WO2020057095A1 - 一种利用感应炉制备碳化硅粉体的方法 - Google Patents
一种利用感应炉制备碳化硅粉体的方法 Download PDFInfo
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- the invention belongs to the technical field of industrial non-metal resource utilization and ceramic powder material preparation, and particularly relates to a method for preparing silicon carbide powder by using an induction furnace.
- SiC engineering ceramics are highly favored in metallurgy, chemical industry, aerospace and other fields because of their excellent properties such as high temperature resistance, corrosion resistance and wear resistance. Obtaining its excellent performance largely depends on the refinement of the microstructure of the sintered body.
- the microstructure of the sintered body is closely related to the size, morphology and distribution of the raw material particles. How to obtain high-quality powder has become the key to the preparation of high-performance SiC engineering materials.
- the traditional SiC powder preparation methods are all solid-phase methods, and it is the main method for industrial production of SiC, and the output exceeds 90% of the total output.
- the solid-phase method is mainly divided into the Acheson method, the vertical furnace method, the high-temperature converter method, and the carbon-silicon direct reaction method.
- the solid-phase method is widely used in industry, the quality of its powder needs to be improved, its particle size and purity cannot meet the needs of high-tech ceramics, and its preparation cycle is long and its efficiency is low. Therefore, how to quickly prepare high-quality silicon carbide powder is an important research direction.
- Induction furnace is an industrial furnace that uses the principle of electromagnetic induction to heat or melt materials. Due to its characteristics of rapid heating, high temperature, and convenient operation and control, the material is protected from contamination during the heating process, thereby ensuring product quality. Therefore, the use of an induction furnace can quickly prepare pollution-free silicon carbide powder, which not only improves the quality of the silicon carbide powder, but also improves the production efficiency and greatly shortens the production cycle.
- the object of the present invention is to overcome the shortcomings of the prior art mentioned above and provide a method for preparing silicon carbide powder by using an induction furnace.
- the main steps of the method are as follows: first, the silicon-based solid material is pre-treated to prepare clinker; then, the appropriate amount of reducing agent is mixed according to the components of the silicon-based solid material to mix the mixture uniformly; finally, the preparation is made In a graphite crucible device, a certain mass of a mixture is placed in a graphite crucible, and silicon carbide powder is prepared by an induction furnace under the condition of buried carbon.
- the present invention adopts the following technical solutions:
- a method for preparing silicon carbide powder by using an induction furnace is performed according to the following steps:
- Step 1 Raw material pretreatment
- the silicon-based solid material is subjected to high-temperature calcination and sieving to obtain a silicon-based clinker;
- the large-sized graphite crucible is placed in the coil of an induction furnace, and the silicon carbide powder is prepared by an induction furnace by heating; wherein, the heating temperature is 1300 to 1600 ° C and the heating time is 2 to 5 minutes.
- the silicon-based solid material is one or more of crystalline silicon cutting waste, iron ore tailings, coal gangue, fly ash, clay, wax stone, andalusite or sillimanite. .
- step 1 calcining and crushing and sieving are used to remove impurities in industrial silicon-based waste residue.
- the calcining operation is performed in a calcining furnace, the calcining temperature is 900 ° C, and the calcining time is 5 hours.
- the calcining furnace is a box-type resistance wire furnace and silicon carbon used in an unprotected atmosphere.
- the crushing and sieving process is as follows: a jaw crusher is used for crushing, and the powder is passed through a 200-mesh sieve to obtain a silicon-based clinker.
- the reducing agent is a carbonaceous substance, which is one or more of carbon black, high-quality coal, or activated carbon.
- the amount of the reducing agent should be higher than the consumption of reacting the reducing agent containing impurity components such as SiO 2 , Si main component, and metal iron oxide in the silicon-based solid material with the reducing agent.
- the equipment for ball milling the silicon-based clinker and the reducing agent together is a planetary ball mill, and the unidirectional operation is performed at a rotation speed of 200 to 400 r ⁇ min -1 for 5 to 8 hours.
- the height of the small-sized graphite crucible is lower than that of the large-sized graphite crucible.
- the added amount of the mixed material is not higher than 1/3 of the volume of the small graphite crucible.
- the induction coil is a copper coil, ensuring that the large-sized graphite crucible is placed in the copper coil, and the distance between the large-sized graphite crucible and the copper coil is 1 to 2 cm.
- the average particle diameter of the obtained silicon carbide powder is 0.5-1 ⁇ m.
- the induction furnace is one of an intermediate frequency induction furnace, a power frequency induction furnace or a vacuum induction furnace.
- a method for preparing silicon carbide powder using an induction furnace according to the present invention realizes the efficient and comprehensive utilization of silicon-based solid materials, and can rapidly improve the quality of silicon-based solid materials while rapidly preparing high-quality silicon carbide powders. Utilization and added value, especially to solve the environmental pollution caused by silicon-based solid waste.
- the method for preparing silicon carbide powder using an induction furnace according to the present invention is simple and easy to operate, has a fast response, and greatly improves production efficiency.
- a method for preparing silicon carbide powder by using an induction furnace according to the present invention, without impurities in the preparation process, is convenient for preparing high-quality silicon carbide powder.
- FIG. 1 is a process flow chart of a method for preparing silicon carbide powder by using an induction furnace according to Embodiments 1 to 3 of the present invention
- Example 2 is an XRD pattern of the silicon carbide powder prepared in Example 1 of the present invention.
- Example 3 is an XRD pattern of the silicon carbide powder prepared in Example 2 of the present invention.
- FIG. 4 is an XRD pattern of the silicon carbide powder prepared in Example 3 of the present invention.
- the diameter of the small-sized graphite crucible used in the following examples is 40 mm, and the diameter of the large-sized graphite crucible is 70 mm.
- the height of the small-sized graphite crucible is lower than that of the large-sized graphite crucible.
- the added amount of the mixed material is not higher than 1/3 of the volume of the small graphite crucible.
- a method for preparing silicon carbide powder by using an induction furnace The process flow chart is shown in FIG. 1 and is performed according to the following steps:
- Step 1 Raw material pretreatment
- the crystalline silicon cutting waste is placed in a box-type resistance wire furnace, calcined at 900 ° C for 5 hours, and then pulverized by a jaw crusher.
- the powder is passed through a 200-mesh sieve to remove polyethylene glycol and water to obtain silicon-based clinker;
- the large-sized graphite crucible is placed in the copper coil without contacting the copper coil.
- the distance between the large-sized graphite crucible and the copper coil is 1 to 2 cm, so that the induction furnace quickly synthesizes silicon carbide powder within 2 minutes.
- the temperature is about 1300 degrees, and the XRD pattern of the obtained silicon carbide powder is shown in FIG. 2.
- the main phases of the obtained silicon carbide powder were 6H-SiC, C (graphite), a small amount of SiO 2 , and the average particle diameter of the synthetic powder was 0.5 ⁇ m.
- a method for preparing silicon carbide powder by using an induction furnace The process flow chart is shown in FIG. 1 and is performed according to the following steps:
- Step 1 Raw material pretreatment
- the crystalline silicon cutting waste is placed in a box-type resistance wire furnace, calcined at 900 ° C for 5 hours, and then pulverized by a jaw crusher.
- the powder is passed through a 200-mesh sieve to remove polyethylene glycol and water to obtain a silicon-based clinker;
- the silicon-based clinker and activated carbon are configured, and the two materials are fully mixed in a planetary ball mill with a ball milling rate of 400 r ⁇ min -1 and a one-way operation for 5 hours to obtain a mixed material;
- the large-sized graphite crucible is placed in the copper coil without contacting the copper coil.
- the distance between the large-sized graphite crucible and the copper coil is 1 to 2 cm, so that the induction furnace quickly synthesizes silicon carbide powder within 2 minutes.
- the induction furnace The temperature is about 1300 degrees, and the XRD pattern of the obtained silicon carbide powder is shown in FIG. 3.
- the phase of the obtained silicon carbide powder was 6H-SiC, C (graphite), no SiO 2 , and the average particle diameter of the synthetic powder was 0.5 ⁇ m.
- a method for preparing silicon carbide powder by using an induction furnace The process flow chart is shown in FIG. 1 and is performed according to the following steps:
- Step 1 Raw material pretreatment
- the crystalline silicon cutting waste is placed in a box-type resistance wire furnace, calcined at 900 ° C for 5 hours, and then pulverized by a jaw crusher.
- the powder is passed through a 200-mesh sieve to remove polyethylene glycol and water to obtain silicon-based clinker;
- the silicon-based clinker and activated carbon are configured, and the two materials are mixed in a planetary ball mill, and the ball milling rate is 400 r ⁇ min -1 , and the unidirectional operation is performed for 5 hours to obtain a mixed material;
- the large-sized graphite crucible is placed in the copper coil without contacting the copper coil.
- the distance between the large-sized graphite crucible and the copper coil is 1 to 2 cm, so that the induction furnace quickly synthesizes silicon carbide powder within 5 minutes. At this time, the induction furnace The temperature is about 1600 degrees.
- the XRD pattern of silicon carbide powder is shown in Figure 4.
- the phase of the obtained silicon carbide powder was ⁇ -SiC, and the average particle diameter of the synthetic powder was 1 ⁇ m.
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Abstract
一种利用感应炉制备碳化硅粉体的方法,包括步骤如下:步骤1,将硅基固料进行高温煅烧与粉碎过筛处理,制得硅基熟料;步骤2,按配比,硅基熟料∶还原剂=100:(10~45),将二者混合,球磨得混匀物料;步骤3,(1)将小尺寸石墨坩埚置于大尺寸石墨坩埚内,并在两个坩埚接触处放满天然石墨粉;(2)将混匀物料置于小尺寸石墨坩埚中,并在小石墨坩埚锅盖上端覆盖充足的天然石墨粉;(3)将大尺寸石墨坩埚置于感应炉线圈内,在1300~1600℃温度下,加热2~5min制得利用感应炉制备碳化硅粉体。
Description
本发明属于工业非金属资源化利用及陶瓷粉体材料制备技术领域,具体涉及一种利用感应炉制备碳化硅粉体的方法。
SiC工程陶瓷因其具有耐高温、抗腐蚀、耐磨损等优异性能,在冶金、化工、航空航天等领域备受青睐。其优良性能的获得很大程度上依赖于烧结体显微结构的精细化。而烧结体的显微结构与原料颗粒的大小、形貌及分布状况等密切相关。如何获得高质量的粉体成为制备高性能SiC工程材料的关键。
目前,传统的SiC粉体制备方法都是固相法,并且其为工业生产SiC的主要方法,产量超过总产量的90%。固相法主要分为阿奇逊(Acheson)法、竖式炉法、高温转炉法、碳硅直接反应法等。固相法虽然在工业上广泛应用,但其粉体的质量有待提高,粒度与纯度不能满足高技术陶瓷的需求,且其制备周期长,效率较低。因此,如何快速制备出高质量的碳化硅粉体是一个重要的研究方向。
感应炉是一种利用电磁感应的原理加热或熔化物料的工业炉,因其具有加热迅速、温度高、操作控制方便等特点,使得物料在加热过程中免受污染,从而保证产品的质量。因此,利用感应炉可以快速制备出无污染的碳化硅粉体,既改善了碳化硅粉体的质量,又提高了生产效率,大大缩短了生产周期。
发明内容:
本发明的目的是克服上述现有技术存在的不足,提供一种利用感应炉制备碳化硅粉体的方法。该方法的主要工序如下:首先,将硅基固料进行预处理,以制得熟料;然后,根据硅基固料的组分掺入适量的还原剂,将混合料混合均匀;最后,制作石墨坩埚装置,将一定质量的混合料置于石墨坩埚内,于埋碳条件下经感应炉制得碳化硅粉体。
为实现上述目的,本发明采用以下技术方案:
一种利用感应炉制备碳化硅粉体的方法,按以下步骤进行:
步骤1:原料预处理
将硅基固料进行高温煅烧与粉碎过筛处理,制得硅基熟料;
步骤2:混料
按配比,硅基熟料∶还原剂=100∶(10~45),将二者混合,球磨得混匀物料;
步骤3:高温合成
(1)将小尺寸石墨坩埚置于大尺寸石墨坩埚内,并在两个坩埚接触处放满天然石墨粉;
(2)将混匀物料置于小尺寸石墨坩埚中,并在小石墨坩埚锅盖上端覆盖充足的天然石墨粉。
(3)将大尺寸石墨坩埚置于感应炉线圈内,加热制得利用感应炉制备碳化硅粉体;其中,所述的加热温度1300~1600℃,加热时间2~5min。
所述的步骤1中,所述的硅基固料为晶体硅切割废料、铁矿石尾矿、煤矸石、粉煤灰、粘土、蜡石、红柱石或硅线石中的一种或多种。
所述的步骤1中,煅烧与粉碎过筛处理用于去除工业硅基废渣中的杂质。
所述的步骤1中,所述的煅烧操作在煅烧炉中进行,煅烧温度为900℃,煅烧时间为5h,所述的煅烧炉为在无保护气氛下使用的箱式电阻丝炉、硅碳棒炉、硅钼棒炉和隧道窑中的一种。
所述的步骤1中,所述的粉碎过筛处理过程为:采用颚式破碎机粉碎处理,粉末经200目筛后,制得硅基熟料。
所述的步骤2中,所述的还原剂为含碳物质,为炭黑、优质煤或活性炭中的一种或多种。
所述的步骤2中,所述的还原剂用量应高于硅基固料中含SiO
2、Si主成分及金属铁氧化物等杂质成分与还原剂反应的消耗量。
所述的步骤2中,所述的硅基熟料和还原剂一起球磨采用的设备为行星式球磨机,以200~400r·min
-1转速单向运行5~8h。
所述的步骤3(1)中,所述的小尺寸石墨坩埚的高度低于大尺寸石墨坩埚。
所述的步骤3(2)中,所述的混匀物料添加量以不高于小石墨坩埚容积的1/3为准。
所述的步骤3(3)中,所述的感应线圈为铜线圈,保证大尺寸石墨坩埚置于铜线圈内,且使大尺寸石墨坩埚与铜线圈距离1~2cm。
所述的步骤3(3)中,制得的碳化硅粉体平均粒径为0.5~1μm。
所述的步骤3(3)中,所述的感应炉为中频感应炉、工频感应炉或真空感应炉中的一种。
本发明的有益效果:
1.本发明的一种利用感应炉制备碳化硅粉体的方法实现了硅基固料的高效综合利用,在快速制备出高质量碳化硅粉体的同时,还可大幅度提高硅基固料的利用率和附加值,尤其解决硅基固体废弃物给环境带来的污染问题。
2.本发明的一种利用感应炉制备碳化硅粉体的方法操作简单易行,反应迅速,大大提高了生产效率。
3.本发明的一种利用感应炉制备碳化硅粉体的方法,制备过程无杂质掺入,便于制备出高质量的碳化硅粉体。
图1是本发明实施例1~3利用感应炉制备碳化硅粉体的方法的工艺流程图;
图2是本发明实施例1制备的碳化硅粉体XRD图;
图3是本发明实施例2制备的碳化硅粉体XRD图;
图4是本发明实施例3制备的碳化硅粉体XRD图。
下面结合实施例对本发明作进一步的详细说明。
以下实施例中采用的小尺寸石墨坩埚直径为40mm,大尺寸石墨坩埚直径为70mm。
小尺寸石墨坩埚的高度低于大尺寸石墨坩埚。
所述的步骤3(2)中,所述的混匀物料添加量以不高于小石墨坩埚容积的1/3为准
如图1所示,一种利用感应炉制备碳化硅粉体的方法的。
实施例1
一种利用感应炉制备碳化硅粉体的方法,其工艺流程图如图1所示,按以下步骤进行:
步骤1:原料预处理
将晶体硅切割废料置于箱式电阻丝炉中,900℃下煅烧5h,再经颚式破碎机粉碎处理,粉末经200目筛,去除聚乙二醇和水,制得硅基熟料;
步骤2:混料
以100∶10的质量配比,配置硅基熟料和活性炭,将两物质置于行星式球磨机中充分混合,球磨速率为400r·min
-1,单向运行5h,得混匀物料;
步骤3:高温合成
(1)将一个小尺寸石墨坩埚置于大尺寸石墨坩埚内,并在两个坩埚接触处放满天然石墨粉;
(2)将7g混匀的粉料置于小尺寸石墨坩埚中,并在石墨坩埚锅盖上端覆盖充足的天然石墨粉。
(3)将大尺寸石墨坩埚置于铜线圈内且不接触铜线圈,大尺寸石墨坩埚与铜线圈距离1~2cm,使之感应炉在2分钟内迅速合成碳化硅粉体,此时感应炉温度约为1300度,制得碳化硅粉体XRD图如图2所示。
经检测,所得碳化硅粉体的主要物相为6H-SiC,C(石墨),少量的SiO
2,且合成粉体的平均粒径为0.5μm。
实施例2
一种利用感应炉制备碳化硅粉体的方法,其工艺流程图如图1所示,按以下步骤进行:
步骤1:原料预处理
将晶体硅切割废料置于箱式电阻丝炉中,900℃下煅烧5h,再经颚式破碎机粉碎处理,粉末经200目筛,去除聚乙二醇和水,制得硅基熟料;
步骤2:混料
以100∶25的质量配比,配置硅基熟料和活性炭,将两物质置于行星式球磨机中充分混合,球磨速率为400r·min
-1,单向运行5h,得混匀物料;
步骤3:高温合成
(1)将一个小尺寸石墨坩埚置于大尺寸石墨坩埚内,并在两个坩埚接触处放满天然石墨粉;
(2)将7g混匀的粉料置于小尺寸石墨坩埚中,并在石墨坩埚锅盖上端覆盖充足的天然石墨粉。
(3)将大尺寸石墨坩埚置于铜线圈内且不接触铜线圈,大尺寸石墨坩埚与铜线圈距离1~2cm,使之感应炉在2分钟内迅速合成碳化硅粉体,此时感应炉温度约为1300度,制得碳化硅粉体XRD图如图3所示。
经检测,所得碳化硅粉体的物相为6H-SiC,C(石墨),无SiO
2,且合成粉体的平均粒径为0.5μm。
实施例3
一种利用感应炉制备碳化硅粉体的方法,其工艺流程图如图1所示,按以下步骤进行:
步骤1:原料预处理
将晶体硅切割废料置于箱式电阻丝炉中,900℃下煅烧5h,再经颚式破碎机粉碎处理,粉末经200目筛,去除聚乙二醇和水,制得硅基熟料;
步骤2:混料
以100∶45的质量配比,配置硅基熟料和活性炭,将两物质置于行星式球磨机中充分混合,球磨速率为400r·min
-1,单向运行5h,得混匀物料;
步骤3:高温合成
(1)将一个小尺寸石墨坩埚置于大尺寸石墨坩埚内,并在两个坩埚接触处放满天然石墨粉;
(2)将7g混匀的粉料置于小尺寸石墨坩埚中,并在石墨坩埚锅盖上端覆盖充足的天然石墨粉。
(3)将大尺寸石墨坩埚置于铜线圈内且不接触铜线圈,大尺寸石墨坩埚与铜线圈距离1~2cm,使之感应炉在5分钟内迅速合成碳化硅粉体,此时感应炉温度约为1600度,碳化硅粉体XRD图如图4所示。
经检测,所得碳化硅粉体的物相为β-SiC,且合成粉体的平均粒径为1μm。
Claims (10)
- 一种利用感应炉制备碳化硅粉体的方法,其特征在于,按以下步骤进行:步骤1:原料预处理将硅基固料进行高温煅烧与粉碎过筛处理,制得硅基熟料;步骤2:混料按配比,硅基熟料∶还原剂=100:(10~45),将二者混合,球磨得混匀物料;步骤3:高温合成(1)将小尺寸石墨坩埚置于大尺寸石墨坩埚内,并在两个坩埚接触处放满天然石墨粉;(2)将混匀物料置于小尺寸石墨坩埚中,并在小石墨坩埚锅盖上端覆盖充足的天然石墨粉;(3)将大尺寸石墨坩埚置于感应炉线圈内,加热制得利用感应炉制备碳化硅粉体;其中,所述的加热温度1300~1600℃,加热时间2~5min。
- 根据权利要求1所述的利用感应炉制备碳化硅粉体的方法,其特征在于,所述的步骤1中,所述的硅基固料为晶体硅切割废料、铁矿石尾矿、煤矸石、粉煤灰、粘土、蜡石、红柱石或硅线石中的一种或多种。
- 根据权利要求1所述的利用感应炉制备碳化硅粉体的方法,其特征在于,所述的步骤1中,煅烧与粉碎过筛处理用于去除工业硅基废渣中的杂质。
- 根据权利要求1所述的利用感应炉制备碳化硅粉体的方法,其特征在于,所述的步骤1中,所述的煅烧操作在煅烧炉中进行,煅烧温度为900℃,煅烧时间为5h,所述的煅烧炉为在无保护气氛下使用的箱式电阻丝炉、硅碳棒炉、硅钼棒炉和隧道窑中的一种。
- 根据权利要求1所述的利用感应炉制备碳化硅粉体的方法,其特征在于,所述的步骤1中,所述的粉碎过筛处理过程为:采用颚式破碎机粉碎处理,粉末经200目筛后,制得硅基熟料。
- 根据权利要求1所述的利用感应炉制备碳化硅粉体的方法,其特征在于,所述的步骤2中,所述的还原剂为炭黑、优质煤或活性炭中的一种或多种。
- 根据权利要求1所述的利用感应炉制备碳化硅粉体的方法,其特征在于,所述的步骤2中,所述的硅基熟料和还原剂一起球磨采用的设备为行星式球磨机,以200~400r·min -1转速单向运行5~8h。
- 根据权利要求1所述的利用感应炉制备碳化硅粉体的方法,其特征在于,所述的步骤3(2)中,所述的混匀物料添加量以不高于小石墨坩埚容积的1/3为准。
- 根据权利要求1所述的利用感应炉制备碳化硅粉体的方法,其特征在于,所述的步骤3(3)中,所述的感应线圈为铜线圈,保证大尺寸石墨坩埚置于铜线圈内,且使大尺寸石墨坩 埚与铜线圈距离1~2cm。
- 根据权利要求1所述的利用感应炉制备碳化硅粉体的方法,其特征在于,所述的步骤3(3)中,制得的碳化硅粉体平均粒径为0.5~1μm。
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