Metal lead-toughened lead oxide ceramic and preparation method thereof

Abstract

The invention relates to metal lead-toughened lead oxide ceramic and a preparation method thereof. The formula of the lead oxide ceramic comprises the following chemical components in percentage by mass: 10-25% of Pb and 75-90% of PbO, or 10-60% of Pb and 40-90% of Pb3O4, or 5-25% of Pb, 50-90% of PbO and 5-45% of Pb3O4. The preparation method comprises the following steps: mixing powders according to the formula, adding deionized water and uniformly grinding, then pre-pressing, grinding the obtained blank into a powder, then adding deionized water and uniformly grinding, then placing the mixture in a metal die and carrying out pressure maintaining and pressure relief treatment to obtain a metal ceramic pressed blank, and sintering the metal ceramic pressed blank to obtain the metal lead-toughened lead oxide ceramic product. The product has a higher bending strength on the basis of meeting a ceramic oxygen control function, and can bear a higher impact load to meet scouring running of liquid metal.

Description

technical field

[0001] The invention belongs to the technical field of metal ceramics, and in particular relates to a metal lead toughened lead oxide ceramic and a preparation method thereof. Background technique

[0002] Liquid metallic lead and liquid lead-bismuth alloys are coolant materials for lead-cooled fast reactors and lead-bismuth cooled fast reactors in the nuclear industry, and ADS spallation neutron target materials for accelerator-driven subcritical systems. Since lead and lead-bismuth alloys are highly corrosive to metal pipes, it is necessary to protect the pipe surface by controlling the oxygen content. Ordinary solid oxygen control technology uses lead oxide ceramics to wash and dissolve in liquid metal. However, due to the high brittleness and poor wear resistance of ceramic materials, they will be quickly damaged and fragmented under the scour of high-temperature liquid metal, which is difficult to meet the requirements of long-term stable operation of t...

Examples

Embodiment 1

[0027] (1) Preparation of ingredients:

[0028] PbO and Pb with a purity greater than 99% 3 o 4 Mix with Pb in a mass ratio of 8:1:1, add 5wt% deionized water, mix thoroughly, grind evenly, pre-press for 4 minutes under 30MPa pressure to obtain pre-pressed tablets, and then pre-pressed tablets Crush and grind, then add 4wt% deionized water, and grind evenly, so as to remove the transverse cracking phenomenon in the pressing molding process.

[0029] (2) Making compact:

[0030] Pour the processed powder into the mold, carry out pressure maintenance and pressure relief treatment, and press it into a green compact of the desired shape. The pressure holding and pressure relief treatment process is to increase the pressure to 8MPa at a speed of 0.1MPa / s, hold the pressure for 3.5min, and then release the pressure at a speed of 0.1MPa / s.

[0031] (3) Microwave sintering treatment:

[0032] The obtained compact is put into a microwave sintering container, and the microwave sint...

Embodiment 2

[0035] (1) Preparation of ingredients:

[0036] Pb and Pb with a purity greater than 99% 3 o 4 Mix according to the mass ratio of 1:1, add 2wt% deionized water, and grind evenly. Pre-compressing under 30MPa pressure for 4min for pre-compression treatment to obtain pre-compression tablets, then crush and grind the pre-compaction tablets, then add 4wt% deionized water, and grind evenly.

[0037] (2) Making compact:

[0038] The powder obtained in the above steps is introduced into the mold, pre-compressed at a pressure of 12MPa for 3 minutes, and then pressure-holding and pressure-releasing are performed, pressurized to a pressure of 8MPa at a speed of less than 0.2MPa / s, and the pressure is maintained for 5min, and then the pressure is less than 0.1MPa / s speed release pressure. Finally, compacts are pressed into the desired shape.

[0039] (3) Conventional sintering treatment:

[0040] The above-mentioned compacts were directly put into a conventional muffle furnace for ...

Embodiment 3

[0043] (1) Preparation of ingredients:

[0044] Mix Pb and PbO with a purity greater than 99% according to the mass ratio of 2:8, add 2wt% deionized water, and grind evenly. Pre-compressing under 30MPa pressure for 4min for pre-compression treatment to obtain pre-compression tablets, then crush and grind the pre-compaction tablets, then add 4wt% deionized water, and grind evenly.

[0045] (2) Making compact:

[0046] The powder obtained in the above steps is introduced into the mold, pre-compressed at a pressure of 15MPa for 5 minutes, and then subjected to pressure-holding and pressure-releasing treatment, pressurized to a pressure of 15MPa at a speed of less than 0.2MPa / s, maintained for 3min, and then pressurized at a rate of less than 0.1MPa / s speed release pressure. Finally, compacts are pressed into the desired shape.

[0047] (3) Conventional sintering treatment:

[0048] The above-mentioned compacts were directly put into a conventional muffle furnace for heating,...

technical field

[0001] The invention belongs to the technical field of metal ceramics, and in particular relates to a metal lead toughened lead oxide ceramic and a preparation method thereof. Background technique

[0002] Liquid metallic lead and liquid lead-bismuth alloys are coolant materials for lead-cooled fast reactors and lead-bismuth cooled fast reactors in the nuclear industry, and ADS spallation neutron target materials for accelerator-driven subcritical systems. Since lead and lead-bismuth alloys are highly corrosive to metal pipes, it is necessary to protect the pipe surface by controlling the oxygen content. Ordinary solid oxygen control technology uses lead oxide ceramics to wash and dissolve in liquid metal. However, due to the high brittleness and poor wear resistance of ceramic materials, they will be quickly damaged and fragmented under the scour of high-temperature liquid metal, which is difficult to meet the requirements of long-term stable operation of t...

Examples

Embodiment 1

[0027] (1) Preparation of ingredients:

[0028] PbO and Pb with a purity greater than 99% 3 o 4 Mix with Pb in a mass ratio of 8:1:1, add 5wt% deionized water, mix thoroughly, grind evenly, pre-press for 4 minutes under 30MPa pressure to obtain pre-pressed tablets, and then pre-pressed tablets Crush and grind, then add 4wt% deionized water, and grind evenly, so as to remove the transverse cracking phenomenon in the pressing molding process.

[0029] (2) Making compact:

[0030] Pour the processed powder into the mold, carry out pressure maintenance and pressure relief treatment, and press it into a green compact of the desired shape. The pressure holding and pressure relief treatment process is to increase the pressure to 8MPa at a speed of 0.1MPa / s, hold the pressure for 3.5min, and then release the pressure at a speed of 0.1MPa / s.

[0031] (3) Microwave sintering treatment:

[0032] The obtained compact is put into a microwave sintering container, and the microwave sint...

Embodiment 2

[0035] (1) Preparation of ingredients:

[0036] Pb and Pb with a purity greater than 99% 3 o 4 Mix according to the mass ratio of 1:1, add 2wt% deionized water, and grind evenly. Pre-compressing under 30MPa pressure for 4min for pre-compression treatment to obtain pre-compression tablets, then crush and grind the pre-compaction tablets, then add 4wt% deionized water, and grind evenly.

[0037] (2) Making compact:

[0038] The powder obtained in the above steps is introduced into the mold, pre-compressed at a pressure of 12MPa for 3 minutes, and then pressure-holding and pressure-releasing are performed, pressurized to a pressure of 8MPa at a speed of less than 0.2MPa / s, and the pressure is maintained for 5min, and then the pressure is less than 0.1MPa / s speed release pressure. Finally, compacts are pressed into the desired shape.

[0039] (3) Conventional sintering treatment:

[0040] The above-mentioned compacts were directly put into a conventional muffle furnace for ...

Embodiment 3

[0043] (1) Preparation of ingredients:

[0044] Mix Pb and PbO with a purity greater than 99% according to the mass ratio of 2:8, add 2wt% deionized water, and grind evenly. Pre-compressing under 30MPa pressure for 4min for pre-compression treatment to obtain pre-compression tablets, then crush and grind the pre-compaction tablets, then add 4wt% deionized water, and grind evenly.

[0045] (2) Making compact:

[0046] The powder obtained in the above steps is introduced into the mold, pre-compressed at a pressure of 15MPa for 5 minutes, and then subjected to pressure-holding and pressure-releasing treatment, pressurized to a pressure of 15MPa at a speed of less than 0.2MPa / s, maintained for 3min, and then pressurized at a rate of less than 0.1MPa / s speed release pressure. Finally, compacts are pressed into the desired shape.

[0047] (3) Conventional sintering treatment:

[0048] The above-mentioned compacts were directly put into a conventional muffle furnace for heating,...

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