CN114213131B - Silicon carbide roller material for roller kiln and preparation method thereof - Google Patents

Silicon carbide roller material for roller kiln and preparation method thereof Download PDF

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CN114213131B
CN114213131B CN202210159922.1A CN202210159922A CN114213131B CN 114213131 B CN114213131 B CN 114213131B CN 202210159922 A CN202210159922 A CN 202210159922A CN 114213131 B CN114213131 B CN 114213131B
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silicon carbide
roller
granularity
micro powder
blank
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CN114213131A (en
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刘桂荣
苏国平
刘新元
苏浩然
胡振华
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Dinggu New Material Tianjin Co ltd
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Abstract

The application provides a carborundum roller rod material for roller kiln and a preparation method thereof, which belongs to the technical field of ceramic materials, and the hot isostatic pressing treatment is carried out on sintered blanks, so that the density of the roller rod material is further improved, and the roller rod material is prepared from the following components in percentage by mass: 8-14% of first-granularity silicon carbide micro powder, 8-20% of second-granularity silicon carbide micro powder, 30-40% of third-granularity silicon carbide micro powder, 20-40% of fourth-granularity silicon carbide micro powder, 2-8% of carbon black and 2-8% of graphite. The density of the silicon carbide roller rod material for the roller kiln prepared by the method is 3.02-3.08 g/cm3The material has the characteristics of room-temperature bending strength of 260-304 MPa, 1200-temperature bending strength of 300-330 MPa, service life of more than 12 months, high density, high bending strength, small amount of free silicon, low porosity and long service life, and is simple in preparation process and suitable for batch production.

Description

Silicon carbide roller material for roller kiln and preparation method thereof
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a silicon carbide roller rod material for a roller kiln and a preparation method thereof.
Background
The roller is a key refractory material in a roller kiln and plays a role in bearing and conveying products in the kiln. With the development of ceramic industry and new energy industry, roller kilns have a lot of extensive applications in architectural ceramics, sanitary ceramics, household ceramics and special ceramics, lithium batteries and photovoltaic industry, the requirements for roller rod materials used in the kilns are continuously improved, and especially the requirements for the strength and high-temperature mechanical properties of the roller rods are updated. The traditional alumina ceramic roller rod cannot meet the use requirement of high-load working conditions due to the limitations of poor thermal shock resistance stability, easy cracking at high temperature, use temperature and the like of the material. In patent CN1287987A, silicon carbide, aluminum oxide, silicon oxide and magnesium oxide are used as raw materials, and the roller rod material is low in density and strength and short in service life by adopting extrusion and vacuum sintering modes.
Disclosure of Invention
In view of the above defects or shortcomings in the prior art, the present application aims to provide a silicon carbide roller rod material for a roller kiln and a preparation method thereof, so as to solve the problems of low density, low bending strength and short service life of the silicon carbide roller rod for the roller kiln, and better meet the use requirements of the silicon carbide roller rod for the roller kiln.
In a first aspect, the application provides a method for preparing a silicon carbide roller material for a roller kiln, which is used for carrying out hot isostatic pressing treatment on a sintered blank after reaction sintering.
Specifically, in the conventional reaction sintering process, liquid silicon infiltrates into the preform under the action of capillary force at high temperature, reacts with carbon in the preform to generate silicon carbide, and in-situ bonds with silicon carbide micro powder particles in the preform, but the infiltrated silicon cannot completely react, and a part of residual silicon still exists in the sintered blank and exists in the sintered blank in the form of free silicon. And the hot isostatic pressing treatment is carried out on the sintered blank by using a hot isostatic pressing machine, and the main functions comprise two aspects: firstly, under the conditions of high temperature and high pressure, the residual free silicon in the sintered blank can react with the residual carbon to generate silicon carbide, thereby further reducing the amount of the free silicon; and secondly, under the action of hot isostatic pressing, micropores in the sintered blank can be compressed and densified, so that the density of the silicon carbide roller material is further improved, and the service life of the roller material under a high-temperature condition is further prolonged.
Preferably, the preparation method comprises the following steps:
adding a binder into the uniformly mixed raw material powder, and stirring, refining and ageing to obtain pug;
extruding the pug to obtain an extrusion blank, and drying to obtain a prefabricated blank;
performing reaction sintering on the prefabricated blank to obtain a sintered blank;
and carrying out hot isostatic pressing treatment on the sintered blank to obtain the roller material.
Preferably, the hot isostatic pressing treatment temperature is 1300-1500 ℃, the treatment pressure is 120MPa, and the heat preservation and pressure maintaining are carried out for 1-3 h.
Preferably, the hot isostatic pressing is performed under an argon atmosphere.
Preferably, the raw material powder comprises, by mass, 8-14% of first-particle-size silicon carbide micro powder with a particle size of 3.5-4 μm, 8-20% of second-particle-size silicon carbide micro powder with a particle size of 9-10 μm, 30-40% of third-particle-size silicon carbide micro powder with a particle size of 48-50 μm, 20-40% of fourth-particle-size silicon carbide micro powder with a particle size of 98-100 μm, 2-8% of 20-50 nm carbon black, 2-8% of 2.5-3.2 μm graphite, and the balance unavoidable impurities.
Specifically, the particle sizes of the first particle size silicon carbide micro powder, the second particle size silicon carbide micro powder, the third particle size silicon carbide micro powder and the fourth particle size silicon carbide micro powder are all fisher particle sizes. The silicon carbide micro powder with different granularity levels is matched, the contact distance between the silicon carbide micro powder can be reduced after mixing, the porosity and the pore size of the raw material powder are reduced, and then the silicon carbide is generated by adding micron-sized graphite and nano-sized carbon black to react with the embedded silicon powder. The newly generated silicon carbide is in-situ combined with silicon carbide micro powder particles in situ in the prefabricated blank, and the residual free silicon in the sintered blank reacts with free carbon under high temperature and high pressure through the post-stage hot isostatic pressing treatment, so that the content of the free silicon is reduced, and in addition, the quantity of micropores in the sintered blank is further reduced through the hot isostatic pressing treatment, so that the sintering density of the final silicon carbide roller rod material is improved.
Preferably, the binder is an aqueous solution of polyvinylpyrrolidone.
Specifically, after the polyvinylpyrrolidone aqueous solution is added into the raw material powder, stirring is carried out for 3-6 hours, and then aging is carried out for 12 hours.
Preferably, the polyvinylpyrrolidone aqueous solution consists of polyvinylpyrrolidone with a mass accounting for 10% of the mass of the raw material powder and deionized water with a mass accounting for 15% of the mass of the raw material powder in percentage by mass.
Preferably, the relative density of the extrusion blank is 60-70%.
Specifically, the extrusion blank is dried for 10-15 hours at the temperature of 40-120 ℃ to obtain the prefabricated blank.
Preferably, in the step of reaction sintering the preform to obtain a sintered blank, the preform is first embedded with silicon powder, and then reaction sintering is performed in a vacuum atmosphere.
Specifically, the prefabricated blank is embedded with silicon powder, placed into a sintering furnace, vacuumized, kept at 1600-1750 ℃ for 2-4 hours, and taken out to obtain a sintered blank. In the sintering process, the silicon powder is melted into liquid at 1600-1750 ℃, the liquid silicon is infiltrated into the carbon-containing prefabricated blank under the action of high-temperature capillary force and reacts with carbon to generate silicon carbide, the newly generated silicon carbide is in-situ combined with silicon carbide micro powder particles in the prefabricated blank, and finally the silicon is infiltrated to fill residual holes in the prefabricated blank, so that the densification process is completed.
In a second aspect, the application provides a silicon carbide roller rod material for a roller kiln, which is prepared from the following components in percentage by mass: 8-14% of first-granularity silicon carbide micro powder with the granularity of 3.5-4 mu m, 8-20% of second-granularity silicon carbide micro powder with the granularity of 9-10 mu m, 30-40% of third-granularity silicon carbide micro powder with the granularity of 48-50 mu m, 20-40% of fourth-granularity silicon carbide micro powder with the granularity of 98-100 mu m, 2-8% of 20-50 nm carbon black, 2-8% of 2.5-3.2 mu m graphite and the balance of inevitable impurities.
Specifically, the granularity of the carbon black is nano-scale and fine, the graphite is micron-scale and coarse, and after the carbon black and the liquid silicon react, the formed silicon carbide particles have different sizes, so that the material particles can be reasonably matched, the density is higher, and the strength is higher.
In conclusion, the application discloses a silicon carbide roller rod material for roller kiln and a preparation method thereof, based on the scheme, the silicon carbide roller rod material has the advantages that the hot isostatic pressing treatment is carried out on the sintered blank obtained after sintering, the quantity of free silicon in the sintered blank is further reduced, the porosity inside the sintered blank is reduced, the density of the silicon carbide roller rod material is improved, the room-temperature and high-temperature bending strength of the roller rod material is improved, the service life of the roller rod made of the roller rod material for roller kiln is further prolonged,and 4 kinds of silicon carbide micro powder with different particle sizes are matched to prepare the silicon carbide roller material, so that the contact distance between the adjacent silicon carbide micro powder can be fully reduced, the porosity and the pore size of the material are reduced, and the density of a sintered blank is improved. The silicon carbide roller material prepared by the method has the density of 3.02-3.08 g/cm through detection3The room-temperature bending strength is 260-304 MPa, the 1200 ℃ bending strength is 300-330 MPa, the service life is more than 12 months, and the silicon carbide roller rod has the characteristics of high density, small quantity of free silicon, low porosity, high bending strength and long service life, can better meet the use requirement of the silicon carbide roller rod for the roller kiln, solves the problems of low density, low bending strength, short service life and the like of the silicon carbide roller rod for the roller kiln, and is simple in preparation process and suitable for batch production.
This application still has following advantage:
(1) the preparation raw materials adopt the conventional silicon carbide micro powder, graphite powder and carbon black powder with different granularities, and are easy to purchase in the market;
(2) the preparation process is a powder metallurgy process, and is simple and easy to operate;
(3) the prepared silicon carbide roller material for the roller kiln has no elements harmful to the environment in the components, does not cause environmental pollution, has simple preparation process and is suitable for batch production.
Drawings
FIG. 1 is a flow chart of a process for preparing a silicon carbide roller material for a roller kiln.
Fig. 2 is a microstructure diagram of a silicon carbide roller rod material for a roller kiln, which is 100 times as large as that in example 1 of the present application.
Fig. 3 is a microstructure diagram of a silicon carbide roller rod material for a roller kiln according to example 1 of the present application, which is 1000 times larger than the above.
FIG. 4 is a microstructure diagram of a silicon carbide roller rod material for roller kilns of comparative example 1 according to the present application at 1000 times.
FIG. 5 is a microstructure diagram of a silicon carbide roller rod material used for roller kilns in comparative example 2 of the present application, which is 1000 times.
Detailed Description
The present application will be described in further detail with reference to examples. It is to be understood that the specific embodiments described herein are merely illustrative of the application and are not limiting of the application. Unless defined otherwise, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The present application will be described in detail with reference to examples.
Example 1
A silicon carbide roller material for a roller kiln is prepared from the following components in percentage by mass: 8% of first-granularity silicon carbide micro powder with the granularity of 3.5-4 mu m, 8% of second-granularity silicon carbide micro powder with the granularity of 9-10 mu m, 40% of third-granularity silicon carbide micro powder with the granularity of 48-50 mu m, 40% of fourth-granularity silicon carbide micro powder with the granularity of 98-100 mu m, 2% of carbon black with the granularity of 20-50 nm, 2% of graphite with the granularity of 2.5-3.2 mu m and the balance of inevitable impurities.
The preparation process flow of the roller material is shown in figure 1, and the specific preparation process comprises the following steps:
preparing raw materials:
putting the first-granularity silicon carbide micro powder, the second-granularity silicon carbide micro powder, the third-granularity silicon carbide micro powder, the fourth-granularity silicon carbide micro powder, the carbon black and the graphite into a mixer, stirring and mixing for 3 hours to obtain raw material powder, then pouring the raw material powder into a kneader, adding polyvinylpyrrolidone aqueous solution consisting of 10% by mass of polyvinylpyrrolidone and 15% by mass of deionized water, stirring and mixing for 3 hours in the kneader, then pouring into a pug mill for refining, and aging for 12 hours to obtain pug for extrusion;
extrusion forming:
putting the pug into an extruder, selecting a proper die according to the required size, extruding the pug by the extruder to prepare an extrusion blank with the required shape, wherein the relative density of the extrusion blank is 60%, and drying the extrusion blank at 40 ℃ for 10h to obtain a prefabricated blank;
reaction sintering:
embedding the prefabricated blank into silicon powder, putting the prefabricated blank into a sintering furnace, vacuumizing and heating to 1600 ℃, and then preserving heat for 2 hours to enable the prefabricated blank to react and sinter in a vacuum atmosphere to obtain a sintered blank;
hot isostatic pressing treatment:
and (3) placing the sintered blank into a hot isostatic pressing machine, filling argon, heating to 1300 ℃, pressurizing to 120MPa, and keeping the temperature and pressure of the sintered blank for 1h under the argon atmosphere to obtain the silicon carbide roller rod material for processing and manufacturing the roller rod for the roller kiln.
The test shows that the density of the roller material is 3.02g/cm3The room-temperature bending strength was 260MPa, the 1200 ℃ bending strength was 300MPa, and the microstructure thereof is shown in FIGS. 2 and 3, and it can be seen that the pores completely disappeared after the hot isostatic pressing treatment. The content of free silicon is 8 percent, the porosity is 0, and both the content of free silicon and the porosity are superior to the GB/T21944.3-2008 standard requirements. Through practical use tests, the service life of the silicon carbide roller rod made of the roller rod material prepared by the process reaches 12-15 months.
Example 2
A silicon carbide roller material for a roller kiln is prepared from the following components in percentage by mass: 14% of first-granularity silicon carbide micro powder with the granularity of 3.5-4 mu m, 20% of second-granularity silicon carbide micro powder with the granularity of 9-10 mu m, 30% of third-granularity silicon carbide micro powder with the granularity of 48-50 mu m, 20% of fourth-granularity silicon carbide micro powder with the granularity of 98-100 mu m, 8% of carbon black with the granularity of 20-50 nm, 8% of graphite with the granularity of 2.5-3.2 mu m and the balance of inevitable impurities.
The preparation process flow of the roller material is shown in figure 1, and the specific preparation process comprises the following steps:
preparing raw materials:
putting the first-granularity silicon carbide micro powder, the second-granularity silicon carbide micro powder, the third-granularity silicon carbide micro powder, the fourth-granularity silicon carbide micro powder, the carbon black and the graphite into a mixer, stirring and mixing for 5 hours to obtain raw material powder, then pouring the raw material powder into a kneader, adding polyvinylpyrrolidone aqueous solution consisting of 10% by mass of polyvinylpyrrolidone and 15% by mass of deionized water, stirring and mixing for 6 hours in the kneader, then pouring into a pug mill for refining, and aging for 12 hours to obtain pug for extrusion;
extrusion molding:
putting the pug into an extruder, selecting a proper die according to the required size, extruding the pug by the extruder to prepare an extrusion blank with the required shape, wherein the relative density of the extrusion blank is 70%, and drying the extrusion blank at 100 ℃ for 15h to obtain a prefabricated blank;
reaction sintering:
embedding the prefabricated blank into silicon powder, putting the prefabricated blank into a sintering furnace, vacuumizing and heating to 1750 ℃, and then preserving heat for 4 hours to enable the prefabricated blank to react and sinter in a vacuum atmosphere to obtain a sintered blank;
hot isostatic pressing treatment:
and (3) putting the sintered blank into a hot isostatic pressing machine, filling argon, heating to 1500 ℃, pressurizing to 120MPa, and keeping the temperature and pressure of the sintered blank for 3 hours under the argon atmosphere to obtain the silicon carbide roller rod material for processing and manufacturing the roller rod for the roller kiln.
The test shows that the density of the roller material is 3.08g/cm3The room-temperature bending strength was 304MPa, the 1200 ℃ bending strength was 330MPa, and the microstructure was similar to that of example 1 and was not repeated. The content of free silicon is 6 percent, the porosity is 0, and both the content of free silicon and the porosity are superior to the requirements of GB/T21944.3-2008 standard.
Example 3
A silicon carbide roller material for a roller kiln is prepared from the following components in percentage by mass: 10% of first-granularity silicon carbide micro powder with the granularity of 3.5-4 mu m, 15% of second-granularity silicon carbide micro powder with the granularity of 9-10 mu m, 35% of third-granularity silicon carbide micro powder with the granularity of 48-50 mu m, 30% of fourth-granularity silicon carbide micro powder with the granularity of 98-100 mu m, 5% of carbon black with the granularity of 20-50 nm, 5% of graphite with the granularity of 2.5-3.2 mu m and the balance of inevitable impurities.
The preparation process flow of the roller material is shown in figure 1, and the specific preparation process comprises the following steps:
preparing raw materials:
putting the first-granularity silicon carbide micro powder, the second-granularity silicon carbide micro powder, the third-granularity silicon carbide micro powder, the fourth-granularity silicon carbide micro powder, the carbon black and the graphite into a mixer, stirring and mixing for 4 hours to obtain raw material powder, then pouring the raw material powder into a kneader, adding polyvinylpyrrolidone aqueous solution consisting of 10% by mass of polyvinylpyrrolidone and 15% by mass of deionized water, stirring and mixing for 4 hours in the kneader, then pouring into a pug mill for refining, and aging for 12 hours to obtain pug for extrusion;
extrusion molding:
putting the pug into an extruder, selecting a proper die according to the required size, extruding the pug by the extruder to prepare an extrusion blank with the required shape, wherein the relative density of the extrusion blank is 65%, and drying the extrusion blank at 80 ℃ for 12h to obtain a prefabricated blank;
reaction sintering:
embedding the prefabricated blank into silicon powder, putting the prefabricated blank into a sintering furnace, vacuumizing and heating to 1650 ℃, and then preserving heat for 3 hours to enable the prefabricated blank to react and sinter in a vacuum atmosphere to obtain a sintered blank;
hot isostatic pressing treatment:
and (3) putting the sintered blank into a hot isostatic pressing machine, filling argon, heating to 1400 ℃, pressurizing to 120MPa, and keeping the temperature and pressure of the sintered blank for 2 hours under the argon atmosphere to obtain the silicon carbide roller rod material for processing and manufacturing the roller rod for the roller kiln.
The test shows that the density of the roller rod material is 3.04g/cm3The room-temperature bending strength was 300MPa, the 1200 ℃ bending strength was 330MPa, and the microstructure was similar to that of example 1 and was not repeated. The content of free silicon is 7%, the porosity is less than 0, and both the content of free silicon and the porosity are superior to the requirements of GB/T21944.3-2008 standard.
Example 4
A silicon carbide roller material for a roller kiln is prepared from the following components in percentage by mass: 12% of first-particle-size silicon carbide micro powder with the particle size of 3.5-4 mu m, 13% of second-particle-size silicon carbide micro powder with the particle size of 9-10 mu m, 32% of third-particle-size silicon carbide micro powder with the particle size of 48-50 mu m, 33% of fourth-particle-size silicon carbide micro powder with the particle size of 98-100 mu m, 6% of carbon black with the particle size of 20-50 nm, 4% of graphite with the particle size of 2.5-3.2 mu m and the balance of inevitable impurities.
The preparation process flow of the roller material is shown in figure 1, and the specific preparation process comprises the following steps:
preparing raw materials:
putting the first-granularity silicon carbide micro powder, the second-granularity silicon carbide micro powder, the third-granularity silicon carbide micro powder, the fourth-granularity silicon carbide micro powder, the carbon black and the graphite into a mixer, stirring and mixing for 3.5 hours to obtain raw material powder, then pouring the raw material powder into a kneader, adding polyvinylpyrrolidone aqueous solution consisting of 10% by mass of polyvinylpyrrolidone and 15% by mass of deionized water, stirring and mixing for 5 hours in the kneader, then pouring into a pugging machine for refining, and aging for 12 hours after refining to obtain pug for extrusion;
extrusion molding:
putting the pug into an extruder, selecting a proper die according to the required size, extruding the pug by the extruder to prepare an extrusion blank with the required shape, wherein the relative density of the extrusion blank is 64%, and drying the extrusion blank at 90 ℃ for 14h to obtain a prefabricated blank;
reaction sintering:
embedding the prefabricated blank into silicon powder, putting the prefabricated blank into a sintering furnace, vacuumizing and heating to 1700 ℃, and then preserving heat for 3.5 hours to enable the prefabricated blank to react and sinter in a vacuum atmosphere to obtain a sintered blank;
hot isostatic pressing treatment:
and (3) putting the sintered blank into a hot isostatic pressing machine, filling argon, heating to 1450 ℃, pressurizing to 120MPa, and keeping the temperature and pressure of the sintered blank for 2.5 hours in the argon atmosphere to obtain the silicon carbide roller rod material for processing and manufacturing the roller rod for the roller kiln.
The test shows that the density of the roller rod material is 3.05g/cm3Room temperature bending strength of 280MPa, a flexural strength at 1200 ℃ of 320MPa, a microstructure similar to that of example 1 and not repeated. The content of free silicon is 6 percent, the porosity is 0, and both the content of free silicon and the porosity are superior to the requirements of GB/T21944.3-2008 standard.
Example 5
A silicon carbide roller material for a roller kiln is prepared from the following components in percentage by mass: 13% of first-particle-size silicon carbide micro powder with the particle size of 3.5-4 mu m, 12% of second-particle-size silicon carbide micro powder with the particle size of 9-10 mu m, 33% of third-particle-size silicon carbide micro powder with the particle size of 48-50 mu m, 32% of fourth-particle-size silicon carbide micro powder with the particle size of 98-100 mu m, 4% of carbon black with the particle size of 20-50 nm, 6% of graphite with the particle size of 2.5-3.2 mu m and the balance of inevitable impurities.
The preparation process flow of the roller material is shown in figure 1, and the specific preparation process comprises the following steps:
preparing raw materials:
putting the first-granularity silicon carbide micro powder, the second-granularity silicon carbide micro powder, the third-granularity silicon carbide micro powder, the fourth-granularity silicon carbide micro powder, the carbon black and the graphite into a mixer, stirring and mixing for 4.5 hours to obtain raw material powder, then pouring the raw material powder into a kneader, adding polyvinylpyrrolidone aqueous solution consisting of 10% by mass of polyvinylpyrrolidone and 15% by mass of deionized water, stirring and mixing for 3.5 hours in the kneader, then pouring into a pug mill for refining, and aging for 12 hours after refining to obtain pug for extrusion;
extrusion molding:
putting the pug into an extruder, selecting a proper die according to the required size, extruding the pug by the extruder to prepare an extrusion blank with the required shape, wherein the relative density of the extrusion blank is 68%, and drying the extrusion blank at 120 ℃ for 12h to obtain a prefabricated blank;
reaction sintering:
embedding the prefabricated blank into silicon powder, putting the prefabricated blank into a sintering furnace, vacuumizing and heating to 1680 ℃, and then preserving heat for 4 hours to enable the prefabricated blank to react and sinter in a vacuum atmosphere to obtain a sintered blank;
hot isostatic pressing treatment:
and (3) putting the sintered blank into a hot isostatic pressing machine, filling argon, heating to 1500 ℃, pressurizing to 120MPa, and keeping the temperature and pressure of the sintered blank for 3 hours under the argon atmosphere to obtain the silicon carbide roller rod material for processing and manufacturing the roller rod for the roller kiln.
The test shows that the density of the roller material is 3.06g/cm3The room-temperature bending strength was 300MPa, the 1200 ℃ bending strength was 330MPa, and the microstructure was similar to that of example 1 and was not repeated. The content of free silicon is 6.5 percent, the porosity is 0, and the content of free silicon and the porosity are both superior to the requirements of GB/T21944.3-2008 standard.
Comparative example 1
A silicon carbide roller material for a roller kiln is prepared from the following components in percentage by mass: 8% of first-granularity silicon carbide micro powder with the granularity of 3.5-4 mu m, 8% of second-granularity silicon carbide micro powder with the granularity of 9-10 mu m, 40% of third-granularity silicon carbide micro powder with the granularity of 48-50 mu m, 40% of fourth-granularity silicon carbide micro powder with the granularity of 98-100 mu m, 2% of carbon black with the granularity of 20-50 nm, 2% of graphite with the granularity of 2.5-3.2 mu m and the balance of inevitable impurities.
The preparation process comprises the following steps:
preparing raw materials:
putting the first-granularity silicon carbide micro powder, the second-granularity silicon carbide micro powder, the third-granularity silicon carbide micro powder, the fourth-granularity silicon carbide micro powder, the carbon black and the graphite into a mixer, stirring and mixing for 3 hours to obtain raw material powder, then pouring the raw material powder into a kneader, adding polyvinylpyrrolidone aqueous solution consisting of 10% by mass of polyvinylpyrrolidone and 15% by mass of deionized water, stirring and mixing for 3 hours in the kneader, then pouring into a pug mill for refining, and aging for 12 hours to obtain pug for extrusion;
extrusion forming:
putting the pug into an extruder, selecting a proper die according to the required size, extruding the pug by the extruder to prepare an extrusion blank with the required shape, wherein the relative density of the extrusion blank is 60%, and drying the extrusion blank at 40 ℃ for 10h to obtain a prefabricated blank;
reaction sintering:
embedding the prefabricated blank in silicon powder, putting the silicon powder into a sintering furnace, vacuumizing, heating to 1600 ℃, and then preserving heat for 2 hours to enable the prefabricated blank to react and sinter in a vacuum atmosphere to obtain the silicon carbide roller rod material for processing and manufacturing the roller rod for the roller kiln.
The test shows that the density of the roller material is 3.00g/cm3The room-temperature bending strength was 220MPa, the 1200 ℃ bending strength was 260MPa, the free silicon content was 14%, the porosity was 0.3%, and the microstructure thereof is shown in FIG. 4. Through practical use tests, the service life of the silicon carbide roller rod made of the roller rod material prepared by the process is 8 months.
Comparative example 2
A silicon carbide roller material for a roller kiln is prepared from the following components in percentage by mass: 18% of first-granularity silicon carbide micro powder with the granularity of 3.5-4 mu m, 18% of second-granularity silicon carbide micro powder with the granularity of 9-10 mu m, 60% of third-granularity silicon carbide micro powder with the granularity of 48-50 mu m, 2% of carbon black with the granularity of 20-50 nm, 2% of graphite with the granularity of 2.5-3.2 mu m and the balance of inevitable impurities.
The preparation process comprises the following steps:
preparing raw materials:
putting the first-granularity silicon carbide micro powder, the second-granularity silicon carbide micro powder, the third-granularity silicon carbide micro powder, the carbon black and the graphite into a mixer, stirring and mixing for 3 hours to obtain raw material powder, then pouring the raw material powder into a kneader, adding polyvinylpyrrolidone aqueous solution consisting of 10% by mass of polyvinylpyrrolidone and 15% by mass of deionized water, stirring and mixing for 3 hours in the kneader, then pouring into a pug mill, refining, and aging for 12 hours to obtain pug for extrusion;
extrusion molding:
putting the pug into an extruder, selecting a proper die according to the required size, extruding the pug by the extruder to prepare an extrusion blank with the required shape, wherein the relative density of the extrusion blank is 60%, and drying the extrusion blank at 40 ℃ for 10h to obtain a prefabricated blank;
reaction sintering:
burying the prefabricated blank in silicon powder, putting the prefabricated blank into a sintering furnace, vacuumizing and heating to 1600 ℃, and then preserving heat for 2 hours to enable the prefabricated blank to react and sinter in a vacuum atmosphere to obtain a sintered blank;
hot isostatic pressing treatment:
and (3) placing the sintered blank into a hot isostatic pressing machine, filling argon, heating to 1300 ℃, pressurizing to 120MPa, and keeping the temperature and pressure of the sintered blank for 1h under the argon atmosphere to obtain the silicon carbide roller rod material for processing and manufacturing the roller rod for the roller kiln.
The test shows that the density of the roller material is 3.01g/cm3The room-temperature bending strength was 230MPa, the 1200 ℃ bending strength was 280MPa, the free silicon content was 10%, the porosity was 0.1%, and the microstructure thereof is shown in FIG. 5. Through practical use tests, the service life of the silicon carbide roller rod manufactured by purchasing the roller rod material prepared by the process is 9 months.
Comparing and analyzing the example 1 and the comparative example 1, it can be seen that, under the same raw material and mixture ratio conditions, the silicon carbide roll rod material of the comparative example 1, which is only subjected to reaction sintering and not subjected to hot isostatic pressing treatment, has lower density, room temperature bending strength and high temperature bending strength than the silicon carbide roll rod material of the example 1, which is subjected to hot isostatic pressing treatment, and higher free silicon content and porosity than the silicon carbide roll rod material of the example 1, which is subjected to hot isostatic pressing treatment, and the service life of the silicon carbide roll rod material of the comparative example 1, which is not subjected to hot isostatic pressing treatment, is 8 months and is obviously lower after time test. The hot isostatic pressing treatment method is characterized in that the hot isostatic pressing treatment is carried out on the roll rod material, and the hot isostatic pressing treatment is carried out on the roll rod material.
Comparing and analyzing the example 1 and the comparative example 2, it can be seen that, under the same conditions of the preparation process, the comparative example 2 adopts 3 kinds of grain sizes of silicon carbide micro powder to prepare the silicon carbide roller rod material, because the grain size components of silicon carbide are changed, the density, room temperature bending strength and high temperature bending strength of the prepared roller rod material are all lower than those of the silicon carbide roller rod material prepared by adopting 4 kinds of grain sizes of silicon carbide micro powder in the example 1, and the free silicon content and the porosity are also higher than those of the silicon carbide roller rod material prepared in the example 1, and after the time test, the service life of the silicon carbide roller rod material prepared in the comparative example 2 is 9 months and is obviously lower. The roller rod material prepared by the silicon carbide micro powder with 4 particle sizes has more excellent performance and greatly prolongs the service life under the same preparation process condition.
It can be seen from the above embodiments that, the application provides a carborundum roller rod material for roller kiln and preparation method thereof, through carrying out hot isostatic pressing to the sintering stock after obtaining the sintering, further reduced free silicon quantity in the sintering stock has reduced the inside porosity of sintering stock improves the density of carborundum roller rod material to improve the room temperature and the high temperature bending strength of roller rod material, and then improve and adopt the life of roller rod for roller kiln of roller rod material preparation, and adopt the carborundum miropowder collocation preparation carborundum roller rod material of 4 different granularities, can fully reduce the contact distance between the adjacent carborundum miropowder, thereby reduce porosity and the pore size of material, improve sintering stock density. The silicon carbide roller material prepared by the method has the density of 3.02-3.08 g/cm through detection3The room-temperature bending strength is 260-304 MPa, the 1200 ℃ bending strength is 300-330 MPa, the service life is more than 12 months, and the silicon carbide roller rod has the characteristics of high density, small quantity of free silicon, low porosity, high bending strength and long service life, can better meet the use requirement of the silicon carbide roller rod for the roller kiln, solves the problems of low density, low bending strength, short service life and the like of the silicon carbide roller rod for the roller kiln, and is simple in preparation process and suitable for batch production.
The above examples are given for the purpose of illustrating the present invention clearly and not for the purpose of limiting the same, and it will be apparent to those skilled in the art that many more modifications and variations can be made in the embodiments described above, and it is not intended to be exhaustive or to limit the invention to the precise forms disclosed.

Claims (10)

1. A preparation method of a silicon carbide roller rod material for a roller kiln is characterized in that a prefabricated blank is embedded by silicon powder and is sintered by reaction at 1600-1750 ℃; and carrying out hot isostatic pressing treatment on the sintered blank to reduce the content of free silicon in the sintered blank, wherein the hot isostatic pressing treatment temperature is 1300-1500 ℃, and the treatment pressure is 120 MPa.
2. The preparation method of the silicon carbide roller rod material for the roller kiln as claimed in claim 1, wherein the preparation method comprises the following steps:
adding a binder into the uniformly mixed raw material powder, and stirring, refining and ageing to obtain pug;
extruding the pug to obtain an extrusion blank, and drying to obtain a prefabricated blank;
performing reaction sintering on the prefabricated blank to obtain a sintered blank;
and carrying out hot isostatic pressing treatment on the sintered blank to obtain the roller material.
3. The method for preparing the silicon carbide roller rod material for the roller kiln according to the claim 1 or 2, characterized in that the hot isostatic pressing treatment is carried out for heat preservation and pressure maintaining for 1-3 h.
4. The method for preparing a silicon carbide roller rod material for a roller kiln as claimed in claim 1 or 2, wherein the hot isostatic pressing treatment is performed under an argon atmosphere.
5. The preparation method of the silicon carbide roller rod material for the roller kiln as claimed in claim 1 or 2, wherein the raw material powder comprises, by mass, 8-14% of a first-particle-size silicon carbide micro powder with a particle size of 3.5-4 μm, 8-20% of a second-particle-size silicon carbide micro powder with a particle size of 9-10 μm, 30-40% of a third-particle-size silicon carbide micro powder with a particle size of 48-50 μm, 20-40% of a fourth-particle-size silicon carbide micro powder with a particle size of 98-100 μm, 2-8% of 20-50 nm carbon black, 2.5-3.2 μm graphite, and the balance unavoidable impurities.
6. The method for preparing the silicon carbide roller rod material for the roller kiln as claimed in claim 2, wherein the binder is polyvinylpyrrolidone aqueous solution.
7. The method for preparing the silicon carbide roller rod material for the roller kiln, as recited in claim 6, wherein the polyvinylpyrrolidone aqueous solution is composed of polyvinylpyrrolidone with a mass of 10% of the mass of the raw material powder and deionized water with a mass of 15% of the mass of the raw material powder, in percentage by mass.
8. The method for preparing the silicon carbide roller rod material for the roller kiln as claimed in claim 2, wherein the relative density of the extrusion blank is 60-70%.
9. The method for preparing a silicon carbide roller rod material for a roller kiln as claimed in claim 2, wherein in the step of subjecting the preform to reaction sintering to obtain a sintered blank, the reaction sintering is performed in a vacuum atmosphere.
10. The silicon carbide roller material for the roller kiln is characterized by being prepared from the following components in percentage by mass: 8-14% of first-granularity silicon carbide micro powder with the granularity of 3.5-4 mu m, 8-20% of second-granularity silicon carbide micro powder with the granularity of 9-10 mu m, 30-40% of third-granularity silicon carbide micro powder with the granularity of 48-50 mu m, 20-40% of fourth-granularity silicon carbide micro powder with the granularity of 98-100 mu m, 2-8% of 20-50 nm carbon black, 2-8% of 2.5-3.2 mu m graphite and the balance of inevitable impurities; the preparation process of the roller material comprises the following steps: silicon powder is used for embedding the prefabricated blank, and reaction sintering is carried out at 1600-1750 ℃; and carrying out hot isostatic pressing treatment on the sintered blank to reduce the content of free silicon in the sintered blank, wherein the hot isostatic pressing treatment temperature is 1300-1500 ℃, and the treatment pressure is 120 MPa.
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