CN102557722A - Method for preparing porous silicon carbide ceramic by using pore-forming agent - Google Patents
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Abstract
The invention discloses a method for preparing porous silicon carbide ceramic by using a pore-forming agent. The method comprises the following steps of: (1) mixing silicon carbide powder and carbon powder, adding phenolic resin, mixing, performing compression molding under the pressure of 2 to 4MPa, and drying for 1 to 3 hours in a baking oven at the temperature of between 80 and 120 DEG C to obtain a green body; (2) putting the green body into a crucible paved with silicon powder, sintering at the temperature of 1,550 to 1,650 DEG C for 0.5 to 3 hours under the condition that the vacuum degree is 0.01 to 0.1Pa, and discharging silicon at the temperature of 1,600 to 1,650 DEG C to obtain a sintered body; and (3) calcining the sintered body in an oxygen furnace at the temperature of between 850 and 900 DEG C for 1 to 4 hours. The porous silicon carbide ceramic with the porosity of 70 percent is obtained by the method comprising the steps of infiltrating a small amount of Si into a pressed body of the SiC and the pore-forming agent, namely the carbon powder to ensure that the Si and the pressed body are combined, discharging the Si, and calcining in the oxygen furnace at the temperature of 850 DEG C.
Description
Technical field
The present invention relates to utilize the pore-forming material carbon dust to combine and prepare the method for porous silicon carbide ceramic, improve the technical field of porous silicon carbide ceramic porosity through reaction infiltration and low temperature calcination technology.
Background technology
Ceramic foam has actual application prospect very widely, like the strainer as molten metal or hot gas, microbe filters such as the germ of clinical medicine, ultra-filtration and separation serum proteins; The filtering membrane of chemical reaction process; The carrier of catalyzer or enzyme etc.The SiC ceramic foam filtering material that this project is developed has good use properties.
Carborundum porous ceramics is the new function material that a lot of holes are arranged in a kind of internal structure.Owing to have low density, HS, high porosity, hypertonicity, big, anticorrosive, anti-oxidant, good characteristics such as thermal insulation, heat-shock resistance and high thermal resistance of specific surface area, carborundum porous ceramics in the general industry field and high-tech area obtained application more and more widely.For example, can be used as solid particle filter, filter for molten metal, heat exchanger, transmitter, insulation and the sound-proof material of high temperature gas cleaning device, diesel emission, the support of the catalyst of vehicle exhaust etc.In addition, they also have the potential application prospect in the bio-medical field.The application of carborundum porous ceramics material has spreaded all over a plurality of fields such as metallurgy, chemical industry, electronics, the energy, aviation, environmental protection, biology.
The preparation carborundum porous ceramics has the kinds of processes method, comprises adding pore-forming material technology, foam process, foam impregnation technology, sol-gel technology etc.Wherein adding the pore-forming material method is in sintering process, and pore-forming material volatilization or decomposition are left matrix and stayed the process method that pore prepares ceramic foam.
Traditional interpolation pore-forming material method, in sintering process, the general employing do not have the well-oxygenated environment of pressure sintering, in order to improve performance of products, adds a certain amount of aluminium powder, aluminum oxide, yttrium oxide etc. usually as sintering aid.With the rising of sintering temperature, sintered compact compactness is high more, thereby void content is descended.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who obtains high porosity and high-intensity carborundum porous ceramics.Use SiC and pore-forming material carbon dust to mix, add a small amount of resol as caking agent, and be pressed into blank, after the infiltration minor amount of silicon, then incinerating way in 850 ℃ of oxygen furnace prepares porous silicon carbide ceramic in vacuum resistance furnace.
Technical scheme of the present invention is: a kind of method of using pore-forming material to prepare porous silicon carbide ceramic, and its step is following:
(1) carbon dust of the carborundum powder of 30-95 weight part, 5-70 weight part is mixed after; Add the resol remix; The add-on of resol is the 3-6% of carborundum powder and carbon dust gross weight; In the moulding of 2-4MPa pressure pressed, be oven dry 1-3 hour in 80-120 ℃ the baking oven at temperature condition then, process green compact;
(2) green compact are put into the crucible that is covered with silica flour; The weight of silica flour is the 4-12% of carborundum powder and carbon dust gross weight, and crucible is put into vacuum oven, is in 1550-1650 ℃ of sintering 0.5-3 hour in vacuum tightness under the condition of 0.01-0.1Pa; And, process sintered blank in 1600-1650 ℃ of row's silicon;
(3) sintered blank was calcined 1-4 hour in 850-900 ℃ oxygen furnace.
The order number of said carborundum powder and carbon dust is the 200-800 order.
The invention has the beneficial effects as follows: use carbon dust as pore-forming material, the quantity of hole can control through the massfraction of pore-forming material like this; The carbon in a spot of resol and the carbon dust of adding generate the silit phase of secondary in the minor amount of silicon reaction that high temperature and infiltration get into, and silicon-carbide particle are connected form the porous material skeleton; Low temperature calcination is removed unnecessary a large amount of carbon dust, thereby forms hole.Through a small amount of Si of infiltration in SiC, pore-forming material carbon dust pressed compact, after making it to combine, row Si and incinerating way in 850 ℃ of oxygen furnace subsequently, obtaining porosity is the porous silicon carbide ceramic more than 70%.Gained porous silicon carbide ceramic pore dimension of the present invention is controlled, porosity is adjustable, be fit to technical scale.The present invention utilizes carborundum powder and carbon dust, and infiltration silicon under vacuum atmosphere adopts the method for low temperature calcination to prepare the porous silicon carbide ceramic material then.Prescription is simple, and porosity is high, and intensity is high, the characteristics of erosion resistance and Heat stability is good.
Embodiment
Embodiment 1
With the 400 purpose SiC powder of 30g and the 400 order C powder uniform mixing of 20g, hybrid mode is wet mixing, makees solvent with alcohol; Mixed 3 hours; And then the resol of adding 2g, and mixed 2 hours, with above stamping of powder moulding; Selecting pressing pressure for use is 2MPa, puts into baking oven then and solidifies 40 minutes in 120 ℃; Above-mentioned sample is placed the crucible of the Si powder that is covered with 5g, be transferred to vacuum sintering furnace, vacuum tightness was 0.01Pa, about 40 minutes of 1550 ℃ of infiltration Si; Be warming up to 1650 ℃ then, about 10 minutes of the row of vacuumizing Si, furnace cooling takes out sample; Then said sample is positioned in the resistance furnace,,, obtains the carborundum porous ceramics material remaining C oxygenolysis in 850 ℃ of sintering 1.5 hours.Porosity is 75%.
Embodiment 2
With the 400 purpose SiC powder of 40g and the 400 order C powder uniform mixing of 30g.Hybrid mode is wet mixing, makees solvent with alcohol, mixes 6 hours, and then adds the resol of 3g, and mixed 3 hours, and with above stamping of powder moulding, selecting pressing pressure for use is 2MPa, puts into baking oven then and solidifies 50 minutes in 120 ℃; Above-mentioned sample is placed the crucible of the Si powder that is covered with 6g, be transferred to vacuum sintering furnace, vacuum tightness is 10
-2Pa was about 40 minutes of 1550 ℃ of infiltration Si; Be warming up to 1650 ℃ then, about 10 minutes of the row of vacuumizing Si, furnace cooling takes out sample; Then said sample is positioned in the resistance furnace, in 850 ℃ of sintering 2.5 hours, with remaining C oxygenolysis.Obtain the carborundum porous ceramics material.Porosity is 70%.
Embodiment 3
A kind of method of using pore-forming material to prepare porous silicon carbide ceramic is characterized in that its step is following:
(1) being that 200 purpose carborundum powders, 5g order number are after 200 purpose carbon dusts mix with 30 g order numbers, adding 1.1g resol remix, in the moulding of 2MPa pressure pressed, is oven dry 1-3 hour in 80 ℃ the baking oven at temperature condition then, processes green compact;
(2) green compact are put into the crucible that is covered with the 1.4g silica flour, crucible are put into vacuum oven, in vacuum tightness be under the condition of 0.01Pa in 1550 ℃ of sintering 0.5-3 hours, and, process sintered blank in 1600 ℃ of row's silicon;
(3) sintered blank was calcined 1 hour in 850 ℃ oxygen furnace, obtain the carborundum porous ceramics material, porosity is 72%.
Embodiment 4
A kind of method of using pore-forming material to prepare porous silicon carbide ceramic is characterized in that its step is following:
(1) being that 800 purpose carborundum powders, 70g order number are after 800 purpose carbon dusts mix with 95g order number, adding 9g resol remix, in the moulding of 4MPa pressure pressed, is oven dry 3 hours in 120 ℃ the baking oven at temperature condition then, processes green compact;
(2) green compact are put into the crucible that is covered with the 19g silica flour, crucible are put into vacuum oven, in vacuum tightness be under the condition of 0.1Pa in 1650 ℃ of sintering 0.5-3 hours, and, process sintered blank in 1650 ℃ of row's silicon;
(3) sintered blank was calcined 4 hours in 900 ℃ oxygen furnace, obtain the carborundum porous ceramics material, porosity is 72%.
Embodiment 5
A kind of method of using pore-forming material to prepare porous silicon carbide ceramic is characterized in that its step is following:
(1) being that 400-600 purpose carborundum powder, 50g order number are after 400-600 purpose carbon dust mixes with 50g order number, adding 5g resol remix, in the moulding of 3MPa pressure pressed, is oven dry 2 hours in 100 ℃ the baking oven at temperature condition then, processes green compact;
(2) green compact are put into the crucible that is covered with the 10g silica flour, crucible are put into vacuum oven, in vacuum tightness be under the condition of 0.05Pa in 1600 ℃ of sintering 2 hours, and, process sintered blank in 1600 ℃ of row's silicon;
(3) sintered blank was calcined 2 hours in 900 ℃ oxygen furnace, obtain the carborundum porous ceramics material, porosity is 73%.
Embodiment 6
A kind of method of using pore-forming material to prepare porous silicon carbide ceramic is characterized in that its step is following:
(1) be that 200-800 purpose carborundum powder, 5-70g order number are after 200-800 purpose carbon dust mixes with 30-95g order number; The order number is the 200-800 order; Add the resol remix, the add-on of resol is the 3-6% of carborundum powder and carbon dust gross weight, in the moulding of 2-4MPa pressure pressed; Be oven dry 1-3 hour in 80-120 ℃ the baking oven at temperature condition then, process green compact;
(2) green compact are put into the crucible that is covered with silica flour; The weight of silica flour is the 4-12% of carborundum powder and carbon dust gross weight, and crucible is put into vacuum oven, is in 1550-1650 ℃ of sintering 0.5-3 hour in vacuum tightness under the condition of 0.01-0.1Pa; And, process sintered blank in 1600-1650 ℃ of row's silicon;
(3) sintered blank was calcined 1-4 hour in 850-900 ℃ oxygen furnace.
Claims (2)
1. method of using pore-forming material to prepare porous silicon carbide ceramic is characterized in that its step is following:
(1) carbon dust of the carborundum powder of 30-95 weight part, 5-70 weight part is mixed after; Add the resol remix; The add-on of resol is the 3-6% of carborundum powder and carbon dust gross weight; In the moulding of 2-4MPa pressure pressed, be oven dry 1-3 hour in 80-120 ℃ the baking oven at temperature condition then, process green compact;
(2) green compact are put into the crucible that is covered with silica flour; The weight of silica flour is the 4-12% of carborundum powder and carbon dust gross weight, and crucible is put into vacuum oven, is in 1550-1650 ℃ of sintering 0.5-3 hour in vacuum tightness under the condition of 0.01-0.1Pa; And, process sintered blank in 1600-1650 ℃ of row's silicon;
(3) sintered blank was calcined 1-4 hour in 850-900 ℃ oxygen furnace.
2. use pore-forming material according to claim 1 prepares the method for porous silicon carbide ceramic, it is characterized in that: the order number of said carborundum powder and carbon dust is the 200-800 order.
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| CN103771858A (en) * | 2014-01-07 | 2014-05-07 | 中原工学院 | Method for preparing porous silicon carbide ceramic employing activated carbon silicification method |
| CN104072190A (en) * | 2014-07-11 | 2014-10-01 | 浙江理工大学 | Preparation method of SiC porous ceramic |
| CN104451319A (en) * | 2014-11-20 | 2015-03-25 | 中原工学院 | Method for preparing Mo (Si, al)2-SiC cermet composite material by reactive infiltration method |
| CN104451320A (en) * | 2014-11-20 | 2015-03-25 | 中原工学院 | Method of preparing Mo(Si,Al)-2-SiC metal ceramic composite material through reaction method |
| CN104989822A (en) * | 2015-06-17 | 2015-10-21 | 宁波东联密封件有限公司 | Mechanical sealing device for kettle |
| CN106187195A (en) * | 2016-06-29 | 2016-12-07 | 华中科技大学 | Use the method that selective laser sintering technique prepares silicon carbide ceramics |
| CN106478105A (en) * | 2016-09-26 | 2017-03-08 | 西安交通大学 | A kind of method that multistep reaction sintering process prepares the thyrite of low residual silicon |
| CN106588085A (en) * | 2016-12-22 | 2017-04-26 | 哈尔滨工业大学 | Method for preparing high-temperature-resistant structural SiC porous ceramics |
| CN107098702A (en) * | 2017-04-21 | 2017-08-29 | 中国航发北京航空材料研究院 | A kind of preparation method of near-net-shape silicon carbide reaction-sintered material |
| CN107399988A (en) * | 2017-08-22 | 2017-11-28 | 东北大学 | A kind of method for preparing alumina carbon SiClx composite porous ceramic using aluminium silicon systems industrial residue |
| CN107686369A (en) * | 2017-08-22 | 2018-02-13 | 东北大学 | A kind of method for preparing carborundum porous ceramics with the carborundum cutting waste material of crystalline silicon |
| CN108002837A (en) * | 2017-11-22 | 2018-05-08 | 永安市鼎丰碳素科技有限公司 | A kind of preparation method of cheap boracic carbon brick |
| CN109678513A (en) * | 2018-12-15 | 2019-04-26 | 中国科学院长春光学精密机械与物理研究所 | A method of it is fine and close based on rarefaction defect reaction-sintering SIC material |
| CN110526713A (en) * | 2019-08-27 | 2019-12-03 | 广东工业大学 | A kind of porous silicon carbide ceramic and its preparation method and application |
| CN110590381A (en) * | 2018-06-12 | 2019-12-20 | 睿健邦生医股份有限公司 | Sintering control method of ceramic material |
| CN113481603A (en) * | 2021-08-02 | 2021-10-08 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of PVT method silicon carbide crystal growth raw material |
| CN114685179A (en) * | 2020-12-29 | 2022-07-01 | 中国科学院上海硅酸盐研究所 | Preparation method of silicon carbide ceramic matrix composite based on infiltration preform pore structure regulation |
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| CN103771858A (en) * | 2014-01-07 | 2014-05-07 | 中原工学院 | Method for preparing porous silicon carbide ceramic employing activated carbon silicification method |
| CN104072190A (en) * | 2014-07-11 | 2014-10-01 | 浙江理工大学 | Preparation method of SiC porous ceramic |
| CN104072190B (en) * | 2014-07-11 | 2016-03-30 | 浙江理工大学 | A kind of preparation method of SiC porous ceramics |
| CN104451320A (en) * | 2014-11-20 | 2015-03-25 | 中原工学院 | Method of preparing Mo(Si,Al)-2-SiC metal ceramic composite material through reaction method |
| CN104451319A (en) * | 2014-11-20 | 2015-03-25 | 中原工学院 | Method for preparing Mo (Si, al)2-SiC cermet composite material by reactive infiltration method |
| CN104989822A (en) * | 2015-06-17 | 2015-10-21 | 宁波东联密封件有限公司 | Mechanical sealing device for kettle |
| CN106187195A (en) * | 2016-06-29 | 2016-12-07 | 华中科技大学 | Use the method that selective laser sintering technique prepares silicon carbide ceramics |
| CN106187195B (en) * | 2016-06-29 | 2018-11-30 | 华中科技大学 | The method that silicon carbide ceramics are prepared using selective laser sintering technique |
| CN106478105B (en) * | 2016-09-26 | 2019-04-09 | 西安交通大学 | A kind of method that multistep reaction sintering process prepares the thyrite of low residual silicon |
| CN106478105A (en) * | 2016-09-26 | 2017-03-08 | 西安交通大学 | A kind of method that multistep reaction sintering process prepares the thyrite of low residual silicon |
| CN106588085A (en) * | 2016-12-22 | 2017-04-26 | 哈尔滨工业大学 | Method for preparing high-temperature-resistant structural SiC porous ceramics |
| CN106588085B (en) * | 2016-12-22 | 2019-07-16 | 哈尔滨工业大学 | A kind of preparation method of high-temperature-resistant structure type SiC porous ceramics |
| CN107098702A (en) * | 2017-04-21 | 2017-08-29 | 中国航发北京航空材料研究院 | A kind of preparation method of near-net-shape silicon carbide reaction-sintered material |
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| CN107686369A (en) * | 2017-08-22 | 2018-02-13 | 东北大学 | A kind of method for preparing carborundum porous ceramics with the carborundum cutting waste material of crystalline silicon |
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| CN108002837A (en) * | 2017-11-22 | 2018-05-08 | 永安市鼎丰碳素科技有限公司 | A kind of preparation method of cheap boracic carbon brick |
| CN108002837B (en) * | 2017-11-22 | 2020-12-25 | 永安市鼎丰碳素科技有限公司 | Preparation method of low-cost boron-containing carbon brick |
| CN110590381A (en) * | 2018-06-12 | 2019-12-20 | 睿健邦生医股份有限公司 | Sintering control method of ceramic material |
| CN109678513A (en) * | 2018-12-15 | 2019-04-26 | 中国科学院长春光学精密机械与物理研究所 | A method of it is fine and close based on rarefaction defect reaction-sintering SIC material |
| CN110526713A (en) * | 2019-08-27 | 2019-12-03 | 广东工业大学 | A kind of porous silicon carbide ceramic and its preparation method and application |
| CN110526713B (en) * | 2019-08-27 | 2022-03-11 | 广东工业大学 | Porous silicon carbide ceramic and preparation method and application thereof |
| CN114685179A (en) * | 2020-12-29 | 2022-07-01 | 中国科学院上海硅酸盐研究所 | Preparation method of silicon carbide ceramic matrix composite based on infiltration preform pore structure regulation |
| CN113481603A (en) * | 2021-08-02 | 2021-10-08 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of PVT method silicon carbide crystal growth raw material |
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Application publication date: 20120711 |