CN108866631B - Preparation of Al3Method for preparing V tetragonal single crystal particles - Google Patents

Preparation of Al3Method for preparing V tetragonal single crystal particles Download PDF

Info

Publication number
CN108866631B
CN108866631B CN201810609629.4A CN201810609629A CN108866631B CN 108866631 B CN108866631 B CN 108866631B CN 201810609629 A CN201810609629 A CN 201810609629A CN 108866631 B CN108866631 B CN 108866631B
Authority
CN
China
Prior art keywords
boron nitride
sheet
tube
block
single crystal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201810609629.4A
Other languages
Chinese (zh)
Other versions
CN108866631A (en
Inventor
范长增
王赛
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yanshan University
Original Assignee
Yanshan University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yanshan University filed Critical Yanshan University
Priority to CN201810609629.4A priority Critical patent/CN108866631B/en
Publication of CN108866631A publication Critical patent/CN108866631A/en
Application granted granted Critical
Publication of CN108866631B publication Critical patent/CN108866631B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • C30B29/52—Alloys
    • 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
    • C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions

Abstract

Preparation of Al3Method for producing V tetragonal single crystal grains, said Al3The chemical components of the V tetragonal single crystal particle raw material are in atomic ratio: 84-86% of Al and 14-16% of V, and the preparation method mainly comprises the steps of grinding and uniformly mixing high-purity Al powder and V powder, then putting the mixture into a hard alloy die, and pressurizing for 200 and 300 seconds in a hydraulic tablet press under the pressure of 3-5MPa to prepare a prepared block body; putting the prepared block into a boron nitride crucible, assembling the prepared block with a pre-dried tubular zirconia, a graphite furnace body, a boron nitride tube, a zirconia sheet, a boron nitride sheet, pyrophyllite and a graphite sheet, putting the assembled blocks and the graphite sheet into a cubic press, setting the pressure to be 3-5GPa, heating to 1340 and 1450 ℃, and preserving the heat for 30-60 min; and keeping the temperature for 1-2h when the temperature is reduced to 1100-1200 ℃. The method has the advantages of simple process, low energy consumption, high efficiency, strong operability and more conventional experimental equipment, and can rapidly and accurately analyze the single crystal structure by matching with the single crystal X-ray diffractometer and related software, thereby providing support for structural analysis and performance optimization from the crystal structure.

Description

Preparation of Al3Method for preparing V tetragonal single crystal particles
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to Al3A preparation method of V tetragonal single crystal particles.
Background
Intermetallic compounds have different crystal structures and atomic structures from the original metals, can form new ordered superlattice structures, and have many distinctive properties and are widely used, such as high temperature applications, electromagnetic applications, and the like. The Al-V alloy has higher thermal stability and corrosion resistance, and meets the highest requirements of the aerospace industry on quality and reliability. In addition, Al-V is used as intermediate alloy and added with elements such as Ni, etc. to further expand the application range. Stabilizing Al in the system3V phase having a tetragonal DO22The structure of the alloy has important significance in developing heat-resistant Al alloy by researching the phase structure of the alloy. Some researchers have conducted calculation simulation and the like on Al3V-phase DO22Structure sum L12The thermodynamics, energy band, electron density and other aspects of the structure are studied to obtain some interesting results, and a few researchers use Al3The V phase is a reinforcing phase to prepare the Al-based composite material so as to improve the related performance. In the previous research, researchers prepared Al by using diffusion experiments and a method of mixing corresponding powder raw materials by a high-energy ball mill and performing arc melting in an argon atmosphere3V phase, even to obtain Al3The Al-based composite material with the V phase as the reinforcing phase adopts ball-milled Al/V2O5Added to molten aluminum, but few researchers have resolved its structure except the first discoverer. Preparation of Al3The method for preparing V has long preparation period, complicated step operation and certain danger, and needs inert gas protection in order to prevent the oxidation preparation process.
Disclosure of Invention
The invention aims to provide the Al preparation method which is simple and convenient to operate, strong in operability, fixed in experimental equipment, low in time consumption and high in preparation efficiency3V tetragonal single crystal grain. The invention mainly utilizes a high-pressure method to fully and uniformly mix pure Al powder and V powder, then prepresses and prepares a sample, directly applies pressure on the uniformly mixed and heated and melted mixed raw materials, and starts a cubic apparatus press according to set temperature, pressure and reaction duration to directly prepare Al3V tetragonal single crystal particles.
The preparation method of the invention comprises the following steps:
(1) preparation of Al3The chemical component atomic ratio of the V single crystal particle raw material is as follows: 84-86% of Al and 14-16% of V; the Al and V are high-purity metal powder.
(2) Fully grinding and uniformly mixing high-purity Al powder and V powder, then loading the mixture into a hard alloy die, and pressurizing for 200 and 300 seconds in a hydraulic tablet press under the pressure of 3-5MPa to obtain a prepared block;
(3) sealing two ends of the whole tubular furnace body by graphite sheets, wherein the tubular furnace body is of a nested structure, the outermost layer is a zirconium oxide tube, sequentially sleeving a boron nitride tube, a graphite tube and a boron nitride crucible, sequentially sealing two ends of the prepared block body prepared in the step (2) by using the boron nitride sheets, the zirconium oxide sheets and the boron nitride sheets from inside to outside, and then placing the tubular zirconium oxide tube, the graphite furnace body, the boron nitride crucible, the boron nitride sheets, the zirconium oxide sheets and the graphite sheets, as well as pyrophyllite squares and a conductive steel bowl used by a cubic press into a drying box with the temperature of 150-.
(4) Loading the prepared block prepared in the step (2) into a boron nitride crucible, assembling the dried graphite combination furnace according to the step (3), loading the graphite combination furnace into a pyrophyllite block, then placing the pyrophyllite block into a pressure cavity of a cubic press, controlling the pressure to be 3-5GPa, heating1340 and 1450 ℃, and preserving the temperature for 30-60 min; when the temperature is reduced to 1100-1200 ℃, the temperature is kept for 2-4h, and the stable tetragonal phase Al is directly obtained after being taken out3V block.
Compared with the prior art, the invention has the following advantages:
1. the method has the advantages of simple process operation, low energy consumption, high efficiency, strong operability and more conventional experimental equipment.
2. The mixed raw materials can be directly used for synthesizing the block containing the stable-phase single crystal by reducing the pretreatment of the raw materials, and the method is an efficient one-step synthesis method.
3. The single crystal structure can be rapidly and accurately analyzed by matching with a single crystal X-ray diffractometer and related software, and support is provided for further analyzing and optimizing the performance of related materials from the crystal structure.
Drawings
FIG. 1 shows Al obtained in example 1 of the present invention3V single crystal particle reciprocal space lattice diagram.
FIG. 2 shows Al analyzed in detail in example 1 of the present invention3V single crystal structure diagram.
FIG. 3 shows Al obtained in example 2 of the present invention3Morphology of V single crystal grains and Al3V crystal EDS spectrum (Area 1).
FIG. 4 shows Al obtained in example 3 of the present invention3SEM image and EDS spectrum of V single crystal particle (Area 1).
Detailed Description
Example 1
(1) Weighing high-purity Al powder and V powder raw materials according to the atomic ratio, wherein the weight of the raw materials is 0.3272g and 0.1176g (according to Al)84V16Weighing), placing the powder into a mortar, fully grinding and uniformly mixing the powder, filling the powder into a hard alloy die with the inner diameter of phi 5mm, and pressurizing the die for 300s in a hydraulic tablet press under 3Mpa to obtain a simple mechanical pressing high-pressure preparation block with the diameter of phi 5mm and the height of 8 mm.
(2) The outer diameter of the zirconia tube is phi 14mm, the inner diameter phi 10mm, the outer diameter phi 10mm, the inner diameter phi 8mm, the outer diameter phi 8mm, the inner diameter phi 6mm and the outer diameter phi 6mm, the inner diameter phi 5mm, all the four tubular furnace heights are 15mm from inside to outside, and the two ends are sealed by graphite sheets with the thickness of phi 14mm and 2mm after combination; the tubular furnace is of a nested structure, the outermost layer is a zirconia tube, and a boron nitride tube, a graphite tube and a boron nitride crucible are sequentially sleeved on the zirconia tube; after the prepared block is filled, two ends of the prepared block are sequentially sealed by a boron nitride sheet with the diameter phi of 5mm and the thickness of 1mm, a zirconium oxide sheet with the diameter phi of 5mm and the thickness of 2mm and a boron nitride sheet with the diameter phi of 5mm and the thickness of 1 mm; and placing conductive steel rings at two ends of the assembling furnace, and placing the prepared materials, pyrophyllite blocks used by a cubic press and the steel rings in a drying box with the temperature of 150 ℃ for drying for more than 4 hours for later use.
(3) Putting the prepared block body prepared in the step (1) into an assembly furnace, assembling the tubular zirconia, the graphite furnace body, the boron nitride sheet, the zirconia sheet, the pyrophyllite and the graphite sheet which are pre-dried in the step (2), and placing the assembly furnace body, the boron nitride sheet, the zirconia sheet, the pyrophyllite and the graphite sheet into a cubic press, wherein the set pressure is 5GPa isostatic pressure; heating to 1380 deg.C, and keeping the temperature for 30 min; and (5) keeping the temperature for 2 hours when the temperature is reduced to 1130 ℃.
(4) Directly cutting off current to stop heating after heat preservation, taking out the block, carefully stripping residual BN outside the block, cleaning the surface to obtain the product containing Al3V monocrystalline block.
As shown in fig. 1, the reciprocal space lattice obtained by diffraction of the sample single crystal is relatively complete. (the observation direction is shown as the coordinates in the figure, and a small number of irregular points are removed for visual observation)
As shown in FIG. 2, for utilizing Al3The crystal structure analyzed by the bulk diffraction data of V gives crystal information in detail.
Example 2
(1) Weighing high-purity Al powder and V powder raw materials according to the atomic ratio, wherein the weight of the raw materials is 0.3381g and 0.1065g (according to Al)6Weighing V atom ratio of 14.3%), putting the powder into a mortar, fully grinding and uniformly mixing, putting into a hard alloy die with the inner diameter of phi 5mm, pressurizing in a hydraulic tablet press for 250s under 4Mpa to obtain a simple mechanical pressing high-pressure prepared block with the diameter of phi 5mm and the height of 8 mm.
(2) The outer diameter of the zirconia tube is phi 14mm, the inner diameter phi 10mm, the outer diameter phi 10mm, the inner diameter phi 8mm, the outer diameter phi 8mm, the inner diameter phi 6mm and the outer diameter phi 6mm, the inner diameter phi 5mm, all the four tubular furnace heights are 15mm from inside to outside, and the two ends are sealed by graphite sheets with the thickness of phi 14mm and 2mm after combination; the tubular furnace is of a nested structure, the outermost layer is a zirconia tube, and a boron nitride tube, a graphite tube and a boron nitride crucible are sequentially sleeved on the zirconia tube; after the prepared block is filled, two ends of the block are sequentially sealed by a boron nitride sheet with the diameter phi of 5mm and the thickness of 1mm, a zirconium oxide sheet with the diameter phi of 5mm and the thickness of 2mm and a boron nitride sheet with the diameter phi of 5mm and the thickness of 1 mm; and placing conductive steel rings at two ends of the assembling furnace, and placing the prepared materials, pyrophyllite blocks used by a cubic press and the steel rings in a drying box with the temperature of 150 ℃ for drying for more than 4 hours for later use.
(3) Putting the prepared block body prepared in the step (1) into an assembly furnace, assembling the tubular zirconia, the graphite furnace body, the boron nitride sheet, the zirconia sheet, the pyrophyllite and the graphite sheet which are pre-dried in the step (2), and placing the assembly furnace body, the boron nitride sheet, the zirconia sheet, the pyrophyllite and the graphite sheet into a cubic press, wherein the set pressure is 4GPa isostatic pressure; heating to 1340 deg.C, and keeping the temperature for 40 min; and (5) keeping the temperature for 4 hours when the temperature is reduced to 1100 ℃.
(4) Directly cutting off current to stop heating after heat preservation, taking out the block, carefully stripping residual BN outside the block, cleaning the surface to obtain the product containing Al3V monocrystalline block.
As shown in FIG. 3, the influence of the subtraction error corresponds to the element ratio, and it is confirmed that the observed crystal grains are Al3V particles.
Example 3
(1) Weighing high-purity Al powder and V powder raw materials according to the atomic ratio, wherein the weight of the raw materials is 0.3274g and 0.1166g (according to Al)84V16Weighing), placing the powder into a mortar, fully grinding and uniformly mixing the powder, filling the powder into a hard alloy die with the inner diameter of phi 5mm, and pressurizing the die for 200s under the pressure of 5MPa in a hydraulic tablet press to obtain a simple mechanical pressing high-pressure preparation block with the diameter of phi 5mm and the height of 8 mm.
(2) The outer diameter of the zirconia tube is phi 14mm, the inner diameter phi 10mm, the outer diameter phi 10mm, the inner diameter phi 8mm, the outer diameter phi 8mm, the inner diameter phi 6mm and the outer diameter phi 6mm, the inner diameter phi 5mm, all the four tubular furnace heights are 15mm from inside to outside, and the two ends are sealed by graphite sheets with the thickness of phi 14mm and 2mm after combination; the tubular furnace is of a nested structure, the outermost layer is a zirconia tube, and a boron nitride tube, a graphite tube and a boron nitride crucible are sequentially sleeved on the zirconia tube. After the prepared block is filled, two ends of the block are sequentially sealed by a boron nitride sheet with the diameter phi of 5mm and the thickness of 1mm, a zirconium oxide sheet with the diameter phi of 5mm and the thickness of 2mm and a boron nitride sheet with the diameter phi of 5mm and the thickness of 1 mm; and placing conductive steel rings at two ends of the assembling furnace, and placing the prepared materials, pyrophyllite blocks used by a cubic press and the steel rings in a drying box with the temperature of 200 ℃ for drying for more than 4 hours for later use.
(3) Putting the prepared block body prepared in the step (1) into an assembly furnace, assembling the tubular zirconia, the graphite furnace body, the boron nitride sheet, the zirconia sheet, the pyrophyllite and the graphite sheet which are pre-dried in the step (2), and placing the assembly furnace body, the boron nitride sheet, the zirconia sheet, the pyrophyllite and the graphite sheet into a cubic press, wherein the set pressure is 3GPa isostatic pressure; heating to 1450 deg.C, and maintaining the temperature for 60 min; and (5) keeping the temperature for 3 hours when the temperature is reduced to 1200 ℃.
(4) Directly cutting off current to stop heating after heat preservation, taking out the block, carefully stripping residual BN outside the block, cleaning the surface to obtain the product containing Al3V monocrystalline block.
As shown in FIG. 4, the influence of weak error is deducted from the spectrum, and the element proportion is in accordance with Al3V, it can be stated that Al is observed3A V single crystal phase.

Claims (1)

1. Preparation of Al3A method of V tetragonal single crystal grains, characterized by:
(1) preparation of Al3The chemical component atomic ratio of the raw materials of the V tetragonal single crystal particles is as follows: 84-86% of Al and 14-16% of V; the Al and the V are high-purity metal powder;
(2) fully grinding and uniformly mixing Al powder and V powder, then loading the mixture into a hard alloy die, and pressurizing for 200 and 300 seconds in a hydraulic tablet press under the pressure of 3-5MPa to obtain a prepared block;
(3) the whole tubular furnace body is of a nested structure, the outermost layer is a zirconium oxide tube, a boron nitride tube, a graphite tube and a boron nitride crucible are sequentially sleeved, and the zirconium oxide tube, the boron nitride tube, the graphite tube and the boron nitride crucible as well as the prepared block, the boron nitride sheet, the zirconium oxide sheet and the graphite sheet prepared in the step (2) and the pyrophyllite square block and the conductive steel bowl used by the cubic press are placed in a drying box with the temperature of 100 and 200 ℃ for drying for more than 4 hours for later use;
(4) putting the dried prepared block into a boron nitride crucible, sealing two ends of the prepared block by using a boron nitride sheet, a zirconium oxide sheet and a boron nitride sheet from inside to outside in sequence, then nesting the dried zirconium oxide tube, the boron nitride tube, a graphite tube and the boron nitride crucible to form a tubular furnace body, sealing two ends by using graphite sheets, then putting the tubular furnace body into a pyrophyllite block, placing the pyrophyllite block into a pressure cavity of a six-sided press, controlling the pressure to 3-5GPa, heating to 1340-1450 ℃, and preserving the heat for 30-60 min; when the temperature is reduced to 1100-1200 ℃, the temperature is kept for 2-4h, and the stable tetragonal phase Al is directly obtained after being taken out3V block.
CN201810609629.4A 2018-06-13 2018-06-13 Preparation of Al3Method for preparing V tetragonal single crystal particles Active CN108866631B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810609629.4A CN108866631B (en) 2018-06-13 2018-06-13 Preparation of Al3Method for preparing V tetragonal single crystal particles

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810609629.4A CN108866631B (en) 2018-06-13 2018-06-13 Preparation of Al3Method for preparing V tetragonal single crystal particles

Publications (2)

Publication Number Publication Date
CN108866631A CN108866631A (en) 2018-11-23
CN108866631B true CN108866631B (en) 2021-01-08

Family

ID=64338902

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810609629.4A Active CN108866631B (en) 2018-06-13 2018-06-13 Preparation of Al3Method for preparing V tetragonal single crystal particles

Country Status (1)

Country Link
CN (1) CN108866631B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112159914A (en) * 2020-09-18 2021-01-01 衢州学院 TiAl micron crystal prepared under high pressure and method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101851781A (en) * 2010-04-01 2010-10-06 新疆大学 Method for preparing AlN mono-crystal nanobelts and nano-branch structure
CN107338471A (en) * 2017-07-27 2017-11-10 燕山大学 A kind of preparation method of high pressure metastable phase Al21Pd8 single crystal grains

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101851781A (en) * 2010-04-01 2010-10-06 新疆大学 Method for preparing AlN mono-crystal nanobelts and nano-branch structure
CN107338471A (en) * 2017-07-27 2017-11-10 燕山大学 A kind of preparation method of high pressure metastable phase Al21Pd8 single crystal grains

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Al-V中间合金制备工艺研究;胡洋;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20130315(第03期);B023-135 *
Factors influencing the deformation mechanisms in the intermetallic compounds Al3Ti and Al3V;Robert Wheeler等;《Philosophical Magazine Letters》;20060913;第62卷(第3期);第143-151页 *

Also Published As

Publication number Publication date
CN108866631A (en) 2018-11-23

Similar Documents

Publication Publication Date Title
JPH05506205A (en) Polishing compact of cubic boron nitride and its manufacturing method
US11827959B2 (en) Metallic matrix composites synthesized with uniform in situ formed reinforcement
CN105732040A (en) Synthesis method for preparing Ti3AlC2 by microwave self-propagating method
CN110484796A (en) A kind of high entropy ceramic particle of transition metal carbide and preparation method thereof
CN108866631B (en) Preparation of Al3Method for preparing V tetragonal single crystal particles
Peillon et al. Effect of TiH2 in the preparation of MMC Ti based with TiC reinforcement
Chanadee et al. Synthesis of WSi2 and W2B intermetallic compound by in-situ self propagating high-temperature synthesis reaction
CN113149659A (en) Nitrogen-containing medium-entropy or high-entropy MAX phase material and preparation method and application thereof
Cai et al. Porous NbAl3/TiAl3 intermetallic composites with controllable porosity and pore morphology prepared by two-step thermal explosion
RU2354501C1 (en) Method of nickel aluminide or titanium aluminide-based powder materials production
CN107338471A (en) A kind of preparation method of high pressure metastable phase Al21Pd8 single crystal grains
NO171901B (en) PROCEDURE FOR THE MANUFACTURE OF ALUMINUM BORIDE, OR A MIXTURE OF SOLID ALUMINUM PARTICLES AND AN ILLUSTRATED MATERIAL
CN110029261A (en) A kind of preparation method of Micro-Nano Hardmetal cutter material
EP0574440A1 (en) Production of metal and metalloid nitrides
Miura et al. Effects of aluminum concentration and compact thickness on reaction synthesis of Ni3Al NiAl alloys
WO1999061671A1 (en) METHOD OF PREPARING AN Al-Ti-B GRAIN REFINER FOR ALUMINIUM-COMPRISING PRODUCTS, AND A METHOD OF CASTING ALUMINIUM PRODUCTS
Zakaryan et al. Preparation of fine-grained silicon from serpentine mineral by magnesiothermic reduction of silica in the presence of reaction products as diluents
EP1285897B1 (en) Method of producing aluminum nitride matrix composite
Chanadee et al. Mechanoactivated SHS of Si–SiC Powders from Natural Sand: Influence of Milling Time
Roy et al. Self-propagating high-temperature synthesis of titanium borides
CN108866632B (en) Preparation of Al2Method for Cu biphase single crystal particles
CN105603227A (en) Preparation method of Al-Co-Ni quasicrystal
RU2161548C2 (en) Method for making powders of refractory compounds
RU2561952C1 (en) Production of monophase intermetallide alloy based on aluminium-titanium system
Ma et al. Effect of gas atmospheres and SiO2 content on preparation and properties of SiO2–Si3N4 composite ceramics via nitridation of diamond-wire saw silicon waste powder

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant