CN103086732B - Fiber enhanced silicon carbide porous ceramic and preparation method and application thereof - Google Patents
Fiber enhanced silicon carbide porous ceramic and preparation method and application thereof Download PDFInfo
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- CN103086732B CN103086732B CN201310020058.8A CN201310020058A CN103086732B CN 103086732 B CN103086732 B CN 103086732B CN 201310020058 A CN201310020058 A CN 201310020058A CN 103086732 B CN103086732 B CN 103086732B
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Abstract
The invention discloses fiber enhanced silicon carbide porous ceramic which is composed of the following components in part by weight: 1 part of a ceramic binder, 1-3 parts of mullite fiber pulp, 8 parts of silicon carbide particles with an average particle size being about 230microns, and 1 part of a pore-forming agent. The preparation method is implemented through the steps that firstly, homogeneous mullite fiber pulp is prepared, so that when the mullite fiber pulp is mixed with a binder and silicon carbide particles with large particle sizes, mullite fibers can be uniformly dispersed but not agglomerated, thereby achieving a good toughening effect in a ceramic matrix. The invention further discloses an application of the fiber enhanced silicon carbide porous ceramic in the aspects of preparing silicon carbide porous ceramics and improving the toughness of silicon carbide porous ceramics.
Description
The present invention obtains national high-tech research evolutionary operation(EVOP) (863 Program) (No.2012 AA03 A610) fund project and subsidizes.
Technical field
The invention belongs to the technical field that porous ceramics filters supporter, relate to the method for making of high temperature filtration supporter carborundum porous ceramics, say more specifically a kind of method that improves high temperature filtration supporter carborundum porous ceramics bending strength.
Background technology
Silicon carbide has very high fusing point, bending strength, fracture toughness property and thermal conductivity, has lower thermal expansivity and density simultaneously.So that silicon carbide is a kind of hot strength is good, heat-shock resistance is strong, thermal conductivity good and corrosion resistant stupalith.Silicon carbide is widely used in the fields such as high temperature furnace lining, rocket nozzle and gas turbine blades thermal barrier coating.The silicon carbide porous ceramic pipe material of making taking silicon carbide as main raw material has high strength, high temperature resistant, corrosion resistant characteristic equally, is widely used in Coal Chemical Industry, thermal power plant and various high-temperature dust removal technical field.Be raw material and have pore connectivity deficiency or the less problem of air vent aperture with the carborundum porous ceramics that pore-forming material is produced gross blow hole with small particle size SiC, this causes its gas permeability lower.And hot gas filtration requires porous ceramics will have high gas permeability.Therefore, can adopt the sic powder of large particle diameter is raw material, and adds content and the suitable pore-forming material of size to improve carborundum porous ceramics air vent aperture and void content, thereby improves its rate of permeation.It is that the silicon carbide of greater particle size of 230 μ m is as raw material that this invention has adopted median size.The lower toughness of porous ceramics has limited its application simultaneously.Therefore, people have carried out a large amount of research in order to improve porous ceramics toughness.Ceramic fiber can be used for reaching because of having higher Young's modulus and intensity the object that improves porous ceramics toughness, mullite fiber is exactly a kind of ceramic fiber with high elastic coefficient, having stable high-temperature performance property, low thermal coefficient of expansion, its use temperature is at 1500 DEG C-1700 DEG C, is widely used in ceramic composite matrix toughness reinforcing.Fiber reinforced dominant mechanism has: fiber is extracted, fibre debonding, crack deflection and bridging toughness reinforcing etc.Wherein fiber is extracted and is referred to the phenomenon skidding off along the interface of it and matrix under stress outside near the fiber of crack tip.Fiber is extracted and can be made crack tip stress relaxation, thereby has slowed down the expansion of crackle.Fiber is extracted needs external force acting, therefore plays toughening effect; Fibre debonding refers to that matrix material has produced new surface after fibre debonding, therefore requires the expenditure of energy; Crack deflection refers to crack tip effect, refers in crack propagation process when crackle meets deflection unit (as wild phase, interface etc.) time institute's run-off the straight and deflection; Bridging is toughness reinforcing refer to for certain bits to the fiber distributing, crackle is difficult to deflection, can only continue expand along original propagation direction.At this moment do not rupture near the fiber at crack tip place, but set up foot bridge in crackle two sides, two sides are connected together.Produce a stress in crack surfaces, to offset the effect of applied stress, thereby make crackle be difficult to further expand, play toughening effect.This invention be exactly used that fiber is extracted, fibre debonding, crack deflection and bridging toughening mechanism, the toughness that improves carborundum porous ceramics with mullite fiber is for technical fields such as gas cleaning at high temperature.
The toughness reinforcing SiC based composite ceramic material of fibrous reinforcement is being used widely aspect high temperature heat structure with its low density, high strength, high tenacity and excellent high temperature resistant and antioxidant property.Compared with the high temperature resistant niobium alloy of current use, its outstanding advantages is that quality is light, more than metal loss of weight 5O%; Ablation rate is little, reusable etc.For fiber reinforcement type matrix material, can fiber dispersedly be the Focal point and difficult point of preparation process in matrix batching, is also the key factor that can fiber play toughening effect in matrix.
Summary of the invention
The object of the invention is to improve the bending strength of carborundum porous ceramics, prepare the filtration supporter carborundum porous ceramics that toughness is higher.The present invention finds by experiment repeatedly, adds a certain amount of mullite fiber to can be good at improving the bending strength of carborundum porous ceramics in silicon carbide ceramics mix.And the carborundum porous ceramics sample finally obtaining still has higher void content and good anti-thermal shock fragility, has completed the present invention for this reason.
For achieving the above object, the invention provides following technical scheme:
A kind of fiber reinforcement type carborundum porous ceramics, is characterized in that it is made up of the raw material of following portions by weight:
Vitrified bond 1
Mullite fiber slurry 1-3
Median size is about 230 μ m silicon-carbide particles 8
Pore-forming material 1;
Described mullite fiber slurry refers to by 20%(w/w) mullite fiber; 80%(w/w) carboxymethylcellulose sodium solution raw material composition; Described pore-forming material refers to by 50%(w/w) graphite and 50%(w/w) gac forms;
Described vitrified bond refers to potassium felspar sand 64.53%, kaolin 12.20% and quartz 23.27% composition.
The preparation method of fiber reinforcement type carborundum porous ceramics of the present invention, is characterized in that being undertaken by following step:
(1) preparation of mullite fiber slurry:
A) by 4g Xylo-Mucine and enough deionized water heated and stirred, boil until total solution weight is 200g, obtain 2% carboxymethylcellulose sodium solution;
B) then the mullite fiber of 40g is divided and joined for 5-8 time in CMC solution, the heated and stirred while adding, tentatively spreads out mullite fiber and makes mixed slurry;
C) mixed slurry is mixed with abrading-ball, under the rotating speed of 280 revs/min, ball milling obtains uniform mullite fiber slurry for 5-8 minutes; Wherein the mass ratio of mixed slurry and abrading-ball is 1:1.5;
(2) containing the preparation of the carborundum porous ceramics of mullite fiber
A) first vitrified bond (composition is potassium felspar sand 64.53%, kaolin 12.20% and quartz 23.27%) and mullite fiber slurry are mixed, then add median size to be about the silicon-carbide particle of 230 μ m, and after being uniformly mixed, be put in the baking oven of 80 DEG C and dry 2 hours;
B) add again graphite and gac as pore-forming material at mix obtained in the previous step, and be uniformly mixed;
C) with electric tablet machine, the mix finally obtaining is depressed to carborundum porous ceramics base substrate in the forming pressure of 3MPa, then at the temperature of 1300 DEG C, sintering obtains the carborundum porous ceramics containing mullite fiber;
The more detailed preparation method of the present invention is as follows:
(1) preparation of mullite fiber slurry:
(a) 4g Xylo-Mucine (CMC) and enough deionized waters are boiled until total solution weight is 200g in heated and stirred, obtain 2% carboxymethylcellulose sodium solution.(can add as required the Xylo-Mucine of different amounts, but the concentration of the carboxymethylcellulose sodium solution of final preparation being 2%)
(b) then the mullite fiber of 40g is divided on a small quantity repeatedly (5-8 time) to join in CMC solution, the heated and stirred while adding, tentatively spreads out mullite fiber.(can add as required the mullite fiber of different amounts, but in the carboxymethylcellulose sodium solution of every 100ml2%, need to add the mullite fiber of 20g)
(c) due to mullite fiber in previous step disperse even not, can by this not too uniformly mixed slurry carry out the Ball milling of a nearly step.Wherein the mass ratio of mixed slurry and abrading-ball is 1:1.5, and uses abrading-ball not of uniform size, and under the rotating speed of 280 revs/min, ball milling obtains uniform mullite fiber slurry for 5-8 minutes.
(2) containing the preparation of the carborundum porous ceramics of mullite fiber:
(a) first vitrified bond (main component is potassium felspar sand, kaolin and quartz) and mullite fiber slurry are mixed by the mass ratio of 1:3, then add median size to be about the silicon-carbide particle of 230 μ m, and after being uniformly mixed, be put into and in the baking oven of 80 DEG C, dry about 2 hours to half-dried, wherein every about 20 minutes, take out and stir to ensure that silicon-carbide particle mixing with binding agent and mullite fiber.It is committed step that mullite fiber is uniformly dispersed between binding agent and silicon-carbide particle, and disperseing mullite fiber by aforesaid method and step is key point of the present invention.
(b) in half-dried mix obtained in the previous step, add again graphite and gac as pore-forming material, and be uniformly mixed.In this two step, the mass ratio of silicon-carbide particle, vitrified bond and pore-forming material used is 8:1:1.
(c) with electric tablet machine, the mix finally obtaining being depressed to several length in the forming pressure of 3MPa is 5cm, the wide rectangular parallelepiped carborundum porous ceramics base substrate for 1cm, the thick 0.5cm of being, then at the temperature of 1300 DEG C, sintering obtains the carborundum porous ceramics sample containing mullite fiber, and sintering curre as shown in Figure 1.
Its principle of preparing is: use sintering process to prepare carborundum porous ceramics, taking SiC(silicon carbide) particle is main raw material, obtain vesicular structure by particle packing and the forming hole method that adds pore-forming material, and add vitrified bond to make can effectively link together between silicon-carbide particle.Prepare burden after repressed moulding, in air atmosphere, obtain SiC porous ceramics in 1300 DEG C of sintering.For the lower defect of carborundum porous ceramics bending strength, in carborundum porous ceramics matrix, add mullite fiber to obtain the carborundum porous ceramics that bending strength is higher.
The present invention further discloses the application of fiber reinforcement type carborundum porous ceramics aspect the toughness of preparation raising carborundum porous ceramics.Main contents of the present invention are to prepare fiber reinforcement type carborundum porous ceramics, make bending strength higher carbon SiClx porous ceramics to be applied to gas cleaning at high temperature filtration supporter.The coal that is particularly applied in integrated gasification combined cycle plants (IGCC) generation technology purifies part.
Feature is first to have prepared uniform mullite fiber slurry; when mullite fiber slurry is mixed with binding agent and greater particle size silicon-carbide particle, mullite fiber can spread out equably and not reunite, and plays good toughening effect in ceramic matrix.Use equipment is: electric tablet machine, high temperature sintering furnace, bending strength test instrument.
The chemical agent that the present invention adopts is as follows:
| Reagent name | Purity classification |
| Silicon-carbide particle | Analytical pure |
| Binding agent | Analytical pure |
| Mullite fiber | Analytical pure (Al 2O 3 72%， SiO 2 28%） |
| Xylo-Mucine | Analytical pure |
| Pore-forming material (graphite+gac) | Analytical pure |
The batching of fiber reinforcement type carborundum porous ceramics mainly comprises silicon-carbide particle, mullite fiber, binding agent and pore-forming material, and this institute is 230 μ m by the median size of silicon-carbide particle.
Testing method:
1. the testing method of void content is to use Archimedes's drainage, adopts deionized water as soaking medium.Concrete steps with reference to related data (reference: physical and chemical inspection-physics fascicle. measure the method .2006 of stupalith density and void content thereof, 42 (6): 289-291).
2. bending strength test method is to use bending strength test instrument to survey the mean value of its three-point bending resistance intensity, and span is 40mm, and loading velocity is 0.5mm/min.Concrete test procedure is with reference to standard GB/T/T1965-1996 (reference: National Standard of the People's Republic of China, porous ceramics bending strength test method GB/T1965-1996,1996-09-13 issue, 1997-04-01 enforcement).
3. the test of hot-cracking resistance is sample to be put into High Temperature Furnaces Heating Apparatus be heated to 1000 DEG C then at air naturally cooling, so circulates after 10 times and surveys its bending strength (reference: Ceramics International.Fabrication of Fiber-Reinforced Porous Ceramics of Al2O3-Mullite and SiC-Mullite Systems.21 (1995) 381-384).
experimental data:
| Properties of sample | Void content (%) | Bending strength (MPa) | Hot-cracking resistance (MPa, circulation be heated to for 10 times 1000 DEG C then cooling in air after) | Bending strength rate of descent (%) after hot-cracking resistance test |
| Containing the sample of mullite fiber | 30.36 | 35.66 | 33.75 | 5.4 |
| Do not contain the sample of mullite fiber | 30.84 | 29.72 | 28.16 | 5.2 |
Above result shows: the carborundum porous ceramics that contains mullite fiber is close with the void content of carborundum porous ceramics that does not contain mullite fiber, reach 30%, but the former bending strength is higher by approximately 20% than the latter's bending strength, and has good hot-cracking resistance.Therefore mullite fiber add the bending strength that really can improve carborundum porous ceramics matrix.
The positively effect that the carborundum porous ceramics that prepared by the present invention contain mullite fiber compared with prior art had is:
(1) effectively raise the bending strength of original carborundum porous ceramics matrix, to ensure better carborundum porous ceramics effect in actual applications.
(2) provide a kind of method of preparing the carborundum porous ceramics that bending strength is higher, provide a kind of thinking for develop more high-intensity carborundum porous ceramics later.
(3) contain the carborundum porous ceramics of mullite fiber because there is higher bending strength, therefore can be applied in the more harsh Working environment of condition, expand the practical ranges of carborundum porous ceramics.
Brief description of the drawings:
Fig. 1 is sintering curre;
Fig. 2 is that this tests prepared inorganic coagulation material process flow sheet;
Fig. 3 is the high-temperature dust removal filtration device taking porous filtering pipe as core devices.
Embodiment
For simple and object clearly, below appropriate omission the description of known technology, in order to avoid those unnecessary details affect the description to the technical program.Below in conjunction with preferred embodiment, the present invention will be further described, is illustrated especially, prepares initial substance Xylo-Mucine, the mullite fiber of the compounds of this invention, the composition of vitrified bond all can have been bought from the market." part " in following examples refer to gram or kilogram.Special instruction be below in all examples common component proportion be: vitrified bond: median size is about 230 μ m silicon-carbide particles: pore-forming material=1:8:1(mass ratio), be that ceramic bonding agent content is 10%, it is 80% that median size is about 230 μ m silicon-carbide particle content, Content of Pore-forming Agents is 10%, and wherein pore-forming material is made up of 50% graphite and 50% gac.
Embodiment 1:
First prepare mullite fiber slurry, 4g Xylo-Mucine and enough deionized water heated and stirred are boiled until total solution weight is 200g, obtain 2% carboxymethylcellulose sodium solution, then the mullite fiber of 40g is divided on a small quantity to the joining in 2% CMC solution of repeatedly (5-8 time), preliminary dispersion, then ball milling obtains uniform mullite fiber slurry.
First vitrified bond (main component is potassium felspar sand 64.53%, kaolin 12.20% and quartz 23.27%) and mullite fiber slurry are mixed by the mass ratio of 1:1, then add median size to be about the silicon-carbide particle of 230 μ m, and after being uniformly mixed, be put in the baking oven of 80 DEG C and dry 2 hours to half-dried, add again graphite and gac as pore-forming material, and be uniformly mixed, then in the forming pressure lower sheeting moulding of 3MPa, sintering at the temperature of 1300 DEG C.
Test result is: with the silicon-carbide particle of 230 μ m, add the vitrified bond of massfraction 10% and the mullite fiber slurry identical in quality with binding agent, the pore-forming material (5% graphite+5% gac) of additional massfraction 10%, after 3MPa compacted under 1300 DEG C of sintering, the void content of the supporter making is 29.03%, and bending strength is 32.41MPa
Embodiment 2:
First the mullite fiber slurry of preparation in vitrified bond (main component is potassium felspar sand 64.53%, kaolin 12.20% and quartz 23.27%) and embodiment 1 is mixed by the mass ratio of 1:2, then add median size to be about the silicon-carbide particle of 230 μ m, and after being uniformly mixed, be put in the baking oven of 80 DEG C and dry 2 hours to half-dried, add again graphite and gac as pore-forming material, and be uniformly mixed, then in the forming pressure lower sheeting moulding of 3MPa, sintering at the temperature of 1300 DEG C.
Test result is: with the silicon-carbide particle of 230 μ m, add the mullite fiber slurry of 2 times of the vitrified bond of massfraction 10% and binding agent quality, the pore-forming material (5% graphite+5% gac) of additional massfraction 10%, after 3MPa compacted under 1300 DEG C of sintering, the void content of the supporter making is 30%, and bending strength is 34.91MPa.
Embodiment 3:
First the mullite fiber slurry of preparation in vitrified bond (main component is potassium felspar sand 64.53%, kaolin 12.20% and quartz 23.27%) and embodiment 1 is mixed by the mass ratio of 1:3, then add median size to be about the silicon-carbide particle of 230 μ m, and after being uniformly mixed, be put in the baking oven of 80 DEG C and dry 2 hours to half-dried, add again graphite and gac as pore-forming material, and be uniformly mixed, then in the forming pressure lower sheeting moulding of 3MPa, sintering at the temperature of 1300 DEG C.
Test result is: with the silicon-carbide particle of 230 μ m, add the mullite fiber slurry of 3 times of the vitrified bond of massfraction 10% and binding agent quality, the pore-forming material (5% graphite+5% gac) of additional massfraction 10%, after 3MPa compacted under 1300 DEG C of sintering, the void content of the supporter making is 30.36%, and bending strength is 35.66MPa.
Embodiment 4:
First the mullite fiber slurry of preparation in vitrified bond (main component is potassium felspar sand 64.53%, kaolin 12.20% and quartz 23.27%) and embodiment 1 is mixed by the mass ratio of 1:3, then add median size to be about the silicon-carbide particle of 230 μ m, and after being uniformly mixed, be put in the baking oven of 80 DEG C and dry 2 hours to half-dried, add again graphite and gac as pore-forming material, and be uniformly mixed, then in the forming pressure lower sheeting moulding of 3MPa, sintering at the temperature of 1300 DEG C.
Test result is: with the silicon-carbide particle of 230 μ m, add the mullite fiber slurry of 3 times of the vitrified bond of massfraction 10% and binding agent quality, the pore-forming material (5% graphite+5% gac) of additional massfraction 10%, after 3MPa compacted under 1290 DEG C of sintering, the void content of the supporter making is 29.03%, and bending strength is 35..45MPa.
Embodiment 5:
First the mullite fiber slurry of preparation in vitrified bond (main component is potassium felspar sand 64.53%, kaolin 12.20% and quartz 23.27%) and embodiment 1 is mixed by the mass ratio of 1:3, then add median size to be about the silicon-carbide particle of 230 μ m, and after being uniformly mixed, be put in the baking oven of 80 DEG C and dry 2 hours to half-dried, add again graphite and gac as pore-forming material, and be uniformly mixed, then in the forming pressure lower sheeting moulding of 3MPa, sintering at the temperature of 1300 DEG C.
Test result is: with the silicon-carbide particle of 230 μ m, add the mullite fiber slurry of 3 times of the vitrified bond of massfraction 10% and binding agent quality, the pore-forming material (5% graphite+5% gac) of additional massfraction 10%, after 3MPa compacted under 1310 DEG C of sintering, the void content of the supporter making is 31.23%, and bending strength is 31.35MPa.
Embodiment 6
The practical application of carborundum porous ceramics for gas cleaning at high temperature
In actual gas cleaning at high temperature application, be that carborundum porous ceramics is made to tubular porous ceramic strainer, the coal that is mainly used in integrated gasification combined cycle plants (IGCC) generation technology purifies part.The generating primary process of IGCC is: first coal is converted in vapourizing furnace to coal gas, coal gas is now raw gas, contains a large amount of dust, sulfurous gas, oxynitride, halogen and basic metal etc.This raw gas after convection current is cooled to 370 DEG C of left and right in dry method dust filter high-temperature dust removal, then wet method is sloughed the impurity such as sulphur, oxynitride, halogen, basic metal, the clean coal gas obtaining combustion power generation in the combustion chamber of internal combustion turbine, the high-temperature tail gas of discharging enters waste heat boiler, make it produce water vapour, and then promote steam turbine generating.Coal gas of high temperature dust removal by filtration is the very important part of IGCC power station gas purification function.Fig. 3 has provided in IGCC to organize the schematic diagram of candle shape porous filtering pipe as the high-temperature dust removal filtration device of core devices more.The bottom sealing of this strainer tube, upper end open.Conventionally pipe range 1500mm, pipe external diameter 60mm, internal diameter 40mm, belongs to larger-size rigidity porous filter.As we know from the figure, high temperature dust coal gas enters after strainer, flows to strainer tube inwall, in this course under impressed pressure effect from porous filtering pipe outer wall, dust has been blocked in strainer tube outer wall, and from the inner outflow of strainer tube is to meet the clean coal gas of high temperature that internal combustion turbine requires.Along with strainer tube outer wall ash cake thickness constantly increases, the filtration pressure drop of the inside and outside both sides of strainer tube also increases thereupon.Reach and set after numerical value in filtration pressure drop, system will be carried out pulse backblowing deashing, squeeze into high pressure nitrogen to strainer tube inside, and the ash cake of strainer tube outer wall is removed.Above-mentioned scavenging process periodic cycle.The efficiency of dust collection of this type of tubular porous ceramic strainer almost can reach 99.9%, and this shows that porous material filter has very high dust removal by filtration efficiency.
Claims (3)
1. a fiber reinforcement type carborundum porous ceramics, is characterized in that it is made up of the raw material of following portions by weight:
Vitrified bond 1
Mullite fiber slurry 1-3
Median size is 230 μ m silicon-carbide particles 8
Pore-forming material 1;
Described mullite fiber slurry refers to by 20%(w/w) mullite fiber; 80%(w/w) carboxymethylcellulose sodium solution raw material composition; Described pore-forming material refers to by 50%(w/w) graphite and 50%(w/w) gac forms;
Described vitrified bond refers to potassium felspar sand 64.53%, kaolin 12.20% and quartz 23.27% composition; It is undertaken by following step:
(1) preparation of mullite fiber slurry:
A) by 4g Xylo-Mucine and enough deionized water heated and stirred, boil until total solution weight is 200g, obtain 2% carboxymethylcellulose sodium solution;
B) then the mullite fiber of 40g is divided and joined for 5-8 time in CMC solution, the heated and stirred while adding, tentatively spreads out mullite fiber and makes mixed slurry;
C) mixed slurry is mixed with abrading-ball, under the rotating speed of 280 revs/min, ball milling obtains uniform mullite fiber slurry for 5-8 minutes; Wherein the mass ratio of mixed slurry and abrading-ball is 1:1.5;
(2) containing the preparation of the carborundum porous ceramics of mullite fiber
A) first vitrified bond and mullite fiber slurry are mixed, then adding median size is the silicon-carbide particle of 230 μ m, and after being uniformly mixed, is put in the baking oven of 80 DEG C and dries 2 hours;
B) add again graphite and gac as pore-forming material at mix obtained in the previous step, and be uniformly mixed;
C) with electric tablet machine, the mix finally obtaining is depressed to carborundum porous ceramics base substrate in the forming pressure of 3MPa, then at the temperature of 1300 DEG C, sintering obtains the carborundum porous ceramics containing mullite fiber.
2. the application of fiber reinforcement type carborundum porous ceramics aspect the toughness of preparation raising carborundum porous ceramics described in claim 1.
3. the application of fiber reinforcement type carborundum porous ceramics aspect the coal purification of integrated gasification combined cycle for power generation described in claim 1.
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| CN2656407Y (en) * | 2001-01-22 | 2004-11-17 | 罗五来 | High temp. formed glassfibre reinforced composite material |
| CN1597619A (en) * | 2004-07-19 | 2005-03-23 | 西北工业大学 | Preparation method of whisker and pacticle toughening ceramic base composite |
| CN102718494A (en) * | 2012-06-21 | 2012-10-10 | 海南大学 | Preparation method of composite silicon carbide ceramic filter membrane material |
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