Method for sintering zirconium diboride ceramic material

Abstract

The invention belongs to the technical field of inorganic composite material preparation, and in particular relates to a method for sintering a zirconium diboride ceramic material. The zirconium diboride ceramic material is prepared from ZrB2, ZrC and Si powder by a discharge plasma sintering process. The ZrB2-SiC-ZrSi2 super-high temperature ceramic material with complete compactness and excellent performance is prepared at a lower temperature of 1500 DEG C.

Description

technical field

[0001] The invention belongs to the technical field of inorganic composite material preparation, in particular to a sintering method of zirconium diboride ceramic material. Background technique

[0002] With the rapid development of aerospace and national defense, modern aircraft (such as hypersonic aircraft, missiles, space shuttles, etc.) Requirements: Be able to adapt to some extreme environments such as supersonic cruise flight, atmospheric reentry, transatmospheric long-duration flight and rocket propulsion. Research on ultra-high temperature materials is a key technical requirement for the development of aerospace and national defense. Therefore, the research on ultra-high temperature materials has very important strategic significance in the country's aerospace and national defense.

[0003] ZrB 2 It has the advantages of high melting point (3245°C), high strength, high hardness, good electrical and thermal conductivity, and good corrosion resistanc...

Examples

Embodiment 1

[0023] Weigh ZrB 2 40g of ZrC powder, 5.5059g of ZrC powder, and 4.4941g of Si powder. Pour all the weighed materials into a ball mill jar, add alcohol and 100g of zirconia balls, and mix the materials on a ball mill at 150 rpm for 4 hours. After the ball milled material is filtered, it is dried in a vacuum drying oven, and after drying, it is sieved 3 times to obtain a mixed raw material mixture.

[0024] Weigh 25g of the above-mentioned mixed raw material mixture, put it into a graphite mold with a diameter of 30mm, carry out discharge plasma sintering under a vacuum atmosphere, raise the temperature to 1500°C at 100°C / min, keep it warm for 5min, press at 40MPa, and cool naturally to obtain ZrB 2 -SiC-ZrSi 2 Ceramic composite materials, SiC and ZrSi in the material 2 The theoretical mass percentage content of is 20wt%.

[0025] figure 1 The ZBZSS20 pattern in the middle is the XRD pattern of the sintered sample. It can be seen from the figure that except for the ZrB 2 ...

Embodiment 2

[0027] Weigh ZrB 2 35g ZrC powder, 8.2588g ZrC powder, and 6.7412g Si powder. Pour all the weighed materials into a ball mill jar, add alcohol and 100g of zirconia balls, and mix the materials on a ball mill at 150 rpm for 4 hours. After the ball-milled material is filtered, it is placed in a vacuum drying oven for drying, and after drying, it is sieved 3 times to obtain a mixed raw material mixture.

[0028]Weigh 25g of the above-mentioned mixed raw material mixture, put it into a graphite mold with a diameter of 30mm, carry out discharge plasma sintering under vacuum atmosphere, raise the temperature to 1500°C at 100°C / min, keep the temperature for 10min, and press 30MPa, and then naturally cool to obtain ZrB 2 -SiC-ZrSi 2 Ceramic composites, SiC and ZrSi in materials 2 The theoretical mass percentage content of is 30wt%.

[0029] figure 1 The ZBZSS30 pattern in the middle is the XRD pattern of the sintered sample. It can be seen from the figure that except for the ZrB ...

Embodiment 3

[0031] Weigh ZrB 2 30g ZrC powder, 11.0117g ZrC powder, and 8.9883g Si powder. Pour all the weighed materials into a ball mill jar, add alcohol and 100g zirconia balls, and mix the materials on a ball mill at 150 rpm for 4 hours. After the ball-milled material is filtered, it is placed in a vacuum drying oven for drying, and after drying, it is sieved 3 times to obtain a mixed raw material mixture.

[0032] Weigh 25g of the above-mentioned mixed raw material mixture, put it into a graphite mold with a diameter of 30mm, carry out discharge plasma sintering under a vacuum atmosphere, heat up to 1500°C at 100°C / min, keep it warm for 15min, and press 20MPa. After natural cooling, the Get ZrB 2 -SiC-ZrSi 2 Ceramic composites, SiC and ZrSi in materials 2 The theoretical mass percentage content of is 40wt%.

[0033] figure 1 The ZBZSS40 pattern in the middle is the XRD pattern of the sintered sample. It can be seen from the figure that except for the ZrB 2 SiC and ZrSi can also...

technical field

[0001] The invention belongs to the technical field of inorganic composite material preparation, in particular to a sintering method of zirconium diboride ceramic material. Background technique

[0002] With the rapid development of aerospace and national defense, modern aircraft (such as hypersonic aircraft, missiles, space shuttles, etc.) Requirements: Be able to adapt to some extreme environments such as supersonic cruise flight, atmospheric reentry, transatmospheric long-duration flight and rocket propulsion. Research on ultra-high temperature materials is a key technical requirement for the development of aerospace and national defense. Therefore, the research on ultra-high temperature materials has very important strategic significance in the country's aerospace and national defense.

[0003] ZrB 2 It has the advantages of high melting point (3245°C), high strength, high hardness, good electrical and thermal conductivity, and good corrosion resistanc...

Examples

Embodiment 1

[0023] Weigh ZrB 2 40g of ZrC powder, 5.5059g of ZrC powder, and 4.4941g of Si powder. Pour all the weighed materials into a ball mill jar, add alcohol and 100g of zirconia balls, and mix the materials on a ball mill at 150 rpm for 4 hours. After the ball milled material is filtered, it is dried in a vacuum drying oven, and after drying, it is sieved 3 times to obtain a mixed raw material mixture.

[0024] Weigh 25g of the above-mentioned mixed raw material mixture, put it into a graphite mold with a diameter of 30mm, carry out discharge plasma sintering under a vacuum atmosphere, raise the temperature to 1500°C at 100°C / min, keep it warm for 5min, press at 40MPa, and cool naturally to obtain ZrB 2 -SiC-ZrSi 2 Ceramic composite materials, SiC and ZrSi in the material 2 The theoretical mass percentage content of is 20wt%.

[0025] figure 1 The ZBZSS20 pattern in the middle is the XRD pattern of the sintered sample. It can be seen from the figure that except for the ZrB 2 ...

Embodiment 2

[0027] Weigh ZrB 2 35g ZrC powder, 8.2588g ZrC powder, and 6.7412g Si powder. Pour all the weighed materials into a ball mill jar, add alcohol and 100g of zirconia balls, and mix the materials on a ball mill at 150 rpm for 4 hours. After the ball-milled material is filtered, it is placed in a vacuum drying oven for drying, and after drying, it is sieved 3 times to obtain a mixed raw material mixture.

[0028]Weigh 25g of the above-mentioned mixed raw material mixture, put it into a graphite mold with a diameter of 30mm, carry out discharge plasma sintering under vacuum atmosphere, raise the temperature to 1500°C at 100°C / min, keep the temperature for 10min, and press 30MPa, and then naturally cool to obtain ZrB 2 -SiC-ZrSi 2 Ceramic composites, SiC and ZrSi in materials 2 The theoretical mass percentage content of is 30wt%.

[0029] figure 1 The ZBZSS30 pattern in the middle is the XRD pattern of the sintered sample. It can be seen from the figure that except for the ZrB ...

Embodiment 3

[0031] Weigh ZrB 2 30g ZrC powder, 11.0117g ZrC powder, and 8.9883g Si powder. Pour all the weighed materials into a ball mill jar, add alcohol and 100g zirconia balls, and mix the materials on a ball mill at 150 rpm for 4 hours. After the ball-milled material is filtered, it is placed in a vacuum drying oven for drying, and after drying, it is sieved 3 times to obtain a mixed raw material mixture.

[0032] Weigh 25g of the above-mentioned mixed raw material mixture, put it into a graphite mold with a diameter of 30mm, carry out discharge plasma sintering under a vacuum atmosphere, heat up to 1500°C at 100°C / min, keep it warm for 15min, and press 20MPa. After natural cooling, the Get ZrB 2 -SiC-ZrSi 2 Ceramic composites, SiC and ZrSi in materials 2 The theoretical mass percentage content of is 40wt%.

[0033] figure 1 The ZBZSS40 pattern in the middle is the XRD pattern of the sintered sample. It can be seen from the figure that except for the ZrB 2 SiC and ZrSi can also...

Images