CN107185459B

CN107185459B - Preparation method of Al4Cu9 single crystal particles

Info

Publication number: CN107185459B
Application number: CN201710622158.6A
Authority: CN
Inventors: 范长增; 陈智银
Original assignee: Yanshan University
Current assignee: Yanshan University
Priority date: 2017-07-27
Filing date: 2017-07-27
Publication date: 2020-03-31
Anticipated expiration: 2037-07-27
Also published as: CN107185459A

Abstract

Al (aluminum)₄Cu₉Method for producing single crystal grains, Al₄Cu₉The single crystal comprises the following chemical components in atomic ratio: 28-31% of Al and 69-72% of Cu; the preparation method mainly comprises the steps of uniformly mixing high-purity Al powder and Cu powder, putting the mixture into a hard alloy die, and applying 3MPa pressure and keeping the pressure for about 180s by using a powder tablet press to obtain a prefabricated block; putting the prepared prefabricated block into a boron nitride crucible, sequentially assembling the boron nitride crucible, a tubular graphite furnace, a graphite sheet and a boron nitride sheet, and then putting the assembled boron nitride crucible, the tubular graphite furnace, the graphite sheet and the boron nitride sheet into a cubic press, wherein the pressure is set between 3 and 5GPa, the peak temperature is controlled between 1100 and 1150 ℃, and the heat preservation is carried out for 30 min; and preserving the heat for 1-2h when the temperature is reduced to 800-950 ℃. The invention has the advantages of simple process, practical and feasible operation method, common experimental equipment and the like, and the generated single crystal has better quality.

Description

Preparation method of Al4Cu9 single crystal particles

Technical Field

The invention belongs to the technical field of metal materials, and particularly relates to a preparation method of single crystal particles.

Background

The modern society with the technology being different day by day is not capable of finding and synthesizing many materials. Al-Cu alloy is a typical alloy system with many alloy phases such as Al₂Cu、AlCu₃And Al₄Cu₉And the like, has excellent performance and wide application. The application of a material is determined by its properties, while the structure determines the properties, and when we need to know a material, not only performance test is needed, but also the structure should be started. While measuring the structure of a material, a single crystal would provide great help. The existing methods for preparing single crystals are many, but all the methods are complex and tedious.

Disclosure of Invention

In order to simply and conveniently prepare single crystals, the invention aims to provide Al with simple process and good quality of generated single crystal particles₄Cu₉A method for preparing single crystal particles. The invention mainly prepares Al by a high-pressure method for pure utilization₄Cu₉Al is prepared by high pressure method after single crystal is evenly mixed₄Cu₉And (3) single crystal.

The technical scheme of the invention is as follows:

(1)Al₄Cu₉the single crystal comprises the following chemical components in atomic ratio: 28-31% of Al and 69-72% of Cu;

(2) uniformly mixing high-purity Al powder and Cu powder, and applying 2-3MPa pressure by using a powder tablet press and keeping the pressure for about 180s to prepare a prefabricated block;

(3) sealing two ends of a tubular furnace body of a graphite furnace with boron nitride sheets externally, sleeving a boron nitride crucible in the graphite furnace, sealing two ends of the crucible with the boron nitride sheets internally, wrapping and conducting the two ends of the graphite furnace with graphite sheets, and then placing the tubular graphite furnace body, the boron nitride crucible, the boron nitride sheets, the pyrophyllite sheets and the graphite sheets together with pyrophyllite blocks and a conducting steel ring used by a cubic press into a drying box at the temperature of 180 ℃ for drying for 3 hours for later use;

(4) putting the prefabricated block prepared in the step (2) into the boron nitride crucible pre-dried in the step (3), sequentially assembling the boron nitride crucible, the tubular graphite furnace, the graphite sheet and the boron nitride sheet, and then putting the assembled boron nitride crucible, the tubular graphite furnace, the graphite sheet and the boron nitride sheet into a cubic press, wherein the pressure is set to be 3-5GPa, the peak temperature is controlled to be 1100-1150 ℃, and the heat preservation is carried out for 30 min; and preserving the heat for 1-2h when the temperature is reduced to 800-950 ℃.

Compared with the prior art, the invention has the following advantages:

the method has the advantages of simple process, feasible operation method, no need of complex equipment, no need of excessive treatment of raw materials, direct use of the raw materials to synthesize the single crystal phase, good quality of generated single crystal particles, and capability of meeting the preparation of various single crystal phase components.

Drawings

FIG. 1 shows Al prepared in example 1 of the present invention₄Cu₉EDS plot of single crystal particles.

FIG. 2 shows Al prepared in example 1 of the present invention₄Cu₉SEM image of single crystal particles.

FIG. 3 shows Al prepared in example 2 of the present invention₄Cu₉SEM image of single crystal particles.

FIG. 4 shows Al prepared in example 3 of the present invention₄Cu₉SEM image of single crystal particles.

Detailed Description

Example 1

(1) 0.56422g of high-purity Al powder and 3.00850g of Cu powder are weighed according to the atomic ratio (Al: Cu is 30:70), the two kinds of powder are uniformly mixed and then are filled into a hard alloy die with the inner diameter phi of 9.6mm, a powder tablet machine is used for pressurizing for 3MPa and keeping for 180s, and a prefabricated block with the diameter phi of 9.6mm and the height of 10mm is obtained;

(2) the graphite furnace is a tubular furnace body with the height of 16.6mm, the outer diameter phi 14mm and the inner diameter phi 12mm, two ends of the tubular furnace body are sealed by boron nitride sheets with the thickness of phi 12mm and the thickness of 3.3mm, a boron nitride crucible is sleeved in the graphite furnace, the crucible is 10mm, the outer diameter phi 12mm and the inner diameter phi 9.6mm, two ends of the graphite furnace body are sealed by boron nitride sheets with the diameter phi 9.6mm and the thickness of 1.2mm, meanwhile, the graphite furnace is wrapped at two ends and is used for conducting, the specification of the graphite sheets is that the diameter phi 14 is 1.6mm, and the graphite furnace, the boron nitride crucible, the boron nitride sheets, pyrophyllite blocks used together with a cubic press and a conductive;

(3) putting the prefabricated block prepared in the step (1) into the boron nitride crucible pre-dried in the step (2), sequentially assembling the boron nitride crucible, the tubular graphite furnace, the graphite sheet and the boron nitride sheet, and then putting the assembled boron nitride crucible, the tubular graphite furnace, the graphite sheet and the boron nitride sheet into a cubic press, wherein the pressure is set to be 5GPa, the peak temperature is controlled to be 1150 ℃, and the heat preservation is carried out for 30 min; and keeping the temperature for 2 hours when the temperature is reduced to 950 ℃. Then directly cutting off the current to stop heating;

(4) taking out the block and cleaning the surface to obtain Al-containing material₄Cu₉A mass of single crystal particles.

For Al₄Cu₉EDS test was performed on the single crystal grain bulk to determine the composition, and as shown in FIG. 1, Al was synthesized from the Spot 2 composition_30.89Cu_69.11Atomic ratio of Al₄Cu₉Accordingly, Al can be judged₄Cu₉The single crystal phase preparation is successful.

Then, a single crystal diffraction test was carried out to confirm Al₄Cu₉Single crystal structure as shown in fig. 2.

Example 2

(1) 0.50738g of high-purity Al powder and 3.09259g of Cu powder are weighed according to the atomic ratio (Al: Cu is 28:72), the two kinds of powder are uniformly mixed and then are filled into a hard alloy die with the inner diameter phi of 9.6mm, a powder tablet machine is used for pressurizing for 3MPa and keeping for 180s, and a prefabricated block with the diameter phi of 9.6mm and the height of 10mm is obtained;

(2) the graphite furnace is a tubular furnace body with the height of 16.6mm, the outer diameter phi 14mm and the inner diameter phi 12mm, two ends of the tubular furnace body are sealed by boron nitride sheets with the thickness of phi 12mm and the thickness of 3.3mm, the graphite furnace is sleeved with a boron nitride crucible, the crucible is 10mm, the outer diameter phi 12mm and the inner diameter phi 9.6mm, two ends of the tubular furnace body are sealed by boron nitride sheets with the diameter phi 9.6mm and the thickness of 1.2mm, and meanwhile, the graphite furnace is wrapped at two ends and is conductive by graphite sheets with the diameter phi 14 and the thickness. Placing a graphite furnace, a boron nitride crucible, a boron nitride sheet, a pyrophyllite square block used by a cubic press and a conductive steel ring in a drying box at the temperature of 180 ℃ for drying for 3 hours for later use;

(3) putting the prefabricated block prepared in the step (1) into the boron nitride crucible pre-dried in the step (2), sequentially assembling the boron nitride crucible, the tubular graphite furnace, the graphite sheet and the boron nitride sheet, and then putting the assembled boron nitride crucible, the tubular graphite furnace, the graphite sheet and the boron nitride sheet into a cubic press, wherein the pressure is set to be 4GPa, the peak temperature is controlled at 1100 ℃, and the heat preservation is carried out for 30 min; keeping the temperature for 2 hours when the temperature is reduced to 800 ℃, and then directly cutting off the current to stop heating;

As shown in FIG. 3, for Al₄Cu₉SEM test of a bulk of single crystal grains revealed the same structure as that of the sample of example 1, and it was found that Al was also successfully produced₄Cu₉Single crystal particles.

Example 3

(1) 0.55768g of high-purity Al powder and 2.94231g of Cu powder are weighed according to the atomic ratio (Al: Cu is 31:69), the two kinds of powder are uniformly mixed and then are filled into a hard alloy die with the inner diameter phi of 9.6mm, a powder tablet machine is used for pressurizing for 3MPa and keeping for 180s, and a prefabricated block with the diameter phi of 9.6mm and the height of 10mm is obtained;

(2) the graphite furnace is a tubular furnace body with the height of 16.6mm, the outer diameter phi 14mm and the inner diameter phi 12mm, two ends of the tubular furnace body are sealed by boron nitride sheets with the thickness of phi 12mm and the thickness of 3.3mm, a boron nitride crucible is sleeved in the graphite furnace, the crucible is 10mm, the outer diameter phi 12mm and the inner diameter phi 9.6mm, two ends of the graphite furnace body are sealed by boron nitride sheets with the diameter phi 9.6mm and the thickness of 1.2mm, meanwhile, the graphite furnace is wrapped at two ends of the graphite furnace and is used for conducting, the specification of the graphite sheets is that the diameter phi 14 is 1.6mm, and the graphite furnace, the boron nitride crucible, the boron nitride sheets, pyrophyllite blocks used together with a cubic.

(3) Putting the prefabricated block prepared in the step (1) into the boron nitride crucible pre-dried in the step (2), sequentially assembling the boron nitride crucible, the tubular graphite furnace, the graphite sheet and the boron nitride sheet, and then putting the assembled boron nitride crucible, the tubular graphite furnace, the graphite sheet and the boron nitride sheet into a cubic press, wherein the pressure is set to be 3GPa, the peak temperature is controlled to be 1150 ℃, and the heat preservation is carried out for 30 min; keeping the temperature for 1h when the temperature is reduced to 900 ℃, and then directly cutting off the current to stop heating;

As shown in FIG. 4, for Al₄Cu₉SEM examination of a bulk of single crystal grains revealed that the morphology was the same as in examples 1 and 2, and thus example 3 also produced Al₄Cu₉Single crystal particles.

Claims

1. Al (aluminum)₄Cu₉A method for producing single crystal particles, characterized by:

(2) uniformly mixing high-purity Al powder and Cu powder, applying 2-3MPa pressure by using a powder tablet press and keeping the pressure for 180s to prepare a prefabricated block;

(3) the graphite furnace is a tubular furnace body, two ends of the tubular graphite furnace are externally sealed by boron nitride sheets, a boron nitride crucible is sleeved in the graphite furnace, two ends of the crucible are internally sealed by the boron nitride sheets, meanwhile, graphite sheets for wrapping and conducting are arranged at two ends of the graphite furnace, and then the tubular graphite furnace, the boron nitride crucible, the boron nitride sheets and the graphite sheets, as well as pyrophyllite blocks and a conducting steel ring used by a cubic press are placed in a drying box at the temperature of 180 ℃ for drying for 3 hours for later use;