CN101962295A - Novel silicon carbide ceramic and preparation method thereof - Google Patents
Novel silicon carbide ceramic and preparation method thereof Download PDFInfo
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- CN101962295A CN101962295A CN 201010297902 CN201010297902A CN101962295A CN 101962295 A CN101962295 A CN 101962295A CN 201010297902 CN201010297902 CN 201010297902 CN 201010297902 A CN201010297902 A CN 201010297902A CN 101962295 A CN101962295 A CN 101962295A
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Abstract
The invention belongs to the field of silicon carbide materials, and in particular relates to a novel silicon carbide ceramic and a preparation method thereof. The novel silicon carbide ceramic is prepared from main materials and auxiliary materials, wherein the main materials comprise the following components in percent by mass: 80 to 90 percent of silicon carbide powder, 6 to 10 percent of silicon powder and 4 to 10 percent of carbon powder; and the auxiliary materials comprise a binder and a dispersant, wherein the dosage of the binder is 1 to 5 percent based on the total mass of the main materials; and the dosage of the dispersant is 0.5 to 1 percent based on the total mass of the main materials. The silicon carbide ceramic prepared by the method has the characteristics of high performance, volume density of between 3.05 and 3.10 g/cm<3>, free silicon content of less than 5 percent, hardness of 90 to 93 HRA, and bending strength of between 400 and 450 MPa.
Description
Technical field
The invention belongs to the carbofrax material field, be specifically related to a kind of novel silicon carbide pottery and preparation method thereof.
Background technology
Silicon carbide ceramics has high strength, high tenacity, low creep properties, the rub resistance wearing and tearing, erosion resistance and good oxidation-resistance, and its excellent mechanical property, lower thermal expansivity and higher heat-conduction coefficient have determined that the thermal shock resistance of silicon carbide ceramics is very good.In recent years, silicon carbide ceramics in the application of machinery, chemical industry, military project, the contour technology industry of the energy more and more widely.At present, industrial silicon carbide ceramics mainly adopts reaction sintering and pressureless sintering dual mode.
The ultimate principle of silicon carbide reaction-sintered is: the liquid-state silicon with reactive behavior is infiltrated carbonaceous porous ceramics biscuit under the effect of capillary force, and generate silicon carbide with the reaction of wherein carbon, newly-generated silicon carbide original position is in conjunction with original silicon-carbide particle in the biscuit, impregnant is filled the residue pore in the biscuit, finishes densification process.After α commonly used-SiC powder and graphite or other can provide the material mixing moulding of carbon source, infiltrate biscuit by liquid-phase silicone and react with carbon and generate β-SiC, and original α-SiC combined become sintered compact.
The ultimate principle of pressureless sintering silicon carbide is: normal pressure-sintered by adding effective sintering aid under higher sintering temperature, and silicon carbide generation crystal conversion during high temperature, thereby the dense sintering body of acquisition silicon carbide.
Though existing silicon carbide ceramic production technology can satisfy the use properties of silicon carbide ceramics, but still have following problem: the deadly defect of (1) reaction sintering silicon carbide ceramic is to contain free silica in the pottery.The existence of free silica has restricted the application of reaction sintering silicon carbide ceramic under high temperature (greater than 1500 ℃) and strong corrosive environment, so the content of free silica is low more good more in the reaction sintering silicon carbide ceramic; (2) though the performance of pressureless sintering silicon carbide ceramics is good, its production cost is higher.Therefore, be necessary to develop a kind of preparation method of novel silicon carbide ceramics, guarantee that every performance index of silicon carbide ceramics do not reduce, also can further reduce production costs.
Summary of the invention
The object of the present invention is to provide a kind of novel silicon carbide pottery and preparation method thereof, its further purpose is to provide a kind of lower-cost silicon carbide ceramics and preparation method thereof.
The present invention is by the following technical solutions: a kind of novel silicon carbide pottery, make through mixing pulping, granulation, compression moulding, sintering with following major ingredient and auxiliary material, the mass percent of major ingredient consists of: silicon carbide powder 80-90%, silica flour 6-10% and carbon dust 4-10%, auxiliary material is binding agent and dispersion agent, the consumption of binding agent is the 1-5% of major ingredient total mass, and the consumption of dispersion agent is the 0.5-1% of major ingredient total mass.
Described silicon carbide powder is made by silicon carbide waste, and described silica flour is made by the waste mortar of the brilliant silicon chip cutting fluid of sun power.
Described binding agent is a polyvinyl alcohol or/and carboxymethyl cellulose, and dispersion agent is one or more the combination in polyoxyethylene glycol, Tetramethylammonium hydroxide, aluminophosphates, the polyacrylic acid.
The preparation method of novel silicon carbide pottery comprises the steps:
(1) gets each raw material in proportion, silicon carbide powder, silica flour, carbon dust are added in the deionized water, add binding agent and dispersion agent successively, ball milling mixing 4-10 hour, the compound slip of one-tenth solid content 50-70%;
(2) compound slip is spray-dried, gets compound granulation powder; Hot blast inlet temperature during described spraying drying is 200-300 ℃, and temperature out is 110-140 ℃, and compound slip flow is 20-100kg/h;
(3) compound granulation powder gets biscuit through dry-pressing formed; Described pressure when dry-pressing formed is 60-200Mpa.
(4) biscuit gets the novel silicon carbide pottery through vacuum sintering, and sintering temperature is 1600-1800 ℃, and soaking time is 2-5 hour.
The preparation process of described silicon carbide powder is: a, be that the acid solution of 1-5 soaks at least 8 hours to remove metal and oxide impurity with silicon carbide waste pH, aqueous slkali soaking 2-4 hour that uses pH＞10 again to remove silicon-dioxide; B, the product of step a is scattered in its quality 0.8-1 water doubly forms suspension, regulate pH≤2 of suspension, stirred 6-14 hour, filter, washing filter cake to washings is a neutrality, dry cake; C, filter cake is scattered in its quality 2-5 organic solvent doubly, adds the tensio-active agent of filter cake quality 0.5-7%, stirred 6-12 hour, remove organic solvent, dry must silicon carbide powder.
Described organic solvent is one or more the combination in dehydrated alcohol, toluene, chloroform, tetracol phenixin and the tetrahydrofuran (THF); Described tensio-active agent is one or more the combination in aluminum-zirconium coupling agent, polyoxyethylene glycol, the silane coupling agent.
The preparation process of described silica flour is: a, solar silicon wafers is cut waste mortar temperature regulation to 20～80 ℃, solid-liquid separation; B, separating obtained solid is added the water pulping to mass concentration 15-90%, the back adopts scraper centrifugal machine to separate; It is 20～40wt% that c, the solid that separation is obtained add water pulping to concentration, and in slurry, add flotation oil by 0.01～0.1% of solid masses, then slurry is squeezed into hydraulic grading device, continue to blast air draught, fully stir after 1-3 hour, flow velocity with 100～500L/h carries out the current flotation again, gets thick silica flour; D, with thick silica flour carry out pickling successively, concentrate, oven dry obtains silica flour.
Described flotation oil is one or more the combination in pine tar, 2# flotation oil, the QX-3 flotation oil; Described solid-liquid separation adopts horizontal centrifuge, vertical centrifugal machine, settling centrifuge or scraper centrifugal machine, and centrifugal speed is 500-1500r/min.
Described binding agent is a polyvinyl alcohol or/and carboxymethyl cellulose, and dispersion agent is one or more the combination in polyoxyethylene glycol, Tetramethylammonium hydroxide, aluminophosphates, the polyacrylic acid.
The present invention compared with prior art has the following advantages:
(1) the novel silicon carbide pottery that adopts raw material of the present invention and method to get, volume density is 3.05-3.10g/cm
3, contents of free si＜5%, hardness is 90-93HRA, bending strength is 400-450MPa;
(2) silicon carbide powder among the present invention adopts the silicon carbide waste of collecting in the industrial production silicon carbide micro-powder to obtain through pre-treatment, pickling, activation modification, drying, the utilization again of this part waste material has alleviated the pressure of factory processes waste material greatly, has created more added value simultaneously;
(3) silica flour among the present invention adopts the tiny polysilicon of uniform particles by the waste mortar recovery of the brilliant silicon chip cutting fluid of sun power, the economic worth of polysilicon is far above waste mortar, the environmental pollution of so not only having avoided waste mortar to produce, also save a large amount of resources, met the policy of national energy-saving and emission-reduction;
(4) the present invention adopts the granulation powder that the silica flour that reclaims in silicon carbide powder that silicon carbide waste makes and the waste mortar is made, directly be pressed into high fine and close ceramics biscuits of carbonized bricks, omit in the existing reaction sintering silicon carbide ceramic silicon chip and suppressed this link, reduced operation, reduced cost.
Description of drawings
Fig. 1 is the granule-morphology of the compound granulation powder of embodiment 1.
Embodiment
Embodiment 1: a kind of novel silicon carbide pottery, the mass percent of its major ingredient consists of: 80% silicon carbide powder, 10% silica flour and 10% carbon dust, its auxiliary material is polyvinyl alcohol and polyoxyethylene glycol, the consumption of polyvinyl alcohol is 1% of a major ingredient total mass, and the total mass of polyoxyethylene glycol is 0.5% of a major ingredient total mass;
Carry out following steps during preparation successively:
(1) preparation silicon carbide powder, is that 1 acid solution soaks 8 hours to remove metal and oxide impurity with silicon carbide waste pH at a, is that 11 aqueous slkali soaking 2 hours is with removal silicon-dioxide with pH again; B, the product of step a is scattered in the water of 0.8 times of its quality and forms suspension, the pH that regulates suspension is 2, stirs 6 hours, filters, and washing filter cake to washings is a neutrality, dry cake; C, filter cake is scattered in the dehydrated alcohol of 2 times of its quality, adds the aluminum-zirconium coupling agent of filter cake quality 0.5%, stirred 6 hours, remove organic solvent, dry must silicon carbide powder;
(2) preparation silica flour, cuts waste mortar temperature regulation to 20 ℃ with solar silicon wafers at a, and adopting centrifugal speed is the horizontal centrifuge solid-liquid separation of 1500r/min; B, separating obtained solid is added the water pulping to mass concentration 15%, the back adopts scraper centrifugal machine to separate; C, isolated solid materials is added water pulping to concentration is 20wt%, and press 0.01～0.1% of solid masses and in slurry, add the 2# flotation oil, silicon carbide is separated with silica flour, then slurry is squeezed into hydraulic grading device, continue to blast air draught, fully stir after 1 hour, the flow velocity with 100L/h carries out the current flotation again, gets thick silica flour; D, with thick silica flour carry out pickling successively, concentrate, oven dry obtains silica flour;
(3) get each raw material in proportion, silicon carbide powder, silica flour, carbon dust are added in the deionized water, add binding agent and dispersion agent successively, ball milling mixed 4 hours, and the one-tenth solid content is 50% compound slip;
(4) compound slip is carried out spraying drying, obtain compound granulation powder, concrete processing condition are during spraying drying: 200 ℃ of hot blast inlet temperatures, 110 ℃ of temperature outs, compound slip flow 20kg/h; The granule-morphology of compound granulation powder as shown in Figure 1, the powder granule after the granulation is spherical in shape as can be seen from Fig. 1, even particle size distribution, for solid, thereby make the granulation powder have excellent flowing, grating is reasonable, is beneficial to the mouldenpress compacting and obtains high fine and close biscuit of ceramics;
(5) adopt 60MPa dry-pressing formed to compound granulation powder, obtain high fine and close biscuit;
(6) above-mentioned biscuit is carried out vacuum sintering, 1600 ℃ of sintering temperatures, soaking time 5 hours obtains the novel silicon carbide pottery, and its volume density is 3.05g/cm
3, contents of free si＜6%, hardness is 90HRA, bending strength is 400MPa.
Embodiment 2: a kind of novel silicon carbide pottery, the mass percent of its major ingredient consists of: 90% silicon carbide powder, 6% silica flour and 4% carbon dust, its auxiliary material is carboxymethyl cellulose and Tetramethylammonium hydroxide, 5% of the consumption major ingredient total mass of carboxymethyl cellulose, the total mass of Tetramethylammonium hydroxide is 1% of a major ingredient total mass;
Carry out following steps during preparation successively:
(1) preparation silicon carbide powder, is that 3 acid solution soaks 9 hours to remove metal and oxide impurity with silicon carbide waste pH at a, is that 12 aqueous slkali soaking 3 hours is with removal silicon-dioxide with pH again; B, the product of step a is scattered in the water of 0.9 times of its quality and forms suspension, the pH that regulates suspension is 1, stirs 12 hours, filters, and washing filter cake to washings is a neutrality, dry cake; C, filter cake is scattered in the toluene of 4 times of its quality, adds the polyoxyethylene glycol of filter cake quality 4%, stirred 9 hours, remove organic solvent, dry must silicon carbide powder;
(2) preparation silica flour, cuts waste mortar temperature regulation to 60 ℃ with solar silicon wafers at a, and adopting centrifugal speed is the vertical centrifugal machine solid-liquid separation of 1000r/min; B, separating obtained solid is added the water pulping to mass concentration 50%, the back adopts scraper centrifugal machine to separate; C, isolated solid materials is added water pulping to concentration is 30wt%, and in slurry, add pine tar by 0.01～0.1% of solid masses, silicon carbide is separated with silica flour, then slurry is squeezed into hydraulic grading device, continue to blast air draught, fully stir after 2 hours, the flow velocity with 300L/h carries out the current flotation again, gets thick silica flour; D, with thick silica flour carry out pickling successively, concentrate, oven dry obtains silica flour;
(3) get each raw material in proportion, silicon carbide powder, silica flour, carbon dust are added in the deionized water, add binding agent and dispersion agent successively, ball milling mixed 10 hours, was mixed with solid content and is 70% compound slip;
(4) compound slip is carried out spraying drying, obtain compound granulation powder, concrete processing condition are during spraying drying: 300 ℃ of hot blast inlet temperatures, 140 ℃ of temperature outs, compound slip flow 100kg/h;
(5) adopt 200MPa dry-pressing formed to compound granulation powder, obtain high fine and close biscuit;
(6) above-mentioned biscuit is carried out vacuum sintering, 1800 ℃ of sintering temperatures, soaking time 3 hours obtains the novel silicon carbide pottery, and its volume density is 3.10g/cm
3, contents of free si＜5%, hardness is 93HRA, bending strength is 450MPa.
Embodiment 3: a kind of novel silicon carbide pottery, the mass percent of its major ingredient consists of: 85% silicon carbide powder, 8% silica flour and 7% carbon dust, its auxiliary material is the mixture and the aluminophosphates of polyvinyl alcohol and carboxymethyl cellulose, 3% of the consumption major ingredient total mass of the mixture of polyvinyl alcohol and carboxymethyl cellulose, the total mass of aluminophosphates is 1% of a major ingredient total mass;
Carry out following steps during preparation successively:
(1) preparation silicon carbide powder, is that 5 acid solution soaks 10 hours to remove metal and oxide impurity with silicon carbide waste pH at a, is that 13 aqueous slkali soaking 4 hours is with removal silicon-dioxide with pH again; B, the product of step a is scattered in the water of 1 times of its quality and forms suspension, the pH that regulates suspension is 1.5, stirs 14 hours, filters, and washing filter cake to washings is a neutrality, dry cake; C, filter cake is scattered in the tetracol phenixin of 5 times of its quality, adds the silane coupling agent of filter cake quality 7%, stirred 12 hours, remove organic solvent, dry must silicon carbide powder;
(2) preparation silica flour, cuts waste mortar temperature regulation to 80 ℃ with solar silicon wafers at a, and adopting centrifugal speed is the settling centrifuge solid-liquid separation of 500r/min; B, separating obtained solid is added the water pulping to mass concentration 90%, the back adopts scraper centrifugal machine to separate; C, isolated solid materials is added water pulping to concentration is 40wt%, and press 0.01～0.1% of solid masses and in slurry, add the QX-3 flotation oil, silicon carbide is separated with silica flour, then slurry is squeezed into hydraulic grading device, continue to blast air draught, fully stir after 3 hours, the flow velocity with 500L/h carries out the current flotation again, gets thick silica flour; D, with thick silica flour carry out pickling successively, concentrate, oven dry obtains silica flour;
(3) get each raw material in proportion, silicon carbide powder, silica flour, carbon dust are added in the deionized water, add binding agent and dispersion agent successively, ball milling mixed 8 hours, was mixed with solid content and is 60% compound slip;
(4) compound slip is carried out spraying drying, obtain compound granulation powder, concrete processing condition are during spraying drying: 250 ℃ of hot blast inlet temperatures, 130 ℃ of temperature outs, compound slip flow 60kg/h;
(5) adopt 100MPa dry-pressing formed to compound granulation powder, obtain high fine and close biscuit;
(6) above-mentioned biscuit is carried out vacuum sintering, 1700 ℃ of sintering temperatures, sintering time 2 hours obtains the novel silicon carbide pottery, and its volume density is 3.07g/cm
3, contents of free si＜5%, hardness is 92HRA, bending strength is 420MPa.
Claims (10)
1. novel silicon carbide pottery, it is characterized in that, make through mixing pulping, granulation, compression moulding, sintering with following major ingredient and auxiliary material, the mass percent of major ingredient consists of: silicon carbide powder 80-90%, silica flour 6-10% and carbon dust 4-10%, auxiliary material is binding agent and dispersion agent, the consumption of binding agent is the 1-5% of major ingredient total mass, and the consumption of dispersion agent is the 0.5-1% of major ingredient total mass.
2. novel silicon carbide pottery as claimed in claim 1 is characterized in that described silicon carbide powder is made by silicon carbide waste, and described silica flour is made by the waste mortar of the brilliant silicon chip cutting fluid of sun power.
3. novel silicon carbide pottery as claimed in claim 1 or 2, it is characterized in that, described binding agent is a polyvinyl alcohol or/and carboxymethyl cellulose, and dispersion agent is one or more the combination in polyoxyethylene glycol, Tetramethylammonium hydroxide, aluminophosphates, the polyacrylic acid.
4. the preparation method of the described novel silicon carbide pottery of claim 1 is characterized in that comprising the steps:
(1) gets each raw material in proportion, silicon carbide powder, silica flour, carbon dust are added in the deionized water, add binding agent and dispersion agent successively, ball milling mixing 4-10 hour, the compound slip of one-tenth solid content 50-70%;
(2) compound slip is spray-dried, gets compound granulation powder; Hot blast inlet temperature during described spraying drying is 200-300 ℃, and temperature out is 110-140 ℃, and compound slip flow is 20-100kg/h;
(3) compound granulation powder gets biscuit through dry-pressing formed; Described pressure when dry-pressing formed is 60-200Mpa;
(4) biscuit gets the novel silicon carbide pottery through vacuum sintering, and sintering temperature is 1600-1800 ℃, and soaking time is 2-5 hour.
5. the preparation method of novel silicon carbide pottery as claimed in claim 4, it is characterized in that, the preparation process of described silicon carbide powder is: a, be that the acid solution of 1-5 soaks at least 8 hours to remove metal and oxide impurity with silicon carbide waste pH, aqueous slkali soaking 2-4 hour that uses pH＞10 again to remove silicon-dioxide; B, the product of step a is scattered in its quality 0.8-1 water doubly forms suspension, regulate pH≤2 of suspension, stirred 6-14 hour, filter, washing filter cake to washings is a neutrality, dry cake; C, filter cake is scattered in its quality 2-5 organic solvent doubly, adds the tensio-active agent of filter cake quality 0.5-7%, stirred 6-12 hour, remove organic solvent, dry must silicon carbide powder.
6. the preparation method of novel silicon carbide pottery as claimed in claim 5 is characterized in that, described organic solvent is one or more the combination in dehydrated alcohol, toluene, chloroform, tetracol phenixin and the tetrahydrofuran (THF); Described tensio-active agent is one or more the combination in aluminum-zirconium coupling agent, polyoxyethylene glycol, the silane coupling agent.
7. as the preparation method of claim 5 or 6 each described novel silicon carbide potteries, it is characterized in that the preparation process of described silica flour is: a, solar silicon wafers is cut waste mortar temperature regulation to 20～80 ℃, solid-liquid separation; B, separating obtained solid is added the water pulping to mass concentration 15-90%, the back adopts scraper centrifugal machine to separate; It is 20～40wt% that c, the solid that separation is obtained add water pulping to concentration, and in slurry, add flotation oil by 0.01～0.1% of solid masses, then slurry is squeezed into hydraulic grading device, continue to blast air draught, fully stir after 1-3 hour, flow velocity with 100～500L/h carries out the current flotation again, gets thick silica flour; D, with thick silica flour carry out pickling successively, concentrate, oven dry obtains silica flour.
8. the preparation method of novel silicon carbide pottery as claimed in claim 7 is characterized in that, described flotation oil is one or more the combination in pine tar, 2# flotation oil, the QX-3 flotation oil; Described solid-liquid separation adopts horizontal centrifuge, vertical centrifugal machine, settling centrifuge or scraper centrifugal machine, and centrifugal speed is 500-1500r/min.
9. as the preparation method of each described novel silicon carbide pottery of claim 4-6, it is characterized in that, described binding agent is a polyvinyl alcohol or/and carboxymethyl cellulose, and dispersion agent is one or more the combination in polyoxyethylene glycol, Tetramethylammonium hydroxide, aluminophosphates, the polyacrylic acid.
10. the preparation method of novel silicon carbide pottery as claimed in claim 7, it is characterized in that, described binding agent is a polyvinyl alcohol or/and carboxymethyl cellulose, and dispersion agent is one or more the combination in polyoxyethylene glycol, Tetramethylammonium hydroxide, aluminophosphates, the polyacrylic acid.
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| CN113582699A (en) * | 2021-07-22 | 2021-11-02 | 武汉工程大学 | Low-viscosity high-solid-content ceramic slurry and preparation method thereof |
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