CN107417287B - Corundum-silicon oxynitride composite refractory material for microwave metallurgical kiln car - Google Patents

Corundum-silicon oxynitride composite refractory material for microwave metallurgical kiln car Download PDF

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CN107417287B
CN107417287B CN201710736091.9A CN201710736091A CN107417287B CN 107417287 B CN107417287 B CN 107417287B CN 201710736091 A CN201710736091 A CN 201710736091A CN 107417287 B CN107417287 B CN 107417287B
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silicon oxynitride
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CN107417287A (en
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徐恩霞
王玉霞
董萌蕾
刘新红
刘萍
赵飞
李婕
薛娟娟
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Sinosteel luonai Technology Co., Ltd
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped 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 aluminium oxide
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    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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Abstract

Disclosure of the inventionThe corundum-silicon oxynitride composite refractory material for the microwave metallurgical kiln car has the advantages of low electromagnetic wave absorption rate, excellent wave permeability, good high-temperature volume stability, good thermal shock resistance and excellent erosion resistance, and the preparation method thereof. The raw materials are as follows: corundum aggregate, corundum fine powder and SiO2Powder of Si and powder of N, forming by press forming2The corundum-silicon oxynitride composite refractory material is prepared by in-situ nitridation reaction sintering in atmosphere, the main crystal phase of the corundum-silicon oxynitride composite refractory material is corundum and silicon oxynitride, and a small amount of β -Si is contained in a matrix3N4β -Sialon and O' -Sialon, having a bulk density of 3.0g/cm3Above, room temperature compressive strength: 170-190MPa, and normal-temperature breaking strength: 25-30MPa, dielectric loss tangent: 0.0014-0.0033, and has good wave permeability.

Description

Corundum-silicon oxynitride composite refractory material for microwave metallurgical kiln car
Technical Field
The invention relates to a refractory material for a microwave metallurgical kiln car, in particular to a refractory material prepared by adding Si powder and Si02A corundum-silicon oxynitride composite refractory material prepared by powder in-situ reaction and a preparation method thereof.
Background
With the continuous development of science and technology, environmental protection is more and more emphasized in life and production. In the traditional heavy industry, particularly high-temperature industries such as metal smelting and the like, the change of a production mode is urgently needed to meet the national development requirement. The emergence of microwave heating technology has enabled high-temperature heating to have a more energy-saving and environment-friendly heating mode, wherein the mode of smelting metal by microwave heating is called green metallurgy, and is a new technology emerging in recent years.
Due to the emergence of microwave metallurgical technology, the refractory material for the microwave metallurgical kiln car is mainly used as a kiln car carrier for bearing materials, the materials enter from a kiln on the kiln car and are discharged from the tail of the kiln after microwave smelting. Because the kiln car is directly unloaded at room temperature during rapid heating and discharging of microwave heating, the refractory material for the kiln car has higher performance requirements: (1) low electromagnetic wave absorption rate and excellent wave permeability: firstly, the refractory material is prevented from absorbing more electromagnetic energy under the action of electromagnetic waves to cause damage to the material due to overhigh temperature, and secondly, energy can be saved, so that limited electromagnetic energy is absorbed by metallurgical materials, and the smelting time is shortened; (2) excellent thermal shock resistance: the impact of larger thermal stress on the material can be resisted in the microwave heating rapid heating process; (3) good high-temperature mechanical properties: the lining material is subjected to various structural stress mechanical actions in the microwave metallurgical reaction process; (4) the corrosion resistance is excellent: the refractory material is contacted with the metallurgical material for a long time at high temperature, and is easy to generate chemical reaction with the metallurgical material, so that the structure of the refractory material is damaged.
Corundum and mullite are refractory materials which are most used in microwave metallurgy at present, have good thermal shock performance, but have poor corrosion resistance of alkaline slag and transmission performance of electromagnetic waves. The dielectric constant of the pure corundum material is generally 8-10, and the alumina has weak microwave absorption capacity and good wave permeability at low temperature. However, the dielectric constant of corundum increases with the rise of temperature, so that the heat loss of corundum in an electromagnetic field is increased, and the corundum material has poor thermal shock resistance and is not suitable for being used as a furnace lining and a kiln car material for microwave heating. The quartz ceramic has very small dielectric constant below 1000 deg.c, dielectric constant of about 4, high wave permeability and small expansion coefficient, and may be used widely in microwave metallurgy. However, since quartz is easy to undergo crystal transformation at high temperature, the maximum use temperature of quartz cannot exceed 1150 ℃, and quartz is not suitable for use in high-temperature microwave metallurgy.
At present, the research on a refractory material system for microwave metallurgy is not available, and if the refractory material meeting the use environment of a microwave metallurgical kiln car can be researched and prepared, the service life of the kiln car can be prolonged, the metallurgical efficiency is improved, the production cost is reduced, fewer and fewer resources on the earth are reasonably utilized, and the waste and the consumption of the resources are reduced.
Disclosure of Invention
In order to solve the problem that the existing refractory material cannot meet the performance requirements of a microwave metallurgical kiln car, the invention provides the corundum-silicon oxynitride composite refractory material for the microwave metallurgical kiln car, which has the advantages of low electromagnetic wave absorption rate, excellent wave permeability, good high-temperature volume stability, good thermal shock resistance and excellent erosion resistance, and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a corundum-silicon oxynitride composite refractory material comprises the following raw materials: corundum aggregate, corundum fine powder and SiO2Powder of Si and powder of N, forming by press forming2The material is prepared by in-situ nitridation reaction sintering under the atmosphere.
The raw materials of the invention are added in parts by weight: 30-45 parts of corundum aggregate with the granularity of 3-1mm, 20-25 parts of corundum aggregate with the granularity of 1-0mm, 15-25 parts of corundum fine powder and SiO23-6 parts of micro powder, 10-15 parts of Si powder, and the addition amount of the bonding agent is 3-6% of the total weight of the raw material.
The corundum aggregate is one or more than two of plate-shaped corundum, fused brown corundum, fused compact corundum and fused white corundum;
wherein the corundum aggregate with the granularity of 3-1mm and 1-0mm is added for the following purposes: according to the fracture morphology chart, short columnar silicon nitride oxide and long columnar silicon nitride grow in the material with corundum particles as the framework, and the silicon oxynitride and the silicon nitride grow on the surface of corundum aggregate or in air holes, so that the effect of buffering stress is achieved in the material, the toughness of the composite material is improved, and the thermal shock stability of the final product is improved and the expansion coefficient is reduced.
The corundum fine powder is one or more than two of plate-shaped corundum, fused brown corundum, fused compact corundum and fused white corundum; the granularity is one or two granularity intervals of less than or equal to 0.088mm and less than or equal to 0.045 mm;
wherein the particle size distribution of the corundum fine powder is that: because the granularity of part of the corundum fine powder reaches the superfine powder level, the superfine powder permeates into the finally obtained crystal phase, and besides silicon oxynitride and silicon nitride, part of Sialon crystal phase is well combined with corundum, so that the strength and the wave permeability of the material are improved.
The SiO2The micro powder is one or more than two of superfine natural quartz sand powder, silicon micro powder and gas-phase silicon oxide micro powder; the purity is more than or equal to 98 percent, and the grain diameter is less than 10 mu m.
Wherein SiO is2The particle size distribution of the micropowder is as follows: SiO 22The granularity reaches the micro-powder level, SiO2The powder can sufficiently penetrate into the gaps of the raw material, so that the main crystal phase of the final product is an in-situ generated silicon oxynitride crystal phase, because the generated silicon oxynitride crystal phase has low electromagnetic wave absorption rate and excellent wave permeability.
The purity of the Si powder is more than or equal to 99 percent, and the granularity is less than or equal to 0.045 mm;
the Si powder reacts with nitrogen in the sintering process to generate phases of silicon nitride, silicon oxynitride and the like in situ, so that the sintering of the material is promoted, the thermal state strength and the wave permeability of the composite material are improved, and the compactness of the material is increased and the erosion resistance is improved. The granularity of the Si powder is less than or equal to 0.045 mm; the purpose is to make silicon powder easier to be completely nitrided at the preparation temperature to form silicon oxynitride.
Wherein the added corundum aggregate and fine powder are the main crystal phase of the material and play the role of a skeleton, and SiO in the matrix2In-situ generation of Si from micro powder and Si powder in high-temperature flowing nitrogen2N2O is combined with corundum aggregate, and Si is removed from the matrix due to the surplus of Si powder and the existence of part of ultramicro corundum powder2N2O and part of Si3N4And Sialon phase generation. Si2N2The crystalline phases of the non-oxides such as O and the like grow on the surface of the corundum aggregate in a columnar shape, so that the material strength and wave permeability of a final product are improved, the internal thermal stress of the material is buffered, the toughness of the composite material is improved, and the thermal shock stability and the expansion coefficient are improved and reduced.
The binding agent is one or more of phenolic resin, dextrin, polyvinyl alcohol, carboxymethyl cellulose and pulp waste liquid.
The preparation method of the corundum-silicon oxynitride composite refractory material for the microwave metallurgical kiln car comprises the following steps:
firstly, 15-25 parts of corundum fine powder and SiO23-6 parts of micro powder and 10-15 parts of Si powder are put into a ball millGrinding the corundum balls in the machine at the rotating speed of 1000-1200 rpm for 180 minutes according to the proportion of the corundum balls to the materials of 1:1 to obtain premixed fine powder;
step two, pouring 30-45 parts of corundum aggregate with the granularity of 3-1mm and 20-25 parts of corundum aggregate with the granularity of 1-0mm into a mixing mill, and then adding 3-6 parts of corundum aggregatewtMixing binder, stirring for 5-10min to make binder uniformly adhere to the surface of corundum granule and wet it, adding the premixed fine powder obtained in step one, stirring for 10-20min to make the material be fully mixed;
step three, putting the mixed materials into a sealed bag, and placing the sealed bag for 12-24h in an air atmosphere with the air humidity of 50-60% at room temperature;
after ageing, preparing the uniformly mixed materials into green bricks by using a hydraulic press under the pressure of 120MPa, and drying the formed green bricks in a drying oven at the temperature of 120 ℃ for 24 hours;
and fifthly, weighing the dried sample, conveying the sample into a nitriding furnace, introducing nitrogen into a sealed furnace door, heating to 1100 ℃ at a heating rate of 5-8 ℃/min under the micro-positive pressure flowing nitrogen atmosphere, preserving heat for 2 hours, heating to 1450 ℃ at a rate of 1-5 ℃/min, preserving heat for 24 hours, and cooling to room temperature along with the furnace to obtain the corundum-silicon oxynitride composite refractory material.
Wherein, firstly, corundum fine powder and SiO are mixed2The powder and Si powder are premixed for the purpose of SiO2The powder, the Si powder and the corundum fine powder can be uniformly mixed, so that the short column-shaped crystal silicon oxynitride formed after nitridation is uniformly distributed, and the strength and the wave permeability of the material are enhanced.
The third step is to make the water in the binding agent uniformly distributed, improve the forming performance of the blank, and make the adobe aggregate and the fine powder uniformly distributed without segregation, so that the final product has low electromagnetic wave absorption rate and excellent wave permeability.
Wherein the temperature of 1100 ℃ in the fifth step is kept, because the nitriding reaction starts at the temperature, the temperature of 1450 ℃ is kept for a long time, which is beneficial to more silicon oxynitride generation and further sintering of the material.
The invention introduces a certain amount of silicon oxide particles by taking corundum as a base materialOptimized combination of powder, silicon powder and raw materials, reasonable particle size ratio, and one-step sintering by adopting in-situ nitridation reaction under high-temperature nitrogen atmosphere to prepare the corundum-silicon oxynitride composite refractory material, wherein the main crystal phase of the material is corundum and silicon oxynitride, and the secondary crystal phase of the material is β -Si3N4β -Sialon, O' -Sialon and other non-oxide binding phases, so that the composite material has excellent wave permeability, high temperature volume stability, thermal shock resistance and corrosion resistance.
The corundum-silicon oxynitride composite material is prepared by adopting in-situ reaction sintering, and silicon oxynitride is not directly added into the raw materials, because the silicon oxynitride and the corundum both belong to high-melting-point phases, higher sintering temperature or sintering aid is needed, better compounding of the materials is not facilitated, and the high-temperature performance of the composite material is greatly influenced3N4And Sialon solid solution, and these products have greatly raised wave permeability, heat expansion and strength.
According to the invention, the silicon oxide micro powder and the Si powder which are relatively cheap are selected as raw materials, and compared with silicon oxynitride powder, the production cost of the material is remarkably reduced while the corundum-silicon oxynitride composite refractory material with good performance is prepared.
The material used by the invention is mainly corundum which is a neutral oxide material and has good erosion resistance to acid and alkaline slag, so the material can be used as a refractory material of a kiln car to sinter materials made of any material, and the application range is wider.
The corundum-silicon oxynitride composite refractory material has the main crystal phases of corundum and silicon oxynitride, and a small amount of β -Si in a matrix3N4β -Sialon and O' -Sialon, having a bulk density of 3.0g/cm3Above, room temperature compressive strength: 170-190MPa, and normal-temperature breaking strength: 25-30MPa, the thermal rupture strength at 1400 ℃ is about 20-30MPa, and the temperature is 1100 ℃ to water cooling times according to YB/T376.1-1995 standardThe number is 10-50 times, and the room-temperature dielectric constant: 8-9, dielectric loss tangent: 0.0014-0.0033, and has good wave permeability.
Detailed Description
The practice and features of the present invention are illustrated below, but the present invention is not limited to the following examples.
Example 1:
firstly, 17 parts of corundum fine powder and SiO2Powder 3 parts, SiO2The method comprises the following steps of putting 10 parts of Si powder with the particle size of 1-5 mu m into a ball mill, and premixing for 120 minutes at the rotating speed of 1000-1200 rpm according to the proportion of corundum balls to materials of 1:1 to obtain premixed fine powder;
step two, pouring 45 parts of corundum aggregate with the granularity of 3-1mm and 25 parts of corundum aggregate with the granularity of 1-0mm into a mixing mill, and then adding 6 parts of corundum aggregatewt% of the bonding agent is started, the mixing mill is started to stir for 10min, so that the bonding agent is uniformly adhered to the surfaces of the corundum particles and is wetted with the corundum particles, the premixed fine powder obtained in the step one is added, and the stirring is carried out for 20min, so that the materials are fully and uniformly mixed;
step three, putting the mixed materials into a sealing bag, and placing the sealing bag in an air atmosphere with room temperature and air humidity of 50-60% for 12-24h for ageing;
after ageing, preparing the uniformly mixed materials into standard brick blanks of 65mm multiplied by 114mm multiplied by 230mm by a hydraulic machine under the pressure of 120MPa, and drying the formed brick blanks in a drying oven at the temperature of 120 ℃ for 24 hours;
and fifthly, weighing the dried sample, conveying the sample into a nitriding furnace, introducing nitrogen into a sealed furnace door, heating to 1100 ℃ at a heating rate of 5-8 ℃/min under the micro-positive pressure flowing nitrogen atmosphere, preserving heat for 2 hours, heating to 1450 ℃ at a rate of 1-5 ℃/min, preserving heat for 24 hours, and cooling to room temperature along with the furnace to obtain the corundum-silicon oxynitride composite refractory material.
The performance indexes of the obtained product are as follows: apparent porosity: 16.3%, bulk density: 3.08g/cm3Normal temperature compressive strength: 182MPa, normal-temperature breaking strength: 27MPa, thermal rupture strength at 1400 ℃: about 20MPa, according to YB/T376.1-1995 standard 1100 ℃ -water cooling times: 42 times, room-temperature dielectric constant: 8.17, dielectric loss tangent:0.0014, good wave permeability. The results of the anti-corrosion experiment show that the anti-corrosion effect on the nickel-iron ore is the best.
Example 2:
firstly, 18 parts of corundum fine powder and SiO25 parts of powder, SiO2The method comprises the following steps of putting 10 parts of Si powder with the particle size of 2-3 mu m into a ball mill, and premixing for 50 minutes at the rotating speed of 1000-1200 rpm according to the proportion of corundum balls to materials of 1:1 to obtain premixed fine powder;
step two, pouring 45 parts of corundum aggregate with the granularity of 3-1mm and 22 parts of corundum aggregate with the granularity of 1-0mm into a mixing mill, and then adding 5 parts of corundum aggregatewt% of the bonding agent is started, the mixing mill is started to stir for 5min, so that the bonding agent is uniformly adhered to the surfaces of the corundum particles and is wetted with the corundum particles, the premixed fine powder obtained in the step one is added, and the stirring is carried out for 10min, so that the materials are fully and uniformly mixed;
step three, putting the mixed materials into a sealed bag, and placing the sealed bag in an air atmosphere with room temperature and air humidity of 50-60% for 12-24h for ageing;
after ageing, preparing the uniformly mixed materials into standard brick blanks of 65mm multiplied by 114mm multiplied by 230mm by a hydraulic machine under the pressure of 120MPa, and drying the formed brick blanks in a drying oven at the temperature of 120 ℃ for 24 hours;
and fifthly, weighing the dried sample, conveying the sample into a nitriding furnace, introducing nitrogen into a sealed furnace door, heating to 1100 ℃ at a heating rate of 5-8 ℃/min under the micro-positive pressure flowing nitrogen atmosphere, preserving heat for 2 hours, heating to 1450 ℃ at a rate of 1-5 ℃/min, preserving heat for 24 hours, and cooling to room temperature along with the furnace to obtain the corundum-silicon oxynitride composite refractory material.
The performance indexes of the obtained product are as follows: apparent porosity: 16.0%, bulk density: 3.00g/cm3Normal temperature compressive strength: 172.91MPa, normal temperature breaking strength: 25.62MPa, hot rupture strength at 1400 ℃: about 24.27MPa, 1100 ℃ water cooling times according to YB/T376.1-1995 standard, 35 times, and the dielectric constant at normal temperature: 9.14, dielectric loss tangent: 0.0033, has good wave permeability. Has good effect of resisting the erosion of the ferronickel ore material smelted by microwave,
example 3:
the first step,Firstly 25 portions of corundum fine powder and SiO2Powder 6 parts, SiO2The method comprises the following steps of putting 14 parts of Si powder with the particle size of 5-10 mu m into a ball mill, and premixing for 40 minutes at the rotating speed of 1000-1200 rpm according to the proportion of corundum balls to materials of 1:1 to obtain premixed fine powder;
step two, pouring 30 parts of corundum aggregate with the granularity of 3-1mm and 25 parts of corundum aggregate with the granularity of 1-0mm into a mixing mill, and then adding 6 parts of corundum aggregatewt% of the bonding agent is started, the mixing mill is started to stir for 10min, so that the bonding agent is uniformly adhered to the surfaces of the corundum particles and is wetted with the corundum particles, the premixed fine powder obtained in the step one is added, and the stirring is carried out for 20min, so that the materials are fully and uniformly mixed;
step three, putting the mixed materials into a sealing bag, and placing the sealing bag in an air atmosphere with the air humidity of 50-60% for 12-24h for ageing;
after ageing, preparing the uniformly mixed materials into standard brick blanks of 65mm multiplied by 114mm multiplied by 230mm by a hydraulic machine under the pressure of 120MPa, and drying the formed brick blanks in a drying oven at the temperature of 120 ℃ for 48 hours;
and fifthly, weighing the dried sample, conveying the sample into a nitriding furnace, introducing nitrogen into a sealed furnace door, heating to 1100 ℃ at a heating rate of 5-8 ℃/min under the micro-positive pressure flowing nitrogen atmosphere, preserving heat for 2 hours, heating to 1450 ℃ at a rate of 1-5 ℃/min, preserving heat for 24 hours, and cooling to room temperature along with the furnace to obtain the corundum-silicon oxynitride composite refractory material.
The performance indexes of the obtained product are as follows: apparent porosity: 16.4%, bulk density: 3.06g/cm3Normal temperature compressive strength: 190.90MPa, normal temperature breaking strength: 28.09MPa, thermal rupture strength at 1400 ℃: about 22.06MPa, 1100 ℃ water cooling times according to YB/T376.1-1995 standard, 27 times, and a room-temperature dielectric constant: 8.72, dielectric loss tangent: 0.0018, has the best wave permeability. The effect of resisting the erosion of the ferronickel ore material smelted by microwave is good.

Claims (3)

1. A corundum-silicon oxynitride composite refractory material for a microwave metallurgical kiln car is characterized in that the raw materials are added in parts by weight: 30-45 parts of corundum aggregate with the granularity of 3-1mm, 20-25 parts of corundum aggregate with the granularity of 1-0mm, and steelJade fine powder 15-25 parts, SiO23-6 parts of micro powder, 10-15 parts of Si powder, and the addition amount of a bonding agent is 3-6% of the total weight of the raw material; SiO 22The micro powder is one or more than two of superfine natural quartz sand powder, silicon micro powder and gas-phase silicon oxide micro powder; SiO 22The purity of the micro powder is more than or equal to 98 percent, the grain diameter is less than 10 mu m, the purity of the Si powder is more than or equal to 99 percent, the grain size is less than or equal to 0.045mm, the main crystal phases of the corundum-silicon oxynitride composite refractory material are corundum and silicon oxynitride, and β -Si is contained in the matrix3N4β -Sialon and O' -Sialon crystalline phases.
2. The corundum-silicon oxynitride composite refractory material for the microwave metallurgical kiln car as claimed in claim 1, wherein: the binder is one or more of phenolic resin, dextrin, polyvinyl alcohol, carboxymethyl cellulose and pulp waste liquid.
3. The preparation method of the corundum-silicon oxynitride composite refractory material for the microwave metallurgical kiln car according to claim 1, characterized by comprising the following steps: firstly, 15-25 parts of corundum fine powder and SiO23-6 parts of micro powder and 10-15 parts of Si powder, and grinding the mixture in a ball mill for 180 minutes at the rotation speed of 1000-1200 rpm according to the proportion of corundum balls to materials of 1:1 to obtain premixed fine powder; step two, pouring 30-45 parts of corundum aggregate with the granularity of 3-1mm and 20-25 parts of corundum aggregate with the granularity of 1-0mm into a mixing mill, and then adding 3-6 parts of corundum aggregatewtMixing binder, stirring for 5-10min to make binder uniformly adhere to the surface of corundum granule and wet it, adding the premixed fine powder obtained in step one, stirring for 10-20min to make the material be fully mixed; step three, putting the mixed materials into a sealed bag, and placing the sealed bag for 12-24h in an air atmosphere with the air humidity of 50-60% at room temperature; after ageing, preparing the uniformly mixed materials into green bricks by using a hydraulic press under the pressure of 120MPa, and drying the formed green bricks in a drying oven at the temperature of 120 ℃ for 24 hours; step five, weighing the dried sample, conveying the sample into a nitriding furnace, introducing nitrogen into a sealed furnace door, heating to 1100 ℃ at a heating rate of 5-8 ℃/min under the micro-positive pressure flowing nitrogen atmosphere, preserving heat for 2 hours, and then heating at a heating rate of 1-5 ℃/minAnd (3) keeping the temperature at 1450 ℃ for 24 hours, and then cooling the mixture to room temperature along with the furnace to obtain the corundum-silicon oxynitride composite refractory material.
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