CN111072389B - SiC ceramic particle surface modification process - Google Patents
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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Abstract
The invention discloses a SiC ceramic particle surface modification process, which comprises the following steps: pretreating SiC particles; preparing surface modified slurry; and (5) surface modification treatment of the SiC particles. The process of the invention forms MoSi on the surface of SiC particles2A film of an intermetallic compound. The film can form Mo-Si-C bonds with SiC particles, and has good bonding property with the SiC particles. When the SiC particles after coating are made into a ceramic preform and then a casting method is adopted to prepare the SiC/Fe-based composite material, the wettability of the SiC particles and the molten iron alloy is good, and MoSi on the surfaces of the SiC particles2The film can inhibit harmful chemical reaction between molten iron and SiC particles, the SiC particles can form firm interface bonding with the iron alloy matrix, the SiC particles can not fall off from the surface of the iron alloy matrix due to low interface bonding strength under abrasion load, and the abrasion resistance of the SiC/Fe composite material can be improved by more than 50%.
Description
Technical Field
The invention relates to a surface modification process of SiC ceramic particles, in particular to a surface modification process of a SiC ceramic particle reinforcement body applied to preparation of an iron-based composite wear-resistant material, and belongs to the field of material surface modification.
Background
In cement production, it is necessary to crush and grind some high hardness minerals such as limestone, quartz sand, cement clinker, slag, etc. on a large scale. At present, most of core wear-resistant parts of crushing and grinding equipment in the cement industry, such as crusher hammers, jaw plates, ball mill lining plates, conical crushing mortar walls, vertical grinding discs, roller press grinding rollers and the like, still adopt single-performance metal wear-resistant materials, such as high-chromium cast iron, medium-chromium alloy steel, high-manganese steel and ultrahigh-manganese steel. For metal materials, the wear-resistant materials have excellent wear resistance, but because the hardness of mineral raw materials in cement production is higher than that of the existing metal wear-resistant materials, the wear-resistant parts are easy to wear out and lose efficacy early in the service process, and the working requirements of crushing and grinding equipment are difficult to meet. Taking the high-chromium cast iron hammer head of the medium-sized sandstone crusher as an example, 1 pair of hammer heads needs to be replaced after 2-4 months of working, thereby greatly reducing the working efficiency of the equipment and simultaneously increasing the labor intensity of workers.
In order to further improve the wear resistance of wear-resistant parts for the cement industry, a great deal of research and development work is carried out on strengthening iron-based alloy reinforced by tungsten carbide and titanium carbide particles in some foreign enterprises at present. The process is mainly to adopt a method of melting infiltration of a metal matrix, firstly to prepare ceramic particles of high-hardness carbide of titanium carbide or tungsten carbide into a porous blank, and then to infiltrate the porous blank under the vacuum condition after melting an iron matrix. Under the production conditions of the process, the ceramic particle titanium carbide or tungsten carbide has good associativity with an iron matrix, and can greatly improve the service life of the wear-resistant material, but the selling price of industrial grade tungsten carbide particles is more than 250 yuan/kg, the selling price of titanium carbide particles is more than 70 yuan/kg, and the price is high, so that the prepared carbide particle reinforced iron-based composite wear-resistant material has high selling price, and the popularization and the use are influenced. Compared with WC and TiC, the SiC ceramic is a high-hardness carbide ceramic, the hardness of the SiC ceramic is higher than that of WC and TiC, meanwhile, the contact angle between SiC particles and molten iron is 0 degree, the SiC particles can be well wetted by the molten iron, and the price of industrial-grade SiC particles is low and is about 15 yuan/kg. At present, SiC particles are often added into aluminum alloy in industry to improve the wear resistance of the aluminum matrix composite. However, when SiC/Fe composite material is prepared, SiC and iron react chemically to generate Fe at the interface of SiC particles and iron matrix3The C brittle phase influences the bonding strength of SiC particles and an iron matrix, and the SiC particles of the SiC/Fe composite wear-resistant material are easy to fall off in the using process, so that the wear-resistant performance of the SiC/Fe composite wear-resistant material is influenced. Therefore, if a novel SiC particle surface modification technology can be developed, when the infiltration method is adopted to prepare the SiC/Fe composite wear-resistant material, the chemical reaction between the SiC particles and molten iron can be inhibited, and the bonding strength between the SiC particles and an iron matrix can be ensured, so that the SiC particles with low price can be utilized to prepare the high-performance SiC/Fe composite wear-resistant materialSiC/Fe composite wear-resistant material.
Disclosure of Invention
The invention aims to develop a SiC particle surface modification process, wherein the modified SiC particles can inhibit the SiC particles from generating chemical reaction with molten iron when the SiC/Fe composite wear-resistant material is prepared by adopting an infiltration method, and harmful Fe can not be generated at the interface of the SiC particles and an iron matrix3C brittle phase, the modified SiC particles and the iron matrix have higher bonding strength, the SiC particles cannot fall off from the iron matrix in the use process of the SiC/Fe composite wear-resistant material, and the material has longer service life.
The technical scheme of the invention is as follows:
a SiC ceramic particle surface modification process is characterized by comprising the following steps:
(1) pretreatment of SiC particles:
firstly, putting industrial grade 1-3mm SiC particles into a muffle furnace, heating to 900-1000 ℃ at the speed of 4-5 ℃/min under the air atmosphere, preserving the temperature for 0.5-1 h, and cooling along with the furnace.
Then putting the calcined SiC particles into a 10wt% HF solution, sealing the HF solution with the SiC particles, and then placing the sealed HF solution in a water bath kettle at 60-70 ℃ for 3-4 hours.
Then taking out the SiC particles from the solution, washing the SiC particles to be neutral by using clear water, and drying the SiC particles at 120 ℃ to finish the pretreatment of the SiC particles.
(2) Preparing surface modified slurry of SiC particles:
the surface modification slurry of the SiC particles comprises the following raw material components in percentage by mass:
technical grade Mo (CO)610 to 15 percent of powder
60-70% of industrial-grade toluene solution
7 to 10 percent of Si powder with the diameter of 1 to 3 microns
5 to 7 percent of polyethylene glycol with the molecular weight of 4000
KH560 silane coupling agent 1% -1.5%
Weighing a specified amount of industrial-grade toluene solution according to the formula, pouring the industrial-grade toluene solution into a container, and adding industrial-grade Mo (CO) under the stirring condition of 800 revolutions per minute6And (2) after the powder is stirred for 0.5-1 hour, adding a KH560 silane coupling agent, stirring for 20-30 minutes under the stirring condition of 800 revolutions per minute, then adding Si powder with the diameter of 1-3 micrometers under the stirring condition of 3000 revolutions per minute, stirring for 1-1.5 hours, then reducing the stirring speed to 800 revolutions per minute, adding polyethylene glycol with the molecular weight of 4000, and stirring for 0.5-1 hour to obtain the surface modification slurry of the SiC particles.
(3) Surface modification treatment of SiC particles
Pouring the SiC particle surface modification slurry obtained in the step 2 into a container, and heating the container filled with the SiC particle surface modification slurry to 60 ℃ in a water bath kettle.
And (3) pouring the surface-treated SiC particles obtained in the step (1) into the SiC particle surface modification slurry to be immersed for 3-5 minutes, and then fishing out the SiC particles by using a stainless steel screen.
Drying the taken SiC particles at room temperature for 24h, putting the SiC particles into a muffle furnace, heating to 200 ℃ at the heating rate of 2 ℃/min and preserving heat for 1-1.5 h under the protection of argon, heating to 500 ℃ at the heating rate of 2-3 ℃/min and preserving heat for 0.5-1 h, heating to 1420 and 1450 ℃ at the heating rate of 5-6 ℃/min, preserving heat for 1-2 h, and cooling along with the furnace to obtain the surface modified SiC ceramic particles.
The invention is further explained below:
(1) and (4) pretreating SiC particles.
The industrial grade SiC particles take quartz sand and petroleum coke as raw materials, and the SiC is generated by the reaction of the quartz sand and the petroleum coke in a resistance furnace under the reducing atmosphere by adopting an Acheson method. The SiC particles produced by the process have a certain amount of residual C on the surface, and the existence of the residual C can influence the subsequent surface modification process of the SiC particles, so that the raw material SiC particles are firstly subjected to heat preservation for 0.5-1 h at the temperature of 900-1000 ℃ in the air atmosphere, and then are subjected to calcination treatment to remove the residual C on the surface of the SiC particles. A layer of smooth and compact SiO is formed on the surface of the calcined SiC particles2Oxide layer (see fig. 1), smooth SiC particle surface is not easily on the surfaceForming a continuous dense modified film so that the calcined SiC particles are placed in a 10wt% HF solution and the SiO on the surface of the SiC particles is etched away by HF2The oxide layer, the surface of the SiC particles soaked by HF, can be roughened significantly (see fig. 2), which is beneficial for the subsequent coating process.
(2) And preparing surface modified slurry of SiC particles.
Toluene is a common industrial organic solvent, has low surface tension and low price, and can dissolve Mo (CO)6And therefore is a solvent for the modified slurry. Mo (CO)6The molybdenum-base coordination compound can be decomposed to generate high-activity molybdenum powder at 200 ℃ in a reducing atmosphere, and is a source of a high-activity molybdenum source in the modified slurry. Adding KH560 silane coupling agent under stirring, the coupling agent can be uniformly dispersed in the solvent, then adding 1-3 micron Si powder, and simultaneously increasing the stirring speed to 3000 r/min. Because the silica powder is fine and easy to agglomerate, it is difficult to disperse uniformly in the organic solvent. Under the condition of stirring, a part of terminal group functional groups of the KH560 silane coupling agent in the solvent can form bonds with the surface of the silicon powder to form ether bonds, the other part of terminal groups of the KH560 silane coupling agent is easily soluble in an organic solvent, and the addition of the KH560 silane coupling agent can promote the agglomeration of the broken fine-grained silicon powder and ensure that the fine-grained silicon powder is uniformly dispersed in the solvent. After stirring for a period of time at a high speed, the silicon powder is uniformly dispersed in the solvent. And then polyethylene glycol with the molecular weight of 4000 is added, the polyethylene glycol is dissolved in the solvent, so that the viscosity of the solution is increased, the coagulation of silicon powder can be prevented after the stirring is stopped, meanwhile, the polyethylene glycol has certain adhesiveness and is a temporary adhesive of surface modified slurry of SiC particles, and the modified film can be firmly adhered to the surfaces of the SiC particles in a subsequent SiC film coating process.
(3) Surface modification treatment of SiC particles
The SiC particle surface modification slurry is heated to 60 ℃ in a water bath, the viscosity of the slurry is reduced along with the rise of the temperature, the surface tension is reduced, the wetting of the SiC particles is facilitated, and a continuous modification film is formed on the SiC surface. Pouring the pretreated SiC particles into the slurry to be immersed for 3-5 minutes, wherein the surface modification slurry can wet the SiC particlesAnd then fishing out the SiC particles by using a stainless steel screen, wherein a layer of modified film is formed on the surfaces of the particles. And drying the fished SiC particles at room temperature for 24 hours, partially volatilizing the toluene organic solvent, and simultaneously solidifying the polyethylene glycol in the slurry to firmly adhere the modified film layer to the surfaces of the SiC particles. Putting the SiC particles into a muffle furnace, heating to 200 ℃ at the heating rate of 2 ℃/min under the protection of argon, and preserving the temperature for 1-1.5 hours, wherein the toluene in the modified slurry is completely volatilized, and meanwhile, Mo (CO)6But also completely decomposed into CO and reduced molybdenum powder. Then heating to 500 ℃ at the heating rate of 2-3 ℃/min, and preserving the heat for 0.5-1 hour, wherein the temporary adhesive polyethylene glycol and the KH560 coupling agent in the modified slurry are completely cracked and volatilized in the process. Then raising the temperature to 1450-1500 ℃ at the speed of 5-6 ℃/min, and preserving the temperature for 1-2 hours. When the furnace temperature is higher than 1420 ℃, the silicon powder in the modified film starts to melt and generates metallurgical bonding with the nearby molybdenum powder to generate MoSi2. After the heat preservation is carried out for a period of time, the silicon powder on the surface of the SiC ceramic particles completely reacts with the molybdenum powder to form a layer of compact MoSi on the surface of the SiC particles2Modified thin film, simultaneously MoSi2The film layer can form Mo-Si-C bonds with the SiC particle matrix at high temperature, and MoSi2The film forms a strong chemical bond with the SiC particles.
The invention has the beneficial effects that:
the process can form a layer of continuous and compact MoSi on the surface of SiC particles2And an intermetallic compound thin film which can form Mo-Si-C bonds with SiC particles and has good bondability with SiC particles (FIG. 3, FIG. 4). MoSi2Has a melting point of 2120 ℃ and a contact angle with molten iron of 12 degrees, the coated SiC particles are made into ceramic preforms, and then a casting method is adopted to prepare the SiC/Fe-based composite material, the modified SiC particles have good wettability with molten iron alloy, and MoSi on the surface of the SiC particles2The film can inhibit harmful chemical reaction between molten iron and SiC particles, no impurity phase is precipitated at the interface, and the SiC particles can be well combined with the iron alloy (figure 5). Under the abrasion load, SiC particles can not fall off from the surface of the iron alloy matrix in advance because of low interface bonding strength, and the abrasion resistance of the SiC/Fe composite material can be improved by more than 50 percent.
Drawings
Fig. 1 shows the surface morphology of the untreated SiC particles.
FIG. 2 shows the surface morphology of the pretreated SiC particles.
FIG. 3 MoSi on the surface of SiC ceramic particles2The intermetallic compound film has a front surface appearance.
FIG. 4 MoSi on the surface of SiC ceramic particles2The cross-sectional morphology of the intermetallic compound film.
FIG. 5 is the interface morphology of the surface modified SiC ceramic particles with the iron alloy matrix.
Detailed Description
The present invention will be further described with reference to the following examples.
Examples
The embodiment provides a surface modification process of SiC ceramic particles, which comprises the following specific steps:
(1) and (4) pretreating SiC particles.
Firstly, putting industrial grade 1-3mm SiC particles into a muffle furnace, heating to 1000 ℃ at the speed of 4 ℃/min under the air atmosphere, preserving heat for 0.5 hour, and cooling along with the furnace. And then putting the calcined SiC particles into a 10wt% HF solution, sealing the HF solution of the placed SiC particles, placing the sealed HF solution of the SiC particles in a water bath kettle at 70 ℃ for 3 hours, taking out the SiC particles from the solution, washing the SiC particles to be neutral by using clear water, and drying the SiC particles at 120 ℃ to finish the pretreatment of the SiC particles.
(2) And preparing surface modified slurry of SiC particles.
The formula of the surface modification slurry of SiC particles is as follows (mass percent):
technical grade Mo (CO)6 powder 15%
69% of industrial-grade toluene solution
10% of Si powder with the diameter of 1-3 microns
Polyethylene glycol 5% with molecular weight of 4000%
KH560 silane coupling agent 1%
Firstly, the prescription is weighed according to the formulaPouring a quantity of technical grade toluene solution into a container, adding technical grade Mo (CO)6 powder under stirring at 800 rpm6And after stirring for 0.5, adding a KH560 silane coupling agent, stirring for 20 minutes under the stirring condition of 800 revolutions per minute, then adding Si powder with the diameter of 1-3 micrometers under the stirring condition of 3000 revolutions per minute, stirring for 1 hour, then reducing the stirring speed to 800 revolutions per minute, adding polyethylene glycol with the molecular weight of 4000, and stirring for 0.5 hour to obtain the surface modification slurry of the SiC particles.
(3) Surface modification treatment of SiC particles
Pouring the SiC particle surface modification slurry obtained in the step 2 into a container, and heating the container filled with the slurry to 60 ℃ in a water bath kettle. And (3) pouring the surface-treated SiC particles obtained in the step (1) into the slurry to be immersed for 3 minutes, and then fishing out the SiC particles by using a stainless steel screen. And drying the fished SiC particles at room temperature for 24 hours, putting the SiC particles into a muffle furnace, heating to 200 ℃ at a heating rate of 2 ℃/min and preserving heat for 1 hour under the protection of argon, then heating to 500 ℃ at a heating rate of 3 ℃/min and preserving heat for 1 hour, then heating to 1450 ℃ at a speed of 6 ℃/min, preserving heat for 1 hour, and cooling along with the furnace to obtain the surface-modified SiC ceramic particles.
Claims (1)
1. A SiC ceramic particle surface modification process is characterized by comprising the following steps:
(1) pretreatment of SiC particles: firstly, putting industrial grade 1-3mm SiC particles into a muffle furnace, heating to 900-1000 ℃ at the speed of 4-5 ℃/min under the air atmosphere, preserving the temperature for 0.5-1 h, and cooling along with the furnace; then putting the calcined SiC particles into a 10wt% HF solution, sealing the HF solution with the SiC particles, and placing the sealed HF solution in a water bath kettle at 60-70 ℃ for 3-4 hours; then taking out the SiC particles from the solution, washing the SiC particles to be neutral by using clear water, and drying the SiC particles at 120 ℃ to finish the pretreatment of the SiC particles;
(2) preparing surface modified slurry of SiC particles: the surface modification slurry of the SiC particles comprises the following raw material components in percentage by mass:
technical grade Mo (CO)6Powder 15%
69-70 percent of industrial-grade toluene solution
7 to 10 percent of Si powder with the diameter of 1 to 3 microns
5 to 7 percent of polyethylene glycol with the molecular weight of 4000
KH560 silane coupling agent 1% -1.5%
The sum of the contents of the components is 100 percent;
weighing a specified amount of industrial-grade toluene solution according to the formula, pouring the industrial-grade toluene solution into a container, and adding industrial-grade Mo (CO) under the stirring condition of 800 revolutions per minute6Powder is stirred for 0.5 to 1 hour, KH560 silane coupling agent is added, stirring is carried out for 20 to 30 minutes under the stirring condition of 800 revolutions per minute, then Si powder with the diameter of 1 to 3 microns is added under the stirring condition of 3000 revolutions per minute, stirring is carried out for 1 to 1.5 hours, the stirring speed is reduced to 800 revolutions per minute, polyethylene glycol with the molecular weight of 4000 is added, and stirring is carried out for 0.5 to 1 hour, thus obtaining surface modification slurry of SiC particles;
(3) performing surface modification treatment on SiC particles, pouring the SiC particle surface modification slurry obtained in the step (2) into a container, and heating the container filled with the SiC particle surface modification slurry to 60 ℃ in a water bath kettle; pouring the surface-treated SiC particles obtained in the step (1) into SiC particle surface modification slurry to be immersed for 3-5 minutes, and then fishing out the SiC particles by using a stainless steel screen mesh; drying the taken SiC particles at room temperature for 24h, putting the SiC particles into a muffle furnace, heating to 200 ℃ at the heating rate of 2 ℃/min and preserving heat for 1-1.5 h under the protection of argon, heating to 500 ℃ at the heating rate of 2-3 ℃/min and preserving heat for 0.5-1 h, heating to 1420 and 1450 ℃ at the heating rate of 5-6 ℃/min, preserving heat for 1-2 h, and cooling along with the furnace to obtain the surface modified SiC ceramic particles.
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| CN102766774A (en) * | 2012-07-10 | 2012-11-07 | 太原理工大学 | Method for strengthening magnesium alloy by doping SiC particles |
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| US4994416A (en) * | 1988-02-04 | 1991-02-19 | Martin Marietta Energy Systems, Inc. | Ceramic composites reinforced with modified silicon carbide whiskers and method for modifying the whiskers |
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| CN102766774A (en) * | 2012-07-10 | 2012-11-07 | 太原理工大学 | Method for strengthening magnesium alloy by doping SiC particles |
| CN103722806A (en) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | Preparation method of multilayer molybdenum-based heat-proof material |
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| MoSi2–再结晶SiC复合材料的高温抗氧化性能及氧化机理;高朋召 等;《硅酸盐学报》;20120630;第40卷(第6期);说明书第1.2样品制备和2.4MoSi2-RSiC复合材料的高温抗氧化机理 * |
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