CN108940125A (en) * | 2018-06-13 | 2018-12-07 | 燕山大学 | It is a kind of to prepare Al13Fe3The method of single crystal grain |
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