CN103664199A - Method for preparing silicon carbide refractory material by taking polycarbosilane as binding agent - Google Patents
Method for preparing silicon carbide refractory material by taking polycarbosilane as binding agent Download PDFInfo
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- CN103664199A CN103664199A CN201210350387.4A CN201210350387A CN103664199A CN 103664199 A CN103664199 A CN 103664199A CN 201210350387 A CN201210350387 A CN 201210350387A CN 103664199 A CN103664199 A CN 103664199A
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Abstract
The invention discloses a method for preparing a silicon carbide refractory material by taking polycarbosilane as a binding agent. According to the method, a raw material is made up of a silicon carbide precursor, namely, polycarbosilane, as a binding agent, and silicon carbide in grain composition, and the silicon carbide formed through in-situ reaction in the sintering process of polycarbosilane is used as binding phase to ultimately prepare a pure silicon carbide product. The added polycarbosilane plays the role of the binding agent in the pressing process, so that a blank has certain strength, the operability is improved, and meanwhile the polycarbosilane can be converted into silicon carbide in situ in the sintering process, so that the function of binding silicon carbide grains is achieved, and the property of a silicon carbide refractory material product is improved.
Description
Technical field
The present invention relates to a kind of preparation method of carborundum refractory, particularly relate to and a kind ofly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent.
Background technology
The premium propertiess such as hot strength is high, thermal conductivity is high owing to having for carborundum refractory, high temperature resistant, corrosion-resistant and good impact resistance, are widely used in the fields such as high-temperature indirect heating material of various smelting furnace linings, high temperature kiln member, strut member, crucible and non-ferrous metal metallurgy industry.
At present, the preparation of carborundum refractory can be divided into by silica bound according to bond material, with clay combination, with aluminum oxide combination and by silicon nitride bonded silicon.The maximum feature of carborundum refractory is exactly that the conservation rate of at high temperature intensity is high, even can be higher than normal temperature strength.Because the refractoriness of bond material is lower, also can cause the refractoriness of silicon carbide articles to reduce.Therefore the silicon carbide articles that, all belongs to lower grade with the carborundum refractory of silicon-dioxide or clay or aluminum oxide combination.Silicon nitride combined with silicon carbide refractory material is because its resistance to cryolite is used widely in electrolytic aluminum field fortunately.But the method is in preparation limit restriction due to depth of nitration during thicker size goods, easily occur that nitrogenize is not thoroughly and the problem of residual silicon.In addition, silicon nitride decomposes and causes the use temperature of silicon nitride products based on silicon carbide under non-nitrogen atmosphere lower 1300 ℃ of above easily generations.
Preparation from carborundum refractory material can overcome the above problems to a great extent, but be mostly at present to adopt from carborundum refractory material, on the basis of silicon-carbide particle grating, add graphite or other carbonaceous materials and metallic silicon power, in sintering process, make it that reaction in－situ Formed SiClx occurs and realize self combination.Because carbon source and silicon source are difficult to realize consistent being uniformly distributed, usually there is the problem of residual silicon or residual carbon, be unfavorable for the raising of carborundum refractory product properties.Adopting silicon carbide precursor body is bonding agent, carbon element silicon distributes according to certain stoichiometric ratio in presoma, as Polycarbosilane, the homogeneity distributing in silicon-carbide particle like this can be guaranteed, and this all will improve the performance of carborundum refractory goods.
As can be seen here, above-mentioned existing carborundum refractory, in preparation method and use, obviously still has inconvenience and defect, and is urgently further improved.In order to solve the problem of above-mentioned existence, relevant manufacturer there's no one who doesn't or isn't seeks solution painstakingly, but have no for a long time applicable design is completed by development always, and general preparation method does not have appropriate preparation method to address the above problem, this is obviously the problem that the anxious wish of relevant dealer solves.Therefore how to found a kind of new method of preparing carborundum refractory, real one of the current important research and development problem that belongs to, also becoming the current industry utmost point needs improved target.
Summary of the invention
Carborundum refractory or the grade for current existing method, prepared are lower, or the problem that use temperature is not high and thick size goods are difficult to preparation, the object of the invention is to, provide a kind of and new take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, to overcome above-mentioned defect.
The object of the invention to solve the technical problems realizes by the following technical solutions.The Polycarbosilane of take proposing according to the present invention is prepared the method for carborundum refractory as bonding agent, wherein: the silicon carbide precursor body Polycarbosilane of take is bonding agent, and form raw material with the silicon carbide of grain composition, utilize silicon carbide that Polycarbosilane forms by reaction in－situ in sintering process in conjunction with phase, finally prepare pure silicon carbide articles.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Aforesaidly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, it comprises the following steps:
(1) in connection with agent Polycarbosilane, mix in mixing machine with the sic raw material of grain composition;
(2) use forming machine or ramming process that the material mixing is pressed into base substrate, and base substrate is dried in baking oven;
(3) base substrate after drying is placed in to vacuum or inert atmosphere stove carries out sintering.
Aforesaidly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, wherein: the silicon carbide specification of described grain composition is respectively: granularity 1.43～2.5mm, purity > 99%; Granularity 0.5～1.43mm, purity > 98%; Granularity 240 orders, purity > 98%; Granularity 2000 orders, purity > 97%.
Aforesaidly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, wherein: the mass ratio that the Polycarbosilane bonding agent adding accounts for raw material is 3～10%; The mass ratio that silicon carbide four kinds of raw materials from coarse to fine of described grain composition account for raw material is respectively: 55～67%, 5～10%, 15～20%, 5～10%.
Aforesaidly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, wherein: in step (1), the mixing time is 5～20min in mixing machine.
Aforesaidly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, wherein: step is dried 4～12h by base substrate in (2) in the baking oven of 80～110 ℃.
Aforesaidly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, wherein: in step (3), sintering temperature is 1300～1500 ℃, and heat preservation sintering 1～5h.
By technique scheme, the present invention be take the method that Polycarbosilane prepares carborundum refractory as bonding agent and is at least had following advantages and beneficial effect: carbon element silicon distributes according to certain stoichiometric ratio in bonding agent Polycarbosilane, its homogeneity distributing in silicon-carbide particle can be guaranteed, more be conducive to improve the level of response of reaction in－situ, avoided due to the skewness of carbon element silicon, easily occurring the problem of residual silicon or residual carbon in the past, be conducive to the raising of carborundum refractory product properties.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technique means of the present invention, and can be implemented according to the content of specification sheets, and for above and other object of the present invention, feature and advantage can be become apparent, below especially exemplified by preferred embodiment, and coordinate accompanying drawing, be described in detail as follows.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the prepared carborundum refractory of the embodiment of the present invention 1.
Fig. 2 is the fracture apperance photo of the prepared carborundum refractory of the embodiment of the present invention 1.
Embodiment
For further setting forth the present invention, reach technique means and the effect that predetermined goal of the invention is taked, below in conjunction with accompanying drawing and preferred embodiment, the Polycarbosilane of take proposing according to the present invention is prepared to its embodiment of method, working method, step, feature and the effect thereof of carborundum refractory as bonding agent, be described in detail as follows.
It is bonding agent that silicon carbide precursor body Polycarbosilane is take in the present invention, and forms raw material with the silicon carbide of grain composition, utilizes silicon carbide that Polycarbosilane forms by reaction in－situ in sintering process in conjunction with phase, finally prepares pure silicon carbide articles.The Polycarbosilane adding plays the effect of bonding agent in pressing process, makes base substrate have certain intensity, has improved its operability.Polycarbosilane can situ converting be silicon carbide in sintering process simultaneously, plays the effect of silicon carbide particle, has improved the performance of silicon carbide articles.
In more detail, aforesaidly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, it comprises the following steps:
(1) in connection with agent Polycarbosilane, mix in mixing machine with the sic raw material of grain composition;
(2) use forming machine or ramming process that the material mixing is pressed into base substrate, and base substrate is dried in baking oven;
(3) base substrate after drying is placed in to vacuum or inert atmosphere stove carries out sintering.
Preferably, the silicon carbide specification of described grain composition is respectively: granularity 1.43～2.5mm, and purity > 99%; Granularity 0.5～1.43mm, purity > 98%; Granularity 240 orders, purity > 98%; Granularity 2000 orders, purity > 97%.
More preferably, the mass ratio that the Polycarbosilane bonding agent adding accounts for raw material is 3～10%; The mass ratio that silicon carbide four kinds of raw materials from coarse to fine of described grain composition account for raw material is respectively: 55～67%, 5～10%, 15～20%, 5～10%.
Preferably, in abovementioned steps (1), in mixing machine, the mixing time is 5～20min; Step is dried 4～12h by base substrate in (2) in the baking oven of 80～110 ℃; In step (3), sintering temperature is 1300～1500 ℃, and heat preservation sintering 1～5h.
Take Polycarbosilane as bonding agent, and form raw material with the silicon-carbide particle (granularity is respectively 1.43～2.5mm, 0.5～1.43mm, 240 orders, 2000 orders) of grain composition, be respectively by mass percentage 3%, 67%, 10%, 15%, 5% ratio is weighed.Above raw material is mixed on planetary Forced Mixing machine 10min, makes base substrate by the material mechanical pressing mixing, and then base substrate is dried to 6h in the baking oven of 100 ℃.Sample after drying is placed in vacuum oven, at 1300 ℃, is incubated 5h sintering.Refer to Fig. 1, the thing phase composite that XRD detects goods is mainly silicon carbide phase, a small amount of Si
2n
2o is because sample slight oxidation in sintering process causes; Refer to Fig. 2, presoma forms a large amount of fibrous nano whiskers in goods inside after sintering; Goods body is close is 2.55gcm
-3, folding strength is 30.6MPa.
Take Polycarbosilane as bonding agent, and form raw material with the silicon-carbide particle (granularity is respectively 1.43～2.5mm, 0.5～1.43mm, 240 orders, 2000 orders) of grain composition, be respectively by mass percentage 7%, 60%, 8%, 16%, 9% ratio is weighed.Above raw material is mixed on planetary Forced Mixing machine 20min, makes base substrate by the material ramming process mixing, and then base substrate is dried to 4h in the baking oven of 110 ℃.Sample after drying is placed in argon gas atmosphere stove, at 1500 ℃, is incubated 1h sintering.The thing phase composite that XRD detects goods is mainly silicon carbide phase, and goods body is close is 2.58gcm
-3, folding strength is 31.1MPa.
Embodiment 3
Take Polycarbosilane as bonding agent, and form raw material with the silicon-carbide particle (granularity is respectively 1.43～2.5mm, 0.5～1.43mm, 240 orders, 2000 orders) of grain composition, be respectively by mass percentage 10%, 55%, 5%, 20%, 10% ratio is weighed.Above raw material is mixed on planetary Forced Mixing machine 5min, makes base substrate by the material mechanical pressing mixing, and then base substrate is dried to 12h in the baking oven of 80 ℃.Sample after drying is placed in vacuum oven, at 1400 ℃, is incubated 3h sintering.The thing phase composite that XRD detects goods is mainly silicon carbide phase, and goods body is close is 2.6gcm
-3, folding strength is 35.4MPa.
The above, it is only preferred embodiment of the present invention, not the present invention is done to any pro forma restriction, although the present invention discloses as above with preferred embodiment, yet not in order to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, when can utilizing the technology contents of above-mentioned announcement to make a little change or being modified to the equivalent embodiment of equivalent variations, in every case be not depart from technical solution of the present invention content, any simple modification of above embodiment being done according to technical spirit of the present invention, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (7)
1. take Polycarbosilane and prepare the method for carborundum refractory as bonding agent for one kind, it is characterized in that: the silicon carbide precursor body Polycarbosilane of take is bonding agent, and form raw material with the silicon carbide of grain composition, utilize silicon carbide that Polycarbosilane forms by reaction in－situ in sintering process in conjunction with phase, finally prepare pure silicon carbide articles.
2. according to claim 1ly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, it is characterized in that it comprises the following steps:
(1) in connection with agent Polycarbosilane, mix in mixing machine with the sic raw material of grain composition;
(2) use forming machine or ramming process that the material mixing is pressed into base substrate, and base substrate is dried in baking oven;
(3) base substrate after drying is placed in to vacuum or inert atmosphere stove carries out sintering.
3. according to claim 1 and 2ly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, it is characterized in that: the silicon carbide specification of described grain composition is respectively: granularity 1.43～2.5mm, purity > 99%; Granularity 0.5～1.43mm, purity > 98%; Granularity 240 orders, purity > 98%; Granularity 2000 orders, purity > 97%.
4. according to claim 1 and 2ly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, it is characterized in that: the mass ratio that the Polycarbosilane bonding agent adding accounts for raw material is 3～10%; The mass ratio that silicon carbide four kinds of raw materials from coarse to fine of described grain composition account for raw material is respectively: 55～67%, 5～10%, 15～20%, 5～10%.
5. according to claim 2ly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, it is characterized in that: in step (1), the mixing time is 5～20min in mixing machine.
6. according to claim 2ly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, it is characterized in that: step is dried 4～12h by base substrate in (2) in the baking oven of 80～110 ℃.
7. according to claim 2ly take Polycarbosilane and prepare the method for carborundum refractory as bonding agent, it is characterized in that: in step (3), sintering temperature is 1300～1500 ℃, and heat preservation sintering 1～5h.
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Cited By (9)
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| CN103864446A (en) * | 2014-03-27 | 2014-06-18 | 中钢集团洛阳耐火材料研究院有限公司 | Silicon carbide bonded carbon-containing fireproof material and preparation method thereof |
| CN104177113A (en) * | 2014-08-08 | 2014-12-03 | 苏州宏久航空防热材料科技有限公司 | SiC bonded ceramic matrix composite material and preparation method thereof |
| CN106336218A (en) * | 2016-08-17 | 2017-01-18 | 山东大学 | Preparation method of high-compactness silicon carbide ceramic |
| CN107188586A (en) * | 2017-07-19 | 2017-09-22 | 合肥铭佑高温技术有限公司 | A kind of preparation method of anti-oxidation refractory material |
| CN107324818A (en) * | 2017-06-13 | 2017-11-07 | 长兴华悦耐火材料厂 | A kind of Tercod and preparation method thereof |
| CN109851362A (en) * | 2018-12-29 | 2019-06-07 | 哈尔滨理工大学 | A kind of 3D molding preparation SiCfThe method of/SiC ceramic composite material |
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| CN113754440A (en) * | 2021-10-29 | 2021-12-07 | 郑州航空工业管理学院 | SiC ceramic material and preparation method thereof |
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| CN102030532A (en) * | 2010-11-09 | 2011-04-27 | 浙江大学 | Surface microporous SiC ceramic material and preparation method thereof |
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| CN102030532A (en) * | 2010-11-09 | 2011-04-27 | 浙江大学 | Surface microporous SiC ceramic material and preparation method thereof |
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Cited By (12)
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| CN103864446A (en) * | 2014-03-27 | 2014-06-18 | 中钢集团洛阳耐火材料研究院有限公司 | Silicon carbide bonded carbon-containing fireproof material and preparation method thereof |
| CN103864446B (en) * | 2014-03-27 | 2015-09-16 | 中钢集团洛阳耐火材料研究院有限公司 | Silicon carbide is in conjunction with carbon containing refractory and preparation method |
| CN104177113A (en) * | 2014-08-08 | 2014-12-03 | 苏州宏久航空防热材料科技有限公司 | SiC bonded ceramic matrix composite material and preparation method thereof |
| CN106336218A (en) * | 2016-08-17 | 2017-01-18 | 山东大学 | Preparation method of high-compactness silicon carbide ceramic |
| CN107324818A (en) * | 2017-06-13 | 2017-11-07 | 长兴华悦耐火材料厂 | A kind of Tercod and preparation method thereof |
| CN107188586A (en) * | 2017-07-19 | 2017-09-22 | 合肥铭佑高温技术有限公司 | A kind of preparation method of anti-oxidation refractory material |
| CN109851362A (en) * | 2018-12-29 | 2019-06-07 | 哈尔滨理工大学 | A kind of 3D molding preparation SiCfThe method of/SiC ceramic composite material |
| CN109851362B (en) * | 2018-12-29 | 2021-09-17 | 哈尔滨理工大学 | SiC prepared by 3D formingfMethod for preparing/SiC ceramic composite material |
| CN111102844A (en) * | 2019-12-12 | 2020-05-05 | 湖南太子新材料科技有限公司 | Preparation method of sagger for sintering lithium battery positive electrode material |
| CN113880590A (en) * | 2021-09-07 | 2022-01-04 | 山东工业陶瓷研究设计院有限公司 | Composite ceramic material and preparation method thereof |
| CN113754440A (en) * | 2021-10-29 | 2021-12-07 | 郑州航空工业管理学院 | SiC ceramic material and preparation method thereof |
| CN113754440B (en) * | 2021-10-29 | 2023-08-22 | 郑州航空工业管理学院 | SiC ceramic material and preparation method thereof |
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