Ceramic connecting piece as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of ceramic connection, and discloses a ceramic connecting piece and a preparation method and application thereof. The method comprises the following steps:dissolving Re2O3 in an inorganic acid to obtain a solution containing Re ions; Al2O3 is added into a solution containing Re ions to be subjected to ball milling and then is subjected to ball millingand mixing with SiC or Si3N4 nano ceramic powder, so that a connecting material is prepared; and the connecting material isplaced between two polished SiC or Si3N4 ceramics to form a sandwich structure; the sandwich structure is heated to 1000-1200 DEG C in a vacuum or protective atmosphere, the temperature is kept, the structure is heated to 1300-1600 DEG C to be calcined, and pressurizing is performed by 0.1-10 MPa to prepare the ceramic connecting piece. By means of the method, the SiC or Si3N4 ceramic can be connected under the low-temperature and low-pressure conditions, the joint is compact and free of defects and has good high-temperature resistance and corrosion resistance, and the ceramic connecting piece can be widely applied to the fields of space flight and aviation, war industry and nuclear energy.

Description

technical field

[0001] The invention belongs to the technical field of non-oxide ceramic materials, and more specifically relates to a ceramic connector and its preparation method and application. Background technique

[0002] Fine ceramics generally have excellent characteristics such as high temperature resistance, high hardness, wear resistance, corrosion resistance, and high temperature strength. They are key materials in the fields of aerospace, military and nuclear energy. Among them, SiC and Si 3 N 4 Especially outstanding. However, due to the high brittleness of ceramic materials, low toughness, weak thermal shock resistance, and poor processability, it is difficult to manufacture parts with large sizes and complex shapes. Therefore, it is necessary to produce components with complex shapes through the connection technology between ceramics. In order to avoid the thermal stress at the joint after the connection due to material differences between the intermediate ...

Examples

Embodiment 1

[0028] 1. Preparation:

[0029] (1) Dilute Y with 3mol / L dilute nitric acid 2 o 3 (purity is 99.99%, particle size is 1μm) is dissolved and prepared to obtain Y(NO 3 ) 3 solution;

[0030] (2) According to Y 2 o 3 and Al 2 o 3 (purity is 99%, particle size is 0.1μm) mass ratio is 55wt%: 45wt%, Al 2 o 3 Join Y(NO 3 ) 3 In the solution, the solvent is absolute ethanol, and the ball milling medium is Si 3 N 4 Grinding balls, mixing in a roller ball mill with 100r / min ball milling for 12h, to obtain a slurry;

[0031] (3) Add 90wt% nano-SiC powder (purity is 99.99%, particle size is 10nm) to the slurry, repeat the above ball milling process for mixing to obtain the connecting layer material;

[0032] (4) Place the connection layer material between two polished SiC ceramics to form a sandwich structure. In the heat treatment furnace, under the condition of nitrogen, the temperature is raised to 1200°C at 20°C / min and kept for 30min; then the temperature is raised to 1...

Embodiment 2

[0035] The difference from Example 1 is: with nano-Si 3 N 4 Powder (purity is 99.99%, particle size is 30nm) as raw material; Lu 2 o 3 Dissolve in 4mol / L nitric acid solution, according to Lu 2 o 3 and Al 2 o 3 The mass ratio of 40wt%: 60wt% is mixed to obtain the intermediate connection material; the sintering process is: heating at 100°C / min to 1000°C, holding for 10 minutes; then heating at 50°C / min to 1300°C, holding for 10 minutes, adding The pressure is 10MPa, the connection environment is vacuum, and Si 3 N 4 Ceramic connectors.

[0036] Si in this example 3 N 4 The thickness of the connection layer of the ceramic connector is 10 μm, the connection strength of the connection layer is 140MPa at room temperature, and 150MPa at a high temperature of 1200°C; Si 3 N 4 The leak rate at the connection between the ceramic and the connection layer is 1×10 -10 Pa·L / s.

Embodiment 3

[0038] The difference from Example 1 is: with nano-Si3 N 4 Powder (purity is 99.99%, particle size is 30nm) as raw material; La 2 o 3 Dissolved in 1mol / L nitric acid solution, according to La 2 o 3 and Al 2 o 3 The mass ratio of 50wt%: 50wt% is mixed to prepare the intermediate connection material; the sintering process is: the temperature is raised to 1100°C at 10°C / min, and the temperature is kept for 60min; The pressure is 0.1MPa, the connection environment is argon, and Si is produced. 3 N 4 Ceramic connectors.

[0039] Si in this example 3 N 4 The thickness of the connection layer of the ceramic connector is 50 μm, and the connection strength of the connection layer is 100 MPa at room temperature and 110 MPa at a high temperature of 1200 ° C; Si 3 N 4 The leakage rate at the connection between the ceramic and the connection layer reaches 1×10 -8 Pa·L / s.

technical field

[0001] The invention belongs to the technical field of non-oxide ceramic materials, and more specifically relates to a ceramic connector and its preparation method and application. Background technique

[0002] Fine ceramics generally have excellent characteristics such as high temperature resistance, high hardness, wear resistance, corrosion resistance, and high temperature strength. They are key materials in the fields of aerospace, military and nuclear energy. Among them, SiC and Si 3 N 4 Especially outstanding. However, due to the high brittleness of ceramic materials, low toughness, weak thermal shock resistance, and poor processability, it is difficult to manufacture parts with large sizes and complex shapes. Therefore, it is necessary to produce components with complex shapes through the connection technology between ceramics. In order to avoid the thermal stress at the joint after the connection due to material differences between the intermediate ...

Examples

Embodiment 1

[0028] 1. Preparation:

[0029] (1) Dilute Y with 3mol / L dilute nitric acid 2 o 3 (purity is 99.99%, particle size is 1μm) is dissolved and prepared to obtain Y(NO 3 ) 3 solution;

[0030] (2) According to Y 2 o 3 and Al 2 o 3 (purity is 99%, particle size is 0.1μm) mass ratio is 55wt%: 45wt%, Al 2 o 3 Join Y(NO 3 ) 3 In the solution, the solvent is absolute ethanol, and the ball milling medium is Si 3 N 4 Grinding balls, mixing in a roller ball mill with 100r / min ball milling for 12h, to obtain a slurry;

[0031] (3) Add 90wt% nano-SiC powder (purity is 99.99%, particle size is 10nm) to the slurry, repeat the above ball milling process for mixing to obtain the connecting layer material;

[0032] (4) Place the connection layer material between two polished SiC ceramics to form a sandwich structure. In the heat treatment furnace, under the condition of nitrogen, the temperature is raised to 1200°C at 20°C / min and kept for 30min; then the temperature is raised to 1...

Embodiment 2

[0035] The difference from Example 1 is: with nano-Si 3 N 4 Powder (purity is 99.99%, particle size is 30nm) as raw material; Lu 2 o 3 Dissolve in 4mol / L nitric acid solution, according to Lu 2 o 3 and Al 2 o 3 The mass ratio of 40wt%: 60wt% is mixed to obtain the intermediate connection material; the sintering process is: heating at 100°C / min to 1000°C, holding for 10 minutes; then heating at 50°C / min to 1300°C, holding for 10 minutes, adding The pressure is 10MPa, the connection environment is vacuum, and Si 3 N 4 Ceramic connectors.

[0036] Si in this example 3 N 4 The thickness of the connection layer of the ceramic connector is 10 μm, the connection strength of the connection layer is 140MPa at room temperature, and 150MPa at a high temperature of 1200°C; Si 3 N 4 The leak rate at the connection between the ceramic and the connection layer is 1×10 -10 Pa·L / s.

Embodiment 3

[0038] The difference from Example 1 is: with nano-Si3 N 4 Powder (purity is 99.99%, particle size is 30nm) as raw material; La 2 o 3 Dissolved in 1mol / L nitric acid solution, according to La 2 o 3 and Al 2 o 3 The mass ratio of 50wt%: 50wt% is mixed to prepare the intermediate connection material; the sintering process is: the temperature is raised to 1100°C at 10°C / min, and the temperature is kept for 60min; The pressure is 0.1MPa, the connection environment is argon, and Si is produced. 3 N 4 Ceramic connectors.

[0039] Si in this example 3 N 4 The thickness of the connection layer of the ceramic connector is 50 μm, and the connection strength of the connection layer is 100 MPa at room temperature and 110 MPa at a high temperature of 1200 ° C; Si 3 N 4 The leakage rate at the connection between the ceramic and the connection layer reaches 1×10 -8 Pa·L / s.