CN103664199B - Take Polycarbosilane as the method that carborundum refractory prepared by bonding agent - Google Patents

Take Polycarbosilane as the method that carborundum refractory prepared by bonding agent Download PDF

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CN103664199B
CN103664199B CN201210350387.4A CN201210350387A CN103664199B CN 103664199 B CN103664199 B CN 103664199B CN 201210350387 A CN201210350387 A CN 201210350387A CN 103664199 B CN103664199 B CN 103664199B
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silicon carbide
polycarbosilane
bonding agent
raw
granularity
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CN103664199A (en
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蔡泽
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Luoyang Shenjia Kiln Co., Ltd.
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LUOYANG XINJUNENG HIGH ENERGY TECHNOLOGY Co Ltd
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Abstract

The invention relates to that a kind of take Polycarbosilane as the method that carborundum refractory prepared by bonding agent, it is for bonding agent with silicon carbide precursor Polycarbosilane, and form raw material with the silicon carbide of grain composition, the silicon carbide utilizing Polycarbosilane to be formed by reaction in-situ in sintering process in conjunction with phase, the pure silicon carbide articles of final preparation.The Polycarbosilane added plays the effect of bonding agent in pressing process, base substrate is made to have certain intensity, improve its operability, Polycarbosilane can situ converting be silicon carbide in sintering process simultaneously, play the effect of silicon carbide particle, improve the performance of carborundum refractory goods.

Description

Take Polycarbosilane as the method that carborundum refractory prepared by bonding agent
Technical field
The present invention relates to a kind of preparation method of carborundum refractory, particularly relating to a kind of take Polycarbosilane as the method that carborundum refractory prepared by 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 field such as high-temperature indirect heating material of various smelting furnace lining, high temperature kiln component, 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, combines with clay, combine with aluminum oxide 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 higher than normal temperature strength.Because the refractoriness of bond material is lower, the refractoriness of silicon carbide articles also can be caused to reduce.Therefore, the silicon carbide articles of lower grade is all belonged to the carborundum refractory that silicon-dioxide or clay or aluminum oxide combine.Silicon nitride combined with silicon carbide refractory material is used widely in electrolytic aluminum field fortunately due to its resistance to cryolite.But the method limit due to the limit of depth of nitration when preparing thicker gauge articles, easily there is the problem of the saturating and residual silicon of nitrogenize.In addition, silicon nitride easily occurs to decompose to cause the use temperature of silicon nitride products based on silicon carbide under non-nitrogen atmosphere lower more than 1300 DEG C.
Can overcome the above problems to a great extent from the preparation of carborundum refractory material, but mostly at present from carborundum refractory material is adopt to add graphite or other carbonaceous materials and metallic silicon power on the basis of silicon-carbide particle grating, in sintering process, makes it that reaction in-situ Formed SiClx occurs and realize self and combine.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.Employing silicon carbide precursor is bonding agent, carbon element silicon distributes according to certain stoichiometric ratio in presoma, as Polycarbosilane, the homogeneity distributed 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 with in use in preparation method, obviously still has inconvenience and defect, and is urgently further improved.In order to solve above-mentioned Problems existing, relevant manufactures there's no one who doesn't or isn't seeks solution painstakingly, but have no applicable design for a long time to be completed by development always, and general preparation method does not have appropriate preparation method to solve the problem, this is obviously the anxious problem for solving of relevant dealer.Therefore how to found a kind of method preparing carborundum refractory newly, one of current important research and development problem of real genus, also becomes the target that current industry pole need be improved.
Summary of the invention
The carborundum refractory prepared for current existing method or grade lower, or use temperature is not high and thick gauge articles be difficult to prepare problem, the object of the invention is to, there is provided a kind of newly take Polycarbosilane as the method that carborundum refractory prepared by bonding agent, to overcome above-mentioned defect.
The object of the invention to solve the technical problems realizes by the following technical solutions.Is the method that carborundum refractory prepared by bonding agent according to the present invention's proposition with Polycarbosilane, and it comprises the following steps:
(1) with silicon carbide precursor Polycarbosilane for bonding agent, form raw material with the silicon carbide of grain composition, raw material mixed in mixing machine;
(2) use forming machine or ramming process that the material mixed is pressed into base substrate, and base substrate is dried 4 ~ 12h in the baking oven of 80 ~ 110 DEG C;
(3) base substrate after drying is placed in vacuum or inert atmosphere stove sinters in 1300 ~ 1500 DEG C, and heat preservation sintering 1 ~ 5h, the silicon carbide utilizing Polycarbosilane to be formed by reaction in-situ in sintering process in conjunction with phase, the pure silicon carbide articles of final preparation.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Aforesaid take Polycarbosilane as the method that carborundum refractory prepared by 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 order, purity >98%; Granularity 2000 order, purity >97%.
Aforesaid take Polycarbosilane as the method that carborundum refractory prepared by bonding agent, wherein: the mass ratio that the Polycarbosilane bonding agent added 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%.
By technique scheme, the present invention is that the method that carborundum refractory prepared by bonding agent at least has following advantages and beneficial effect with Polycarbosilane: carbon element silicon distributes according to certain stoichiometric ratio in bonding agent Polycarbosilane, the homogeneity making it distribute in silicon-carbide particle can be guaranteed, more be conducive to the level of response improving reaction in-situ, avoid the problem in the past easily occurring residual silicon or residual carbon due to the skewness of carbon element silicon, 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 technique means of the present invention can be better understood, and can be implemented according to the content of specification sheets, and can become apparent to allow above and other object of the present invention, feature and advantage, 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 carborundum refractory prepared by the embodiment of the present invention 1.
Fig. 2 is the fracture apperance photo of the carborundum refractory prepared by the embodiment of the present invention 1.
Embodiment
For further setting forth the present invention for the technique means reaching predetermined goal of the invention and take and effect, below in conjunction with accompanying drawing and preferred embodiment, be that bonding agent prepares its embodiment of method of carborundum refractory, working method, step, feature and effect thereof with Polycarbosilane to what propose according to the present invention, be described in detail as follows.
The present invention for bonding agent, and forms raw material with the silicon carbide of grain composition with silicon carbide precursor Polycarbosilane, the silicon carbide utilizing Polycarbosilane to be formed by reaction in-situ in sintering process in conjunction with phase, the pure silicon carbide articles of final preparation.The Polycarbosilane added plays the effect of bonding agent in pressing process, makes base substrate have certain intensity, improves its operability.Polycarbosilane can situ converting be silicon carbide in sintering process simultaneously, plays the effect of silicon carbide particle, improves the performance of silicon carbide articles.
In more detail, aforesaid is the method that carborundum refractory prepared by bonding agent with Polycarbosilane, and it comprises the following steps:
(1) with silicon carbide precursor Polycarbosilane for bonding agent, form raw material with the silicon carbide of grain composition, raw material mixed in mixing machine;
(2) use forming machine or ramming process that the material mixed is pressed into base substrate, and base substrate is dried 4 ~ 12h in the baking oven of 80 ~ 110 DEG C;
(3) base substrate after drying is placed in vacuum or inert atmosphere stove sinters in 1300 ~ 1500 DEG C, and heat preservation sintering 1 ~ 5h, the silicon carbide utilizing Polycarbosilane to be formed by reaction in-situ in sintering process in conjunction with phase, the pure silicon carbide articles of final preparation.
Preferably, 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 order, purity >98%; Granularity 2000 order, purity >97%.
More preferably, the mass ratio that the Polycarbosilane bonding agent added 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), the time mixing in mixing machine is 5 ~ 20min.
Embodiment 1
Take Polycarbosilane as bonding agent, and (granularity is respectively 1.43 ~ 2.5mm, 0.5 ~ 1.43mm, 240 orders with the silicon-carbide particle of grain composition, 2000 orders) form raw material, be respectively 3% by mass percentage, 67%, 10%, 15%, the ratio of 5% is weighed.Mix above raw material on planetary Forced Mixing machine 10min, the material mechanical pressing mixed made base substrate, then base substrate is dried 6h in the baking oven of 100 DEG C.Sample after drying is placed in vacuum oven, at 1300 DEG C, 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 caused due to sample slight oxidation in sintering process; Refer to Fig. 2, presoma forms a large amount of fibrous nano whisker in goods inside after sintering; Goods body is close is 2.55gcm -3, folding strength is 30.6MPa.
Embodiment 2
Take Polycarbosilane as bonding agent, and (granularity is respectively 1.43 ~ 2.5mm, 0.5 ~ 1.43mm, 240 orders with the silicon-carbide particle of grain composition, 2000 orders) form raw material, be respectively 7% by mass percentage, 60%, 8%, 16%, the ratio of 9% is weighed.Mix above raw material on planetary Forced Mixing machine 20min, the material ramming process mixed made base substrate, then base substrate is dried 4h in the baking oven of 110 DEG C.Sample after drying is placed in argon gas atmosphere stove, at 1500 DEG C, 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 (granularity is respectively 1.43 ~ 2.5mm, 0.5 ~ 1.43mm, 240 orders with the silicon-carbide particle of grain composition, 2000 orders) form raw material, be respectively 10% by mass percentage, 55%, 5%, 20%, the ratio of 10% is weighed.Mix above raw material on planetary Forced Mixing machine 5min, the material mechanical pressing mixed made base substrate, then base substrate is dried 12h in the baking oven of 80 DEG C.Sample after drying is placed in vacuum oven, at 1400 DEG C, 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 any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be do not depart from technical solution of the present invention content, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.

Claims (1)

1. one kind is the method that carborundum refractory prepared by bonding agent with Polycarbosilane, it is characterized in that: with silicon carbide precursor Polycarbosilane for bonding agent, and form raw material with the silicon carbide of grain composition, the silicon carbide utilizing Polycarbosilane to be formed by reaction in-situ in sintering process is in conjunction with phase, the pure silicon carbide articles of final preparation, the folding strength of described pure silicon carbide articles is 35.4MPa;
Its concrete preparation method is as follows:
(1) mixed in planetary Forced Mixing machine with the sic raw material of grain composition by bonding agent Polycarbosilane, mixing time is 5 ~ 20min, and the mass ratio that Polycarbosilane accounts for raw material is 3 ~ 10%;
(2) use forming machine or ramming process that the material mixed is pressed into base substrate, and base substrate is dried in the baking oven of 80 ~ 110 DEG C;
(3) base substrate after drying is placed in vacuum or inert atmosphere stove sinters, sintering temperature is 1300 ~ 1500 DEG C, and heat preservation sintering 1 ~ 5h;
The silicon carbide specification of above-mentioned grain composition is respectively: granularity 1.43 ~ 2.5mm, purity >99%; Granularity 0.5 ~ 1.43mm, purity >98%; Granularity 240 order, purity >98%; Granularity 2000 order, purity >97%, the mass ratio that its four kinds of specifications from coarse to fine account for raw material is respectively: 55 ~ 67%, 5 ~ 10%, 15 ~ 20%, 5 ~ 10%.
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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
CN104177113B (en) * 2014-08-08 2017-02-22 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
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

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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
CN102417366A (en) * 2011-08-30 2012-04-18 北京理工大学 Pore gradient silicon carbide porous ceramic and preparation method thereof

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