CN1341578A - Method for preparing silicon carbide porous ceramic pipe - Google Patents
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Abstract
The preparation method of silicon carbide porous ceramic pipe is characterized by that it uses silicon carbide as aggregate, uses the eutectic mixture formed from feldspar and clay as anchoring agent, uses active carbon and other organic substance as pore-forming agent material and utilizes the slip casting process to obtain the porous ceramic material with higher porosity and a certain pore size. Said invention adopts the addition of inorganic electrolyte to regulate pH value, specific weight and viscosity of slurry material and control fluidity and stability of slurry material, and the model for forming adopts specially-treated gypsum model, and the strength of the biscuit can be improved by means of organic and inorganic adhesive. Said invention adopts a normal pressure sintering process to prepare the invented porous ceramic pipe whose porosity can be up to 60-65% and pore size is about 14 micrometers. By changing firing temp. the pore size distribution can be changed. It can be used for filtration and dust collection of high-temp. chimney, filtration purification of water resouce, and also can be used as carrier of catalyst for gas (or water) purification.
Description
Technical Field
The invention relates to a preparation method of silicon carbide porous ceramic, in particular to a SiC porous ceramic tube prepared by slip casting. Belongs to the field of porous ceramics.
Background
Porous ceramics can be divided into two types with diametrically opposite conditions of action. One is for separation of the two phases; the second is to disperse one phase into the other, i.e. to combine the two. As a honeycomb material which can exert excellent properties in the aspects of separation, dispersion, absorption and fluid contact, the honeycomb material is widely applied to industrial sectors such as chemical industry, petroleum industry, smelting industry, textile industry, pharmaceutical industry, food industry, machinery industry, cement industry and the like. With the expansion of the application range of the porous ceramic, the material of the porous ceramic is changed from common argillaceous to a high-temperature-resistant and corrosion-resistant structural ceramic material.
Porous ceramics are classified into mesh type and foam type. The mesh type is made of high permeability mesh ceramic by soaking polymer foam into slurry and then processing at high temperature; the foam type is a porous ceramic formed by foaming a pore-forming agent through a sintering reaction. The invention belongs to foam type porous ceramics.
At present, how to treat high-temperature dust-containing gas is always a pressing topic in various industrial departments. The ideal method is filtration dust removal. The most critical in filter dust removal is the choice of filter material. Glass fiber or modified glass fiber is adopted in China in large quantity, but the glass fiber or the modified glass fiber can not resist high temperature (less than or equal to 400 ℃), so that for high-temperature flue gas (or coal gas) with the temperature of more than 400 ℃, a method of filtering after cooling treatment by using cold-doped air is only adopted, and a large amount of sensible heat and energy are wasted. For porous ceramics functioning as a filter element at high temperatures, in addition to a certain pore size and air permeability, the porous ceramics are required to have sufficient mechanical strength, thermal shock resistance, no liquid phase adhering dust, and the like at high temperatures. For this purpose, the refractoriness of the aggregate particles is sufficiently high, and the binder should not exhibit a liquid phase at the application temperature, nor should the reaction product of the interface reaction layer with the aggregate. Another problem is that the thermal shock resistance is excellent, so that the normal use can be ensured. For this reason, it is necessary to use a material having a low coefficient of expansion. However, no patent report exists at home and abroad about slip casting of silicon carbide porous ceramic tubes so far, and a porous ceramic sample with cross pores or a ceramic filter core rod structure prepared by an extrusion or compression molding method has complex process and higher cost (ceram. Bull., Vol.70, No.9, 1991). Therefore, the development of a porous ceramic material with high temperature resistance, high strength, excellent thermal shock resistance and high permeability is urgent.
Disclosure of Invention
The invention aims to provide a method for preparing a silicon carbide porous ceramic tube by slip casting.
The invention is characterized in that SiC ceramic with high-temperature strength, small expansion coefficient, strong wear resistance, good thermal stability, large thermal conductivity, thermal shock resistance and chemical corrosion resistance is selected as aggregate, and the simplest slip casting process and normal pressure sintering system are adopted to obtain the annular porous ceramic tube with high strength, 60 percent of porosity and 14 to 20 microns of pore size.
The silicon carbide porous ceramic tube prepared by slip casting and normal pressure sintering mainly comprises the following four steps:
firstly, selecting raw materials
1. Aggregate: silicon carbide particles are selected as aggregate materials, the basic particle size is 8 microns, the largest particle is smaller than 28 microns, and the smallest particle size is larger than 3 microns.
2. Binding agent: potassium feldspar and bentonite are taken as raw materials, and eutectic mixture consisting of potassium oxide, aluminum oxide and silicon oxide is taken as a reference formula; the sodium metasilicate is an auxiliary binder, so that on one hand, the strength of the molded blank body can be improved; on the other hand, the material can participate in grain boundary phase reaction at high temperature, so that the bonding strength is improved. The ratio of the auxiliary binder to the binder is controlled within the range of 1: 3 (weight ratio); when the content of the auxiliary binder is too low, the improvement effect of the green body strength and the porous ceramic body strength is not obvious, and when the content is too high, the corrosivity of the gypsum model is enhanced, and the forming quality and the service life of the gypsum model are influenced.
3. Pore-forming agent: active carbon powder, sawdust, starch, polystyrene and the like are used as pore-forming agent materials. The pore former material oxidizes or burns at high temperatures to generate gases that escape, thereby forming pores and pore channels within the ceramic.
Secondly, slurry control: the slurry control mainly refers to the control of the fluidity and stability of the slurry, and is implemented by adjusting the pH value, the viscosity and the specific gravity of the slurry through the type and the dosage of the inorganic electrolyte.
1. Fluidity of the slurry
Factors affecting the fluidity of the slurry are:
(1) specific gravity of slurry, solid phase particle size and shape
The resistance to mud flow comes primarily from three aspects: the mutual attraction of water molecules themselves; attraction between solid phase particles and water molecules; collision resistance when solid phase particles move relatively. Empirical formulas show that:
δ＝δ0×(1-C)+k1Cn+k2Cm(1)
wherein δ represents the mud flow resistance; delta0Represents the viscosity of the liquid medium; c represents the specific gravity of the slurry, N, m, k1，k2Is a constant.
The more irregular the solid phase particles,the lower the fluidity of the slurry.
The greater the specific gravity, the greater the flow resistance; when the specific gravity is too small, the density of the biscuit is easy to reduce in the forming process. Therefore, the specific gravity of the solution should be controlled to be 1.3-1.5g/cm3And (3) a range.
(2) Inorganic electrolyte (deflocculant)
The role of the inorganic electrolyte (deflocculant) is mainly to avoid particle agglomeration by changing the bilayer thickness of the micelles in the slurry and the ZETA potential of the surface of the silicon carbide particles. The inorganic electrolyte used as the deflocculant must have the conditions:
a. can be dissociated into univalent cations (such as Na) with strong hydration capability;
b. can be directly dissociated or hydrolyzed to provide sufficient OH-Rendering the clay alkaline;
c. its cation can form insoluble salt or stable complex with the harmful ion in slurry to cause flocculation.
The inorganic electrolyte meeting the 3 conditions is one or two of sodium carbonate, sodium metasilicate and potassium carbonate, and the adding amount is 0.6-0.8% (weight percentage).
2. Stability of the slurry
The stability of the slurry is the key to ensure the density uniformity of the formed biscuit and is mainly influenced by the following factors:
(1) pH value
The magnitude of the pH directly affects the ZETA potential of the silicon carbide particle surface. As the pH value corresponding to the isoelectric point of the silicon carbide particles is 3-4, the pH value of the slurry is adjusted to be far away from the isoelectric point, namely, thepH value is within the range of 8-12, and the slurry has good stability.
(2) Viscosity of the oil
The organic substances for adjusting the viscosity include: polyvinyl alcohol, polyacrylamide, sodium polyacrylate; the inorganic substance is sodium metasilicate. The addition amount is 2.5-5% (volume percent), and the viscosity of the slurry is adjusted to be 20-35 mpa-s.
(3) Plasticizer agent
The plasticizer is added to ensure that the water in the slurry is uniformly removed in the curing process, and bentonite and the purple wood knots are used as the plasticizer. The addition amount is 0.5-1% (weight percentage).
During the physical dehydration process, after the slurry is injected into the model, the water is gradually discharged due to the action of the capillary tubes in the gypsum model. When a layer of blank body can be formed on the inner surface of the model, water must firstly pass through the capillary holes of the blank body layer and then enter the capillary holes of the model, and the resistance to dehydration comes from both the model and the blank body. In the early stage of grouting, the resistance of the model plays a main role; in the later stage of grouting, the resistance caused by the increase of the thickness of the blank plays a main role. The amount of resistance generated by the green body depends on the nature of the slurry and the structure of the green body. The slurry containing more plastic raw materials and more colloid particles has large dehydration resistance, and the blank formed in the model has large density and large resistance.
Improvement and treatment of plaster model
1. Improvement of model
The porosity of the gypsum model selected for slip casting is about 30%, and the diameter of the air hole is about3 microns. The model before and after treatment is shown in figure 1, and a radian transition area is added between the bottom walls after improvement; meanwhile, the gypsum model is decomposed into two parts, so that the forming quality is improved, cracks are avoided, and the demolding and model finishing and cleaning are facilitated.
2. Model processing
The chemical coagulation process means that a certain amount of CaSO is dissolved when the slurry contacts the plaster mold4It undergoes an ion exchange reaction with the clay and sodium silicate in the slurry:
so that a layer of Na-clay close to the surface of the plaster model is changed into Ca-clay, and the suspension in the slurry is converted into a coagulation state. The gypsum plays a role of a flocculating agent, promotes the slurry to be flocculated and hardened, and shortens the blank forming time. CaSiO with low solubility is generated through the reaction3The reaction is promoted to continuously proceed to the right, and Na is generated2SO4Is water soluble and is drawn into the capillaries of the mold. When the mold is dried, Na2SO4Precipitated as white, hairy crystals due to CaSO4The dissolution and reaction of (2) increase the capillary of the model, and the surface of the model has pockmarks, thus reducing the mechanical strength. Therefore, before grouting forming, the inner wall of the gypsum model is cleaned and placed in a drying box to be dried for 3 hours at the temperature of 60 ℃, and the water absorption uniformity of the model is ensured.
Fourthly, drying and sintering of biscuit
And drying the biscuit obtained by slip casting and then finallysintering the biscuit.
The drying process is divided into two stages, firstly, the biscuit is dried for 3 hours at 50 ℃ to eliminate larger moisture gradient in the biscuit; then dried at 100 ℃ for 3 hours. After the sample is dried, the sample is sintered under normal pressure at the temperature of 1200-1280 ℃, and the temperature is kept for 1-3 hours.
The porous ceramic is subjected to mercury-pressing test, and has porosity of 60-65%, pore diameter of 14-20 μm, and volume density of 1.1g/cm3(ii) a The electron probe microstructure analysis surface and fracture morphology finds that the pore channel is a three-dimensional network structure and the acicular mullite crystal is separated out locally. The existence of the mullite phase can greatly improve the strength of the porous ceramic. When the material is sintered at a lower temperature, the pore size distribution range is larger, and the porosity is lower; the increase in temperature can reduce the range of pore size distribution, and increase the porosity, but the reference pore size is not changed.
The slip casting silicon carbide porous ceramic tube provided by the invention has the outstanding characteristics that:
(1) the silicon carbide powder is used as the aggregate of the porous ceramic, and has good thermal conductivity, thermal shock resistance and small thermal expansion coefficient;
(2) the eutectic mixture consisting of feldspar and clay is selected as a bonding agent, and the bonding performance with silicon carbide particles is good;
(3) adopting active carbon and related organic matter particles as pore-forming agents;
(4) the grouting forming process is adopted, the process is simple, and the cost is low;
(5) improvement and treatment method of plaster model;
(6) the normal pressure sintering method is adopted, the sintering temperature is 1200-1280 ℃, and the heat preservation is carried out for 1-3 hours. The pore size distribution range can be changed by changing the firing temperature;
(7) the air holes are distributed in the ceramic body in a three-dimensional net structure.
Drawings
FIG. 1 is a schematic diagram of a gypsum model before and after improvement
(a) Before improvement, the model is an integral body, the bottom of the mold cavity is in right-angle transition, biscuit cracks are easy to generate, demolding is difficult, and the model is inconvenient to clean;
(b) after improvement, the mold consists of an upper part and a lower part, so that demolding and cleaning are facilitated, the bottom of the mold cavity is in arc transition, and forming cracks are avoided.
FIG. 2 shows the mercury intrusion test results for porous ceramics fired at 1240 ℃ with pore size on the abscissa and volume content on the ordinate.
FIG. 3 shows the mercury intrusion test results for a porous ceramic fired at 1280 ℃ with pore size on the abscissa and volume content on the ordinate, and 20 μm pores are present in addition to 14 μm pores.
FIG. 4 is a microscopic analysis photograph of the surface electron probe for the slip casting of silicon carbide porous ceramics provided by the present invention, which can observe the three-dimensional network distribution of the pores.
FIG. 5 is a scanning electron micrograph showing a localized acicular mullite phase, thereby increasing the strength of the porous ceramic.
Detailed Description
The embodiments and effects are further illustrated by the following non-limiting examples:
example 1
Silicon carbide micropowder is selected as an aggregate material, potassium feldspar and bentonite form a binding agent in a ratio of 3: 2, activated carbon is used as a pore-forming agent, the silicon carbide micropowder, the potassium feldspar and the bentonite are prepared according to a weight percentage of 65: 5: 30, the mixture is subjected to ball milling and mixing for 4 hours, 50 percent of sodium metasilicate and polyvinyl alcohol respectively (volume ratio) and 50 percent of sodium carbonate and potassium carbonate inorganic electrolyte respectively (weight ratio) are added, 0.8 percent of bentonite is added as a plasticizer, stirring and ageing are carried out for 48 hours, and the specific gravity of the slurry is 1.4g/cm3The viscosity is 25 mpa.s, the PH is about 10, the model is cleaned and dried, then slurry is poured, the biscuit is respectively dried at 50 ℃ and 100 ℃, the biscuit is sintered at 1240 ℃ and is kept warm for 2 hours, and the obtained excessive substancesPore ceramic size about 14 microns, as shown in fig. 3; the porosity was about 60%. Acicular mullite devitrification locally appears, and the observation result of a scanning electron microscope is shown in figure 5, so that the strength of the silicon carbide porous ceramic tube is improved.
Example 2
Silicon carbide micropowder is selected as aggregate materialThe potash feldspar and the bentonite form a bonding agent in a ratio of 3: 2, the activated carbon is a pore-forming agent, the potash feldspar and the bentonite are prepared according to the weight percentage of 65: 5: 30, the mixture is subjected to ball milling and mixing for 4 hours, 2.2 vol% of polyacrylamide and 0.7 wt% of purple wood knots are added, the viscosity of the slurry is 30mpa&s, the PH is about 11, and the specific gravity is 1.35g/cm3Firing at 1280 ℃, and keeping the temperature for 1.5 hours, wherein the pores with the diameter of 20 microns exist in addition to the pores with the diameter of 14 microns, as shown in figure 4; the porosity was about 65%, and the rest was the same as in example 1.
Claims (10)
1. A method for preparing a silicon carbide porous ceramic tube comprises the technical processes of slurry preparation, ageing, forming and sintering, and is characterized in that: (1) selecting silicon carbide as the aggregate of the porous ceramic, taking a eutectic mixture consisting of potassium oxide, aluminum oxide and silicon oxide as a reference formula as a binding agent, sodium metasilicate as an auxiliary binding agent, controlling the proportion of the two in a weight ratio of 3: 1, and taking activated carbon and other organic matter particles as pore-forming agents; (2) adopting slip casting process, regulating pH value of the slurry to 8-12, viscosity to 20-35 mpa.s and specific gravity to 1.3-1.5g/cm by regulating the type and dosage of inorganic electrolyte3Thereby controlling the fluidity and stability of the slurry; (3) the bottom of the gypsum model is in arc transition and is treated at low temperature, so that the forming process is uniform and the demoulding is easy; (4) the normal pressure sintering is adopted, the porosity, the pore size and the distribution of the porous ceramic tube are changed by changing the sintering temperature, and the pores are distributed in a three-dimensional net structure.
2. The method of claim 1, wherein the silicon carbide powder as an aggregate has a primary particle size of 8 microns, a maximum of 28 microns, and a minimum of greater than 3 microns; the bonding agent takes potassium feldspar and bentonite as raw materials; the pore-forming agent material is one or more of activated carbon micro powder, starch granules, polystyrene particles and sawdust; the ratio of the three components is 65: 5: 30 (weight percentage).
3. The method for preparing a silicon carbide porous ceramic tube as claimed in claim 1, wherein the inorganic electrolyte is one or two of sodium carbonate, sodium metasilicate and potassium carbonate added in an amount of 0.6 to 0.8 wt%.
4. The method for preparing silicon carbide porous ceramic tube as claimed in claim 1, wherein the organic substance for adjusting the viscosity of the slurry is polyvinyl alcohol, polyacrylamide and sodium polyacrylate, and the inorganic substance is sodium metasilicate added in an amount of 2-2.5 wt%.
5. The method for preparing a silicon carbide porous ceramic tube as set forth in claim 1, wherein bentonite and rosewood are used as plasticizers in an amount of 0.5 to 1 wt% in order to uniformly remove moisture during the curing of the slurry.
6. The method of making a silicon carbide porous ceramic tube according to claim 1, wherein said gypsum model has a porosity of about 30% and a pore diameter of about 3 microns; the low-temperature treatment was previously dried at 60 ℃ for 3 hours.
7. The method for preparing a silicon carbide porous ceramic tube as set forth in claim 1, wherein the biscuit after the slip casting is dried in two steps at 50 ℃ and 100 ℃ respectively.
8. The method for preparing silicon carbide porous ceramic tube as claimed in claim 1, wherein the sintering temperature range of the normal pressure sintering is 1200-1280 ℃, and the holding time is 1-3 hours.
9. The method of preparing a silicon carbide porous ceramic tube according to claim 1 or 8, wherein the silicon carbide porous ceramic tube has a porosity of about 60%, a pore size of about 14 μm, and a three-dimensional network distribution of pore channels.
10. The method for producing a silicon carbide porous ceramic tube as set forth in claim 1 or 8, wherein the oxidation product on the surface of the silicon carbide participates in the grain boundary reaction, and a new mullite phase appears.
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| CN115531980A (en) * | 2021-06-30 | 2022-12-30 | 大西洋过滤器和泳池配件有限责任公司 | Improved ceramic filter material for water treatment |
| WO2023272946A1 (en) * | 2021-06-30 | 2023-01-05 | 武汉工程大学 | Sic smoke particle collector and preparation method thereof |
| CN116639998A (en) * | 2023-07-27 | 2023-08-25 | 天津爱思达航天科技股份有限公司 | Porous silicon carbide ceramic material and preparation method thereof |
| CN116639998B (en) * | 2023-07-27 | 2023-10-31 | 天津爱思达航天科技股份有限公司 | Porous silicon carbide ceramic material and preparation method thereof |
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