METHOD OF HIGH-THROUGHPUT HOT ISOSTATIC PRESSING MICRO-SYNTHESIS FOR THE COMBINATORIAL MATERIALS AND SLEEVE MOULD THEREOF

Abstract

The invention relates to a method of high-throughput hot isostatic pressing micro-synthesis for the combinatorial materials and a sleeve mould thereof. The sleeve mould (2) comprises a honeycomb-array-sleeve (3) and an upper cover (4), wherein a plurality of single cells (6) are tightly arranged inside the honeycomb-array-sleeve (3), an exhaust tube (5) is arranged on the upper cover (4), after the single cells (6) are filled with powder materials, the upper cover (4) is sealed welding on the honeycomb-array-sleeve (3), and the honeycomb-array-sleeve (3) and the upper cover (4) are both integrally produced by additive manufacturing. According to the method and the sleeve mould, the powder metallurgy hot isostatic pressing process is utilized to prepare small-size bulk combinatorial materials with multiple discrete components rapidly at one time. This method has the characteristics of high sintering speed, high compaction density, good thermal diffusivity, short production cycle and low material consumption. This invention successfully overcomes drawbacks of current material preparation, such as unitary combination of components, huge material consumption and high cost.

Claims

1. A method of high-throughput hot isostatic pressing micro-synthesis for the combinatorial materials, wherein the method is a powder metallurgy high-throughput preparation method of multi-component materials at one time, specifically comprising the following steps: 1) powder preparation and sleeve manufacturing: weighing a series of basic material powder of a specified mass and to-be-added elements or component powder, and mixing uniformly according to a designed mixture ratio, to prepare mixture powder series with different combinations of components; integrally printing and forming a sleeve mould (2) by additive manufacturing manner; wherein the sleeve mould (2) comprises a honeycomb-array-sleeve (3) and an upper cover (4), a plurality of single cells (6) are tightly arranged inside the honeycomb-array-sleeve (3), and an exhaust tube (5) is arranged on the upper cover (4); 2) powder filling and degassing: uniformly and densely filling a mixture powder series with different combinations of components respectively into each single cell (6) of the honeycomb-array-sleeve (3); sealing and welding the upper cover (4) on the honeycomb-array-sleeve (3); and degassing through the exhaust tube (5) at a limiting temperature, and closing the exhaust tube (5) for leakage detection; 3) hot isostatic pressure processing: placing the sleeve mould (2) obtained in step 2) in a hot isostatic press apparatus (1), and performing densification molding and thermal diffusion according to a preset temperature, pressure and time and other process parameters; taking out the sleeve mould (2) and stripping off an outer sleeve, to obtain a bulk combinatorial materials with different components, and to be used in follow-up analysis and characterization.

2. The method of high-throughput hot isostatic pressing micro-synthesis for the combinatorial materials of claim 1, wherein in step 2), the exhaust tube (5) is adopted to vacuumize to 110.sup.5-110.sup.4Pa at 20-40 C., vacuum is maintained and heated up to 500-600 C., the exhaust tube (5) is adopted to continuously vacuumize for 4-6 hours, degassing is performed, air and moisture in the sleeve mould (2) are removed, and then the exhaust tube (5) is closed.

3. The method of high-throughput hot isostatic pressing micro-synthesis for the combinatorial materials of claim 1, wherein in step 3), according to differences in prepared materials, hot isostatic pressing is performed for 5-10 hours at a temperature of 500-1400 C. and a pressure of 120-200 MPa.

4. The method of high-throughput hot isostatic pressing micro-synthesis for the combinatorial materials of claim 1, wherein a sample manufactured through the method has a size of 10-50 mm and a mass of 200-1000 g.

5. A sleeve mould use for the method of high-throughput hot isostatic pressing micro-synthesis for the combinatorial materials of claim 1, wherein the sleeve mould (2) comprises a honeycomb-array-sleeve (3) and an upper cover (4), a plurality of single cells (6) are tightly arranged inside the honeycomb-array-sleeve (3), an exhaust tube (5) is arranged on the upper cover (4), after the single cells (6) are filled with powder materials, the upper cover (4) is sealed welding on the honeycomb-array-sleeve (3), and the honeycomb-array-sleeve (3) and the upper cover (4) are both integrally produced by additive manufacturing manner.

6. The sleeve mould of claim 5, wherein a cross section of the single cell (6) is a regular hexagon.

7. The sleeve mould of claim 5, wherein the material of the honeycomb-array-sleeve (3) is a metal with a melting point being higher than that of the prepared powder material series with different combinations of components.

8. The sleeve mould of claim 5, wherein an inner wall of each single cell (6) of the honeycomb-array-sleeve (3) is sprayed with boron nitride high-temperature-resistant coating.

9. The sleeve mould of claim 5, wherein a wall thickness of the single cell (6) is less than 0.5 mm

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0031] FIG. 1 is a schematic diagram of a use state of a sleeve mould 2 in a hot isostatic press apparatus 1 in the present invention;

[0032] FIG. 2 is a structural schematic diagram of a sleeve mould 2 of the present invention;

[0033] FIG. 3 is a three-dimensional structural schematic diagram of a honeycomb-array-sleeve 3 in the present invention.

[0034] reference numerals in the figures:

TABLE-US-00001 1 hot isostatic press apparatus 2 sleeve mould 3 honeycomb-array-sleeve 4 upper cover 5 exhaust tube 6 single honeycomb cell

DETAILED DESCRIPTION OF THE EMBODIMENTS

[0035] The present invention will be further described below in combination with accompanying drawings and embodiments.

[0036] The method of high-throughput hot isostatic pressing micro-synthesis for the combinatorial materials in the present invention includes the following steps:

[0037] step 1: weighing a series of basic material powder of a specified mass and to-be-added element or component powder, and mixing uniformly according to a certain designed mixture ratio, to prepare mixture powder series with different combinations of components; and integrally producing a sleeve mould 2 by additive manufacturing;

[0038] step 2: uniformly and densely filling a mixture powder series with different combinations of components respectively into each single cell 6 of a honeycomb-array-sleeve 3 of a sleeve mould 2;

[0039] step 3: sealing and welding an upper cover 4 provided with an exhaust tube 5 on the honeycomb-array-sleeve 3;

[0040] step 4: degassing the sleeve mould 2 through the exhaust tube 5 at a limiting temperature, and closing the exhaust tube 5 for leakage detection;

[0041] step 5: placing a sleeve mould 2 in a hot isostatic press apparatus 1, as shown in FIG. 1, and performing densification molding and thermal diffusion according to a preset temperature, pressure and time and other process parameters; and

[0042] step 6: taking out the sleeve mould 2 and stripping off an outer sleeve, to obtain a bulk combinatorial materials with different components, and to be used in follow-up analysis and characterization.

[0043] Preferably, the mixture powder series with different combinations of components are mixed metal powder of multiple components.

[0044] As shown in FIG. 2 and FIG. 3, the sleeve mould 2 includes the honeycomb-array-sleeve 3 and the upper cover 4, a plurality of single cells 6 are tightly arranged inside the honeycomb-array-sleeve 3, to isolate metal powders of different components; and a cross section of the single cell 6 is a regular hexagon. An exhaust tube 5 is arranged on the upper cover 4. The honeycomb-array-sleeve 3 and the upper cover 4 are both integrally produced by additive manufacturing.

[0045] Preferably, the material of the honeycomb-array-sleeve 3 is a metal with a melting point being higher than that of the prepared mixture powder series with different combinations of components.

[0046] Preferably, an inner wall of each single honeycomb cell 6 of the honeycomb-array-sleeve 3 is sprayed with boron nitride high-temperature-resistant coating, to prevent diffusion with powder materials with different combinations of components.

[0047] Preferably, a wall thickness of the single cell 6 is less than 0.5 mm, to facilitate temperature conduction and equilibrium of the honeycomb-array-sleeve 3 and compaction densification of the honeycomb-array-sleeve 3.

Embodiment

[0048] In the present embodiment, a hot isostatic pressing high-throughput micro-synthesis method for bulk materials with multiple combinations of components is described with a ternary alloy of iron, cobalt and nickel as an example. Specific steps of the present embodiment are as follows:

[0049] step 1: respectively weighing iron, cobalt and nickel powder with 19 different component ratios, wherein a total mass of each part is 100 g, a mass ratio of iron, cobalt and nickel powder is specified in the following table, and the iron, cobalt and nickel powder is respectively mechanically mixed uniformly, to prepare a mixture powder series with 19 combinations of components;

TABLE-US-00002 Mass ratio of 19 components of iron, cobalt and nickel powder Fe Co Ni Fe:Co:Ni Fe:Co 3Fe:Co 6Fe:Co Fe:6Co Fe:3Co Co:Ni 3Co:Ni 6Co:Ni Co:6Ni Co:3Ni Fe:Ni 3Fe:Ni 6Fe:Ni Fe:6Ni Fe:3Ni

[0050] step 2: uniformly and densely filling the powder basic metal series with 19 combinations of components into each single cell 6 of the honeycomb-array-sleeve 3;

[0051] step 3: sealing and welding the upper cover 4 and the exhaust tube 5 on the honeycomb-array-sleeve 3, to prepare a sleeve mould 2;

[0052] step 4: vacuumizing through the exhaust tube 5 to 110.sup.4Pa at 25 C., maintaining vacuum and heating up to 500 C., continuously vacuumizing for 4 hours through the exhaust tube 5, degassing, removing air and moisture in the sleeve mould 2, and then closing the exhaust tube 5, and detecting leakage of the sleeve mould 2, wherein the sleeve mould 2 is sealed well; P step 5: placing the sleeve mould 2 in a hot isostatic press apparatus 1, and performing hot isostatic pressing diffusion for 10 hours at a target temperature of 1050 C. and a pressure of 120 MPa for moulding; and

[0053] step 6: cooling to room temperature, taking out the sleeve mould 2 and stripping off an outer sleeve, to obtain a bulk combinatorial material, and to be used in follow-up analysis and characterization.