CN115340362A - Alumina fiber reinforced magnesia carbon sliding plate and preparation process thereof - Google Patents

Alumina fiber reinforced magnesia carbon sliding plate and preparation process thereof Download PDF

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Publication number
CN115340362A
CN115340362A CN202211043809.3A CN202211043809A CN115340362A CN 115340362 A CN115340362 A CN 115340362A CN 202211043809 A CN202211043809 A CN 202211043809A CN 115340362 A CN115340362 A CN 115340362A
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percent
granularity
minutes
alumina fiber
fused magnesia
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闫昕
刘士范
陈松林
蒋正跃
胡建辉
徐琳琳
袁彪
孙旭东
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Huadong Ruitai Technology Co ltd
Ruitai Technology Co ltd
YIXING REFRACTORY MATERIAL CO Ltd
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Huadong Ruitai Technology Co ltd
Ruitai Technology Co ltd
YIXING REFRACTORY MATERIAL CO Ltd
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    • C04B35/03Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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Abstract

The invention relates to an alumina fiber reinforced magnesia carbon sliding plate and a preparation process thereof, wherein alumina fibers are added and uniformly dispersed in a matrix to form an organic composite whole, so that the load borne by a matrix material is reduced, and the free energy of crack propagation is consumed; meanwhile, the spinel phase is generated by the in-situ reaction of the spinel phase and MgO in the matrix through high-temperature treatment, the mechanical property of the material is improved, and the thermal shock stability of the material is improved.

Description

Alumina fiber reinforced magnesia carbon sliding plate and preparation process thereof
Technical Field
The invention relates to an alumina fiber reinforced magnesia-carbon sliding plate and a preparation process thereof, belonging to the field of inorganic non-metallic material subject refractory materials.
Background
The sliding nozzle is a molten steel control device in the continuous casting process, can accurately adjust the flow of the molten steel from a ladle to a tundish, ensures the quality of a cast steel billet, and is an indispensable functional element in the continuous casting. The sliding plate brick needs to have good thermal shock resistance stability and high-temperature mechanical property due to the long-time bearing of thermal shock and mechanical scouring of molten steel and the frequent actions of rapid cooling and rapid heating.
In recent years, the smelting proportion of calcium-treated steel is increased year by year, and the traditional Al 2 O 3 -ZrO 2 -C and Al 2 O 3 the-C sliding plate is not resistant to corrosion and scouring when the calcium-treated steel is cast, and is easy to generate special horseshoe-shaped corrosion damage, so that the service life is influenced. Although the traditional MgO-C sliding plate does not react with CaO and FeO to generate eutectic compounds, the MgO-C sliding plate is suitable for casting steel grades such as calcium-treated steel, high-oxygen steel and the like, but has poor thermal shock stability, easy stripping, low strength and short service life.
The oxide fiber/oxide ceramic matrix composite can work for a long time in a high-temperature oxidation environment, and cannot form catastrophic fracture due to oxidation. The oxide ceramic fiber which is most widely researched and applied is alumina-based fiber, the alumina fiber has the characteristics of high modulus and strength, good thermal shock stability, chemical stability and the like, and can be effectively bonded with a matrix material to form a composite material with excellent performance, so that the mechanical property of the material is improved, and the thermal shock stability of the material is improved.
The aluminum oxide fiber reinforced magnesium-carbon sliding plate is researched and developed, the aluminum oxide fiber is added into the sliding plate, the thermal shock stability of the sliding plate is improved, and the high-temperature mechanical property of the material is improved, so that the use requirement of calcium-treated steel continuous casting production is met.
Disclosure of Invention
The invention relates to an alumina fiber reinforced magnesia carbon sliding plate and a preparation process thereof, wherein alumina fibers are added and uniformly dispersed in a matrix to form an organic composite whole, so that the load borne by the matrix material is reduced, the expansion free energy of cracks is consumed, and simultaneously, the alumina fiber reinforced magnesia carbon sliding plate and MgO in the matrix react in situ at high temperature to generate a spinel phase to form a high-strength net structure, so that the mechanical property of the material is improved, and the thermal shock stability of the material is improved.
The formula (weight and particle size content) of the invention is as follows:
(1) 7 to 15 percent of fused magnesia with the granularity of 5 to 3mm
(2) 15 to 25 percent of fused magnesia with the granularity of 3 to 1mm
(3) 10 to 20 percent of fused magnesia with the granularity of 1 to 0mm
(4) 5 to 15 percent of silicon carbide with the granularity of 1 to 0mm
(5) 25 to 35 percent of fused magnesia with the granularity of 0.045mm
(6) 3 to 6 percent of metal aluminum powder with the particle size of 0.045mm
(7) 2 to 4 percent of boron carbide with the particle size of 0.045mm
(8) 2 to 10 percent of alumina fiber
(9) 3 to 5 percent of carbon source powder
(10) 3 to 6 percent of binding agent, and is added in addition, the total mass percent of the raw materials is not counted
MgO of the fused magnesia is more than or equal to 97.5 percent;
the SiC is more than or equal to 97 percent;
the metallic aluminum Al is more than or equal to 95 percent;
the boron carbide B 4 C≥88%;
The alumina fiber is discontinuous fiber, wherein Al is 2 O 3 The diameter is more than or equal to 85 percent and is 10 to 15 mu m;
the carbon source powder is prepared by mixing crystalline flake graphite and carbon black according to the proportion of 1;
the binding agent is prepared by mixing phenolic resin and organic silicon modified resin according to the ratio of 4 to 1.
The specific process comprises the following steps:
(1) Strongly premixing the fused magnesia fine powder with the granularity of 0.045mm, the metal aluminum, the boron carbide and the carbon source powder for 15-20 minutes;
(2) Adding fused magnesia and silicon carbide particles of 5-3 mm, 3-1 mm and 1-0 mm into a mixer with a rod-shaped stirring blade according to a proportion, carrying out dry mixing for 2 minutes, adding alumina fiber, stirring and dispersing for 5-10 minutes, adding all bonding agents, mixing for 3-5 minutes, adding all premixed fine powder and micro powder, mixing for 15-20 minutes, and homogenizing through strong mixing to obtain a mixture, wherein the effective time is 30-35 minutes;
(3) Discharging the mixture to remove agglomerated large blocks, and ageing the mixture for 20 to 30 hours under the conditions of constant temperature and constant humidity;
(4) Pressing and forming;
(5) Naturally drying for 20-30 hours, and then drying for 30-48 hours at 220-280 ℃;
(6) Sintering at 1550-1650 deg.C for 12-18 h.
The magnesium-carbon sliding plate produced by the invention has excellent mechanical property and thermal shock stability, and compared with the prior art, the magnesium-carbon sliding plate has the remarkable difference that:
(1) A mixer with rod-shaped stirring blades is adopted, the contact area of the mixer and fibers is small, the fibers are prevented from being damaged, the alumina fibers are uniformly dispersed, a reaction interface of the alumina fibers and a base material is designed, and the thermal shock stability of the material is improved. The alumina fiber which is uniformly dispersed and MgO in the matrix are subjected to high-temperature heat treatment to generate in-situ reaction, and a spinel phase is generated at an interface, so that the alumina fiber and the matrix material are combined into ceramic, and the combination is tighter. Meanwhile, the magnesia-alumina spinel has good erosion resistance, abrasion resistance and good thermal shock stability.
(2) Alumina fiber toughening mechanism. The alumina fiber has high strength (1.4 to 2.45GPa), high modulus (190 to 385GPa), low thermal expansion coefficient and uniform distribution in the matrix material to form an organic composite whole, when an external load acts on the matrix material, the matrix material can transfer a part of the load to the alumina fiber, so that the load of the matrix material is reduced, when the stress borne by the fiber is greater than the self-strength, the fiber is broken and pulled out, so that the diffusion energy of cracks is consumed, and the toughness and the plasticity are provided for the matrix material.
(3) The alumina fiber can effectively consume the free energy of crack diffusion, and improve the toughness and mechanical property of the material. The fibers have larger surface area than the particles, and when the cracks are expanded to the fibers, the cracks need to deflect longer paths, so that more crack expansion free energy is consumed; meanwhile, the crack deflects, and the crack propagation path is zigzag, so that the surface energy of the crack is increased, the reinforcing effect is achieved, and the strength of the material is improved.
Detailed Description
Example 1
The following formulations (weight and particle size content) were used:
(1) 7 percent of fused magnesia with the granularity of 5-3 mm
(2) 25 percent of fused magnesia with the granularity of 3-1 mm
(3) 15 percent of fused magnesia with the granularity of 1-0 mm
(4) 10 percent of silicon carbide with the granularity of 1-0 mm
(5) 30 percent of fused magnesia with the granularity of 0.045mm
(6) 4 percent of metal aluminum powder with the particle size of 0.045mm
(7) Boron carbide with particle size of 0.045mm 4%
(8) 2 percent of alumina fiber
(9) Carbon source powder 3%
(10) 3.8% of a binding agent, 3% of phenolic resin and 3% of organic silicon resin, excluding the total mass percentage of the raw materials
The preparation process comprises the following parts:
(1) Strongly premixing the fused magnesia fine powder with the granularity of 0.045mm, the metallic aluminum, the boron carbide and the carbon source powder for 15 minutes;
(2) Adding fused magnesia and silicon carbide particles of 5-3 mm, 3-1 mm and 1-0 mm into a mixer with a rod-shaped stirring blade according to a proportion, carrying out dry mixing for 2 minutes, adding alumina fiber, stirring and dispersing for 5 minutes, adding all bonding agents, mixing for 3 minutes, adding all premixed fine powder and micro powder, mixing for 20 minutes, and homogenizing to obtain a mixture through strong mixing, wherein the effective time is 30 minutes;
(3) Discharging the mixture to remove agglomerated large blocks, and ageing the mixture for 24 hours under the conditions of constant temperature and constant humidity;
(4) Pressing and forming;
(5) Naturally drying for 30 hours, and then drying for 48 hours at 220 ℃;
(6) Firing at 1550 ℃ for 18 hours.
Table 1 shows the specifications and formulation of the raw materials and their properties of example 1, which, when tested, had a bulk density of 3.12g/cm 3 The apparent porosity is 7.6%, the normal temperature compressive strength reaches 156MPa, the high temperature rupture strength (1400 ℃ multiplied by 0.5 h) is 26MPa, the sliding plate has micro cracks, no through cracks and no peeling phenomenon after being used for trial in 120-ton ladle casting calcium treatment steel in a steel mill, the average service life is 4 times, and the use requirements of the existing products are met.
Example 2
The following formulations (weight and particle size content) were used:
(1) 15 percent of fused magnesia with the granularity of 5-3 mm
(2) 20 percent of fused magnesia with the granularity of 3-1 mm
(3) 10 percent of fused magnesia with the granularity of 1-0 mm
(4) 5 percent of silicon carbide with the granularity of 1-0 mm
(5) 28 percent of fused magnesia with the granularity of 0.045mm
(6) 6 percent of metal aluminum powder with the particle size of 0.045mm
(7) Boron carbide 2% with particle size of 0.045mm
(8) 10 percent of alumina fiber
(9) Carbon source powder 4%
(10) 5.5% of a binding agent, 4% of phenolic resin and 1% of organic silicon resin, and the total mass percentage of the raw materials is not counted
The process comprises the following parts:
(1) Strongly premixing the fused magnesia fine powder with the granularity of 0.045mm, the metal aluminum, the boron carbide and the carbon source powder for 17 minutes;
(2) Adding fused magnesia and silicon carbide particles of 5-3 mm, 3-1 mm and 1-0 mm into a mixer with a rod-shaped stirring blade according to a proportion, carrying out dry mixing for 2 minutes, adding alumina fiber, stirring and dispersing for 10 minutes, adding all bonding agents, mixing for 5 minutes, adding all premixed fine powder and micro powder, mixing for 18 minutes, and homogenizing to obtain a mixture through strong mixing, wherein the effective time is 35 minutes;
(3) Discharging the mixture to remove agglomerated large blocks, and ageing the mixture for 30 hours under the conditions of constant temperature and constant humidity;
(4) Pressing and forming;
(5) Naturally drying for 24 hours, and then drying for 30 hours at 280 ℃;
(6) Firing at 1650 ℃ for 12 hours.
Table 1 shows the specifications and formulation of the raw materials and their properties of example 2, which, when tested, had a bulk density of 3.21g/cm 3 The apparent porosity is 6.6%, the normal temperature compressive strength reaches 161MPa, the high temperature rupture strength (1400 ℃ multiplied by 0.5 h) is 28MPa, the average service life is 4.1 times, the hole expansion is uniform, and the phenomena of steel clamping, galling and the like do not exist when the method is used for casting calcium-treated steel in 100 tons of steel ladles in a steel mill.
Example 3
The following formulations (weight and particle size content) were used:
(1) 10 percent of fused magnesia with the granularity of 5-3 mm
(2) 15 percent of fused magnesia with the granularity of 3-1 mm
(3) 20 percent of fused magnesia with the granularity of 1-0 mm
(4) 8 percent of silicon carbide with the granularity of 1-0 mm
(5) 32 percent of fused magnesia with the granularity of 0.045mm
(6) 3 percent of metal aluminum powder with the particle size of 0.045mm
(7) Boron carbide with the particle size of 0.045mm 3%
(8) 4 percent of alumina fiber
(9) Carbon source powder 5%
(10) 4.8% of a binding agent, 1% of phenolic resin and organic silicon resin, excluding the total mass percentage of the raw materials
The process comprises the following steps:
(1) Strongly premixing the fused magnesia fine powder with the granularity of 0.045mm, the metal aluminum, the boron carbide and the carbon source powder for 18 minutes;
(2) Adding fused magnesia and silicon carbide particles with the particle sizes of 5-3 mm, 3-1 mm and 1-0 mm into a mixer with a rod-shaped stirring blade according to a certain proportion, carrying out dry mixing for 2 minutes, adding alumina fiber, stirring and dispersing for 7 minutes, adding all bonding agents, mixing for 3 minutes, adding all premixed fine powder and micro powder, mixing for 20 minutes, and homogenizing into a mixture through strong mixing, wherein the effective time is 32 minutes;
(3) Discharging the mixture to remove agglomerated large blocks, and ageing the mixture for 26 hours under the conditions of constant temperature and constant humidity;
(4) Pressing and forming;
(5) Naturally drying for 26 hours, and then drying for 36 hours at 260 ℃;
(6) Firing at 1600 ℃ for 16 hours.
Table 1 shows the specifications and formulation of the raw materials and their properties of example 3, which was tested to have a bulk density of 3.15g/cm 3 The apparent porosity is 6.4%, the normal temperature compressive strength reaches 158MPa, the high temperature rupture strength (1400 ℃ multiplied by 0.5 h) is 20MPa, the average service life is 4.1 times when the high temperature rupture strength is tried out in 80 ton ladle casting calcium treatment steel in a steel mill, and the used plate surface is flat without steel clamping, through cracks, peeling and the like.
Example 4
The following formulations (weight and particle size content) were used:
(1) 8 percent of fused magnesia with the granularity of 5-3 mm
(2) 16 percent of fused magnesia with the granularity of 3-1 mm
(3) 12 percent of fused magnesia with the granularity of 1-0 mm
(4) 15 percent of silicon carbide with the granularity of 1-0 mm
(5) 35 percent of fused magnesia with the granularity of 0.045mm
(6) 3 percent of metal aluminum powder with the particle size of 0.045mm
(7) Boron carbide with particle size of 0.045mm 3%
(8) 5 percent of alumina fiber
(9) Carbon source powder 3%
(10) 6% of binding agent, 2% of phenolic resin and organic silicon resin, excluding raw materials in percentage by mass
The process comprises the following parts:
(1) Strongly premixing the fused magnesia fine powder with the granularity of 0.045mm, the metal aluminum, the boron carbide and the carbon source powder for 16 minutes;
(2) Adding fused magnesia and silicon carbide particles of 5-3 mm, 3-1 mm and 1-0 mm into a mixer with a rod-shaped stirring blade according to a proportion, carrying out dry mixing for 2 minutes, adding alumina fiber, stirring and dispersing for 8 minutes, adding all bonding agents, mixing for 4 minutes, adding all premixed fine powder and micro powder, mixing for 17 minutes, and homogenizing to obtain a mixture through strong mixing, wherein the effective time is 31 minutes;
(3) Discharging the mixture to remove agglomerated large blocks, and ageing the mixture for 28 hours under the conditions of constant temperature and constant humidity;
(4) Pressing and forming;
(5) Naturally drying for 28 hours, and then drying for 40 hours at the temperature of 240 ℃;
(6) Firing at 1620 ℃ for 15 hours.
Table 1 shows the specifications and formulation of the raw materials and their properties of example 4, which, when tested, had a bulk density of 3.14g/cm 3 The apparent porosity is 6.5%, the normal temperature compressive strength reaches 153MPa, the high temperature rupture strength (1400 ℃ multiplied by 0.5 h) is 24MPa, the average service life is 4.5 times when the high temperature rupture strength is tried out in 80-ton ladle casting calcium treatment steel in a steel mill, the used plate surface is flat, the hole expansion is uniform, and the phenomena of block falling, peeling, galling and the like are avoided.
The specifications, formulations and test performances of the raw materials of the sliding plate prepared by the above embodiment are as follows in table 1:
Figure DEST_PATH_IMAGE001

Claims (3)

1. an alumina fiber reinforced magnesium-carbon sliding plate comprises the following components in percentage by weight:
(1) 7-15% of fused magnesia with the granularity of 5-3 mm;
(2) 15 to 25 percent of fused magnesia with the granularity of 3 to 1 mm;
(3) 10-20% of fused magnesia with the granularity of 1-0 mm;
(4) 5 to 15 percent of silicon carbide with the granularity of 1 to 0 mm;
(5) 25-35% of fused magnesia with the granularity of 0.045 mm;
(6) 3 to 6 percent of metal aluminum powder with the granularity of 0.045 mm;
(7) 2 to 4 percent of boron carbide with the granularity of 0.045 mm;
(8) 2 to 10 percent of alumina fiber;
(9) 3-5% of carbon source powder;
(10) 3-6% of binding agent, and the total mass percentage of the raw materials is not added.
2. The alumina fiber reinforced magnesium carbon skateboard of claim 1, wherein: mgO of the fused magnesia is more than or equal to 97.5 percent; the SiC is more than or equal to 97 percent; the metal aluminum Al is more than or equal to 95 percent; the boron carbide B 4 C is more than or equal to 88 percent; the alumina fiber is discontinuous fiber, wherein Al is 2 O 3 More than or equal to 85 percent, and the diameter is 10 to 15 mu m; the carbon source powder is prepared by mixing crystalline flake graphite and carbon black according to the proportion of 1; the binding agent is prepared by mixing phenolic resin and organic silicon modified resin according to the ratio of 4 to 1.
3. A process for preparing the alumina fiber reinforced magnesia carbon slide board according to any one of claims 1 to 2, comprising the steps of:
(1) Strongly premixing the fused magnesia fine powder with the granularity of 0.045mm, the metal aluminum, the boron carbide and the carbon source powder for 15-20 minutes;
(2) Adding fused magnesia and silicon carbide particles of 5-3 mm, 3-1 mm and 1-0 mm into a mixer with a rod-shaped stirring blade according to a proportion, carrying out dry mixing for 2 minutes, adding alumina fiber, stirring and dispersing for 5-10 minutes, adding all bonding agents, mixing for 3-5 minutes, adding all premixed fine powder and micro powder, mixing for 15-20 minutes, and homogenizing through strong mixing to obtain a mixture, wherein the effective time is 30-35 minutes;
(3) Discharging the mixture to remove agglomerated large blocks, and ageing the mixture for 20-30 hours under the conditions of constant temperature and constant humidity;
(4) Pressing and forming;
(5) Naturally drying for 20-30 hours, and then drying for 30-48 hours at 220-280 ℃;
(6) Sintering at 1550-1650 deg.c for 12-18 hr.
CN202211043809.3A 2022-08-30 2022-08-30 Alumina fiber reinforced magnesia carbon sliding plate and preparation process thereof Pending CN115340362A (en)

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Application publication date: 20221115