CN101027251A - 金属碳化物及其制备方法 - Google Patents
金属碳化物及其制备方法 Download PDFInfo
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- CN101027251A CN101027251A CNA2005800302710A CN200580030271A CN101027251A CN 101027251 A CN101027251 A CN 101027251A CN A2005800302710 A CNA2005800302710 A CN A2005800302710A CN 200580030271 A CN200580030271 A CN 200580030271A CN 101027251 A CN101027251 A CN 101027251A
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- metallic carbide
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- 238000000034 method Methods 0.000 title claims abstract description 49
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- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 6
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
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- 229910052748 manganese Inorganic materials 0.000 claims abstract description 5
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
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- 239000002121 nanofiber Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- 238000010189 synthetic method Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
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Abstract
金属碳化物合成物和通过一步法合成金属碳化物的方法,其中将不同金属的氧化物与球形或纤维状纳米结构的碳物理混合,并感应加热至一定的温度范围(900℃-1900℃),所述的不同金属包括但不限于Si、Ti、W、Hf、Zr、V、Cr、Ta、B、Nb、Al、Mn、Ni、Fe、Co和Mo,其中所述金属氧化物与碳反应形成不同的金属碳化物。该方法在所得到的金属碳化物中保持了所述起始碳前体的初始形态。该方法还产生了高结晶的金属纳米碳化物。所述金属碳化物产物应用于高温热电装置、量子阱、光电装置、半导体、人体装甲、车辆装甲、催化剂,并作为诸如铝的金属和其它合金中的不连续补强剂。
Description
发明人
PRADHAN,Bhabendra,360 Bloombridge Way N.W.,Marietta,Georgia 30066 US,印度公民;
TANDON,Deepak,1708 English Ivey Lane,Kennesaw,Georgia,30144 US,印度公民;
TAYLOR,Rodney,L.,美国公民6304 Benbrooke Overlook,Acworth,Georgia,30101 US;和
HOFFMAN,Paul,B.,美国公民205 Greenhill Drive,Dallas,Georgia,30132 US。
相关申请的交叉引用
在此要求2004年9月9日提交的序号为10/937,043的美国专利申请的优先权。
在此将2004年9月9日提交的序号为10/937,043的美国专利申请引入作为参考。
关于联邦政府资助的研究或开发的声明
无
参考“缩微胶片附录”
无
发明背景
1.发明领域
本发明涉及金属碳化物的产生。更具体地,本发明涉及通过一步法由多种碳材料产生金属碳化物,其中将金属氧化物与碳源混合并采用新的感应加热法将该金属氧化物转化为所述的金属碳化物。
2.发明背景
在现有技术中,通常以多步法产生金属碳化物,其中,首先将来自含碳气体的碳热解沉积在金属氧化物上。随后通过电阻加热至1200℃或更高的温度,在惰性气氛中将所得复合材料还原数小时,得到所述金属碳化物。
一现有技术参考文献教导了一步法(J.Mat.Sci 33(1998)1049-1055)。然而,该参考文献还在更长的反应时间内使用了电阻加热。在这些现有技术的操作中,与起始材料的粒度的相比,所得到的金属碳化物的粒度增加了,并且在所得产物中,EDS显示的残余氧的存在表明转化是不完全的。
本申请中,以下术语定义如下:
1.“形态”用于描述在金属碳化物产物中含碳反应物的大小和形状。
2.本文使用“TEM”-(透射电子显微镜)来提供形态的描述。
3.本文使用“XRD”-(X射线衍射)来定义晶体结构和晶相。
4.本文使用STEMEDS、EDS-(电子衍射光谱)来进行微量元素分析。
在申请人的实验方法中,申请人预期,结果是金属碳化物包裹碳核。所得到的意想不到的结果是全部金属碳化物产物合成物保持碳前体的形态,该结果将得到进一步的解释。
发明概述
在本发明中,提供了通过一步法合成金属碳化物的方法,其中将不同金属的氧化物与不同的纳米结构的碳前体物理混合,并感应加热至900-1900℃,其中所述金属氧化物与所述碳反应以形成不同的金属碳化物,所述不同金属包括但不限于Si、Ti、W、Hf、Zr、V、Cr、Ta、B、Nb、Al、Mn、Ni、Fe、Co和Mo,并且不同的纳米结构的碳前体可以是球形的(20nm)或纤维状的(60nm)。该方法在所得的金属碳化物中保持了起始碳前体的初始形态。产生的金属纳米碳化物还是高结晶的。这些颗粒中大多数是单晶金属碳化物。该方法的转化率为超过80%转化为金属碳化物,残余物包含未转化的过量碳。
在另一申请中,纳米结构的SiC(和其它碳化物)可以用作铝和其它合金中的补强剂。在此情况中,该纳米结构的SiC是将应力集中最小化的纳米大小的球形碳化物。还提供了与中或高结构的碳黑聚集体具有相同形状的分支碳化物聚集体,该分支碳化物聚集体增加了裂纹路径迂曲度并可以捕获裂纹。
因此,本发明的主要目的是产生高结晶的纤维状纳米金属碳化物;
本发明的另一目的是产生纳米金属碳化物,在所得到的金属碳化物中保持所述碳前体的形态;
本发明的另一目的是提供通过使用感应加热法产生金属碳化物的方法;
本发明的另一目的是产生金属碳化物,使用EDS通过不存在O以及使用XRD通过不存在任意其它相证实了MOx完全转化为金属碳化物;
本发明的另一目的是提供产生金属碳化物的半连续或连续方法;
本发明的另一目的是提供金属碳化物产物,可以在现有技术的金属碳化物所应用的领域中使用该金属碳化物。
本发明的另一目的是提供能够替代氢化催化剂中的贵金属的金属碳化物;
本发明的另一目的是提供具有特定纳米级应用的纳米纤维碳化物,在所述应用中,粒度的要求排除了使用现有技术的金属碳化物;以及
本发明的另一目的是提供了金属碳化物产物,该金属碳化物具有不限于如下方面的应用:高温热电装置、量子阱、光电装置、半导体、人体装甲、车辆装甲、催化剂、不连续补强剂、结构补强、改善耐磨性、提供耐腐蚀性、增强高温稳定性、提供抗辐射性以及提供提高的导热性。
本发明的另一目的是提供了金属碳化物产物,其中不连续补强剂存在于铝和其它合金中以减少应力集中且分支纳米大小的碳聚集体增加了裂纹路径迂曲度并可以捕获裂纹。
附图的简要说明
为了进一步理解本发明的性质、目的和优点,应该参考详细说明并结合以下附图,其中相同的附图标记表示相同的元件,并且其中:
图1描述本发明中参与金属碳化物产生的通常的化学反应和反应条件;
图2是本发明的金属碳化物产生装置的示意图;
图3是本发明中实施用于产生和收集金属碳化物的半连续方法的金属碳化物产生装置的示意图;
图4是TEM,其显示了本发明的方法中所使用的前体碳黑的形态;
图5是本发明中由碳黑合成的B4C的TEM;
图6是TEM,其显示了本发明的方法中所使用的前体碳纳米纤维的形态;
图7是由本发明的方法所产生的碳化钼的TEM;
图8是本发明的方法所产生的在SiC纤维表面上的SiC晶体的TEM;
图9是本发明的方法所产生的TiC的TEM;
图10包含本发明的方法中来源于碳黑的金属碳化物的XRD谱;
图11包含本发明的方法中来源于碳纳米纤维的金属碳化物的XRD谱;
表1提供了在图10和11的XRD谱中的主相和次相的鉴定。
优选实施方案的详细说明
在通过一步法由碳材料产生金属碳化物中,参考图1-11和表1。如前所述,总的来说本发明涉及产生诸如碳化硅、碳化钛和碳化钼以及其它金属碳化物的合成方法。该方法包括单一步骤,其中将不同金属的氧化物与不同的纳米结构的碳前体物理混合,该不同金属例如Si、Ti、W、Hf、Zr、V、Cr、Ta、B、Nb、Al、Mn、Ni、Fe、Co和Mo,所述不同的纳米结构的碳前体可以是球形的(20nm)或纤维状的(60nm)。该球形碳颗粒的直径为8-200nm,而该纤维状碳的直径为1-200nm。将该混合物感应加热至900-1900℃以便该金属氧化物与该碳反应来形成不同的金属碳化物。在使用此方法时,在所得的金属碳化物中保持了该碳前体的初始形态。产生的该碳化物是高结晶的。此方法的转化率为超过80%转化为金属碳化物,残余物包含未转化的过量碳。
以下是实施例1中将二氧化硅与所述纳米碳前体化合的实验实施例;实施例2中将二氧化钛与所述纳米碳前体化合的实验实施例;实施例3中将氧化钼与所述纳米碳前体化合的实验实施例;以及实施例4中将氧化硼与所述纳米碳前体化合的实验实施例。
实验实施例:
实施例1
SiO2+3C—→SiC+2CO
通过使用10g二氧化硅和作为前体的6g纳米碳来合成碳化硅粉末。该SiO2粉末的平均粒度为约40μm及比表面积为5m2/g,该碳源是碳黑(CDX975,253m2/g,平均粒度为21nm)或者是纤维状纳米碳(68.5m2/g,平均直径为70nm)。首先,使用刮勺或球磨机将碳源和二氧化硅物理混合,直到充分混合为止。然后将该混合物置于石墨坩锅中并放在位于感应线圈内的石英容器中。用1SLM流速的Ar气吹扫该容器。吹扫30分钟后,将该石墨坩锅的温度30分钟内升至1400℃,并在所要温度下保持少于15分钟。然后在Ar流中将该石墨坩锅冷却。所得样品的XRD图样显示,所形成的粉末颗粒是单相六方碳化硅颗粒。透射电子显微镜显示来源于CB的产物的粒度为20-100nm,而该纤维状纳米碳完全转化为形态与该碳前体的形态相匹配的碳化硅。在此产生的碳化硅的热分析(Thermogrametric analysis)(以除去剩余的碳)显示转化率为约95%。STEMEDS证实了该碳化硅颗粒是非常高纯的。
实施例2:
TiO2+3C—→TiC+2CO
通过使用13.33g二氧化钛和作为前体的6g纳米碳来作为前体合成碳化钛粉末。该TiO2粉末的平均粒度为约32μm及比表面积为45m2/g,该碳源或者是碳黑(CDX975,253m2/g,平均粒度为21nm)或者是纤维状纳米碳(68.5m2/g,平均直径为70nm)。开始首先,使用刮勺或球磨机将碳源和二氧化钛物理混合,直到充分混合为止。然后将该混合物置于石墨坩锅中并放在位于感应线圈内的石英器皿容器中内。用1SLM流速的Ar气吹扫该器皿容器。吹扫30分钟后,将该石墨坩锅的温度30分钟内升至1400℃,并在<15分钟内保持在所要的温度下保持少于15分钟。然后在Ar流中将该石墨坩锅冷却。所得样品的XRD图样显示所形成的粉末颗粒是单相立方形单相碳化钛颗粒。透射电子显微镜显示来源于CB的产物的粒度为20-100nm,而该纤维状纳米碳完全转化为形态与该碳前体的形态相匹配的碳化钛。STEMEDS证实了该碳化钛颗粒均是非常高纯的。
实施例3
Mo2O3+4C—→Mo2C+3CO
通过使用24g二氧化钼和作为前体的6g纳米碳来合成碳化钼粉末。该Mo2O3粉末的平均粒度为约20-40nm及比表面积为48m2/g,该碳源是碳黑(CDX975,253m2/g,平均粒度为21nm)或者是纤维状纳米碳(68.5m2/g,平均直径为70nm)。首先,使用刮勺或球磨机将碳源和钼氧化物物理混合,直到充分混合为止。然后将该混合物置于石墨坩锅中并放在位于感应线圈内的石英容器中。用1SLM流速的Ar气吹扫该容器。吹扫30分钟后,将该石墨坩锅的温度30分钟内升至1350℃,并在所要的温度下保持少于15分钟。然后在Ar流中将该石墨坩锅冷却。所得样品的XRD图样显示所形成的粉末颗粒是单相六方碳化钼颗粒。透射电子显微镜显示来源于CB的产物的粒度为20-100nm,而该纤维状纳米碳完全转化为形态与该碳前体的形态相匹配的碳化钼。STEMEDS证实了该碳化钼颗粒是非常高纯的。
实施例4:
B2O3+7C—→B4C+6CO
通过使用14g氧化硼和作为前体的8.4g纳米碳来合成碳化硼粉末。该B2O3粉末的平均粒度为约40nm及比表面积为5m2/g,该碳源是碳黑(CDX975,253m2/g,平均粒度为21nm)或者是纤维状纳米碳(68.5m2/g,平均直径为70nm)。首先,使用刮勺或球磨机将碳源和氧化硼物理混合,直到充分混合为止。然后将该混合物置于石墨坩锅中并放在位于感应线圈内的石英容器中。用1SLM流速的Ar气吹扫该容器。吹扫30分钟后,将该石墨坩锅的温度30分钟内升至1300℃,并在所要的温度下保持少于15分钟。然后在Ar流中将该石墨坩锅冷却。所得样品的XRD图样显示所形成的粉末颗粒是单相六方碳化硼颗粒。透射电子显微镜显示来源于CB的产物的粒度为20-100nm,而该纤维状纳米碳完全转化为形态与该碳前体的形态相匹配的碳化硼。
现在参看图1至11和表1:图1,描述了与本发明相关的化学反应和反应条件:
xC+MyO(x-1)→MYC+(x-1)CO,其中M选自包括但不限于Si、B、Ta、Zr、Cr、V、W、Hf、Ti和Mo。所述反应要求将金属氧化物和纳米碳的均匀混合物在惰性气体流中,在900℃-1900℃下感应加热,并在此温度下保持加热1-30分钟。
图1中所述的产生所述金属碳化物的间歇式和半连续方法分别在图2和图3中进行了示意性描述。在图2中描述的装置应用于实施例1至实施例4中。
图2提供了以间歇式实施所述金属碳化物的实验方法的示意图。在图2中,描述了进入被感应线圈18环绕的石英反应器14中的氩气(箭头12),该石英反应器的类型通常是工业中公知的,并其含有石墨坩锅16。金属氧化物和碳的混合物20置于石墨坩锅16内。然后通过感应线圈18将该混合物加热至900℃-1900℃。将该氩气排出(箭头22),所得金属碳化物保留在坩锅16内以便收集。
图3提供了半连续或连续产生金属碳化物的示意图。如其所述,可通过使用石英反应器14半连续地合成金属碳化物粉末。石英反应器14包括含有所述金属氧化物和碳的混合物20的石墨坩锅16。还包括环绕所述石英反应器的感应线圈18,以便如图2所述加热该混合物。然而,在图3中所述的半连续方法中,提供了含有预混合的金属氧化物和碳前体31的进料器30。将氩气(箭头12)引入进料器30中的金属氧化物和碳源的混合物31中,并将该混合物由空气输送至石墨坩锅16中,在那里通过该感应线圈18将该混合物加热至900℃-1900℃之间的所要温度,并在此温度下保持1-30分钟。提供了收集器34,可将所得金属碳化物通过真空线35从坩锅16中输送至该收集器中以便收集。用1SLM流速的氩气12吹扫该石英反应器。该方法可重复进行以实现金属碳化物的半连续产生,而无需打开该反应系统。
图4至图9是透射电子显微照片,其描述前述实施例1-4中使用的代表性的碳反应物(4、6)及产生的有代表性的碳化物产物(5、7-9)的形态。
图4是描述了在所述实验中用作前体的纳米碳黑的形态的TEM。该碳黑是CDX-975(Columbian Chemicals Co.),平均粒度为21nm。
图5是描述了实施例4中所述的由图4所示的碳黑产生的碳化硼(B4C)的TEM。
图6是描述了实施例1-4中所用的碳纳米纤维前体的TEM。该材料的氮吸附法表面积为68m2/g且平均纤维直径为70nm。
图7是实施例3中所述的由图6所示的碳纳米纤维产生的碳化钼纤维的TEM。注意到了存在附着在该纤维表面的Mo2C结晶。
图8描述了实施例1中所述的由图6所示的碳纳米纤维产生的SiC纤维的TEM。STEM/EDAX分析显示在该产品中不存在残留的氧,这表明完全转化为该碳化物。
图9是描述了实施例2中所述的由图6所示的碳纳米纤维产生的TiC纤维的TEM。STEM/EDAX分析显示在该产品中不存在残留的氧,这表明完全转化为该碳化物。
现在参看题为“XRD图谱的主要相和次要相的鉴定”的表1,还对来自实施例1-4中的样品进行了XRD分析。三种样品(A-31077、A-31078和A-31079)是来源于碳黑(CDX975,A027276)的不同金属碳化物,而样品A-31080、A-31081和A-31082是来源于碳纳米纤维(样品A-30887)的相似的金属碳化物。图10中显示了来自源于CB的金属碳化物的XRD谱,而图11中显示了来自源于纤维的金属碳化物的谱。峰的匹配显示由该两种起始材料产生的碳化物的相中不存在差异。表1中列出了在XRD谱中主组分峰和次组分峰。这些结果证明该起始材料基本上完全转化为其各自的碳化物。
仅通过实例方式提供了前述实施方案,本发明的范围只受到所附权利要求的限制。
Claims (32)
1.由金属氧化物与纳米碳前体的反应产生的金属碳化物合成物。
2.如权利要求1所述的合成物,其中所述金属氧化物选自Si、Ti、W、Hf、Zr、Cr、Ta、B、V、Nb、Al、Mn、Ni、Fe、Co和Mo的金属氧化物。
3.如权利要求1所述的合成物,其中所述纳米碳包括球形或纤维状纳米结构的碳。
4.如权利要求3所述的合成物,其中所述球形碳的颗粒直径为8-200nm。
5.如权利要求3所述的合成物,其中所述纤维状碳的直径为1-200nm。
6.如权利要求1所述的合成物,其中将所述金属氧化物和纳米碳前体感应加热到900℃至1900℃。
7.如权利要求6所述的合成物,其中在感应电炉中实现所述金属氧化物和纳米碳前体的加热。
8.金属碳化物合成物,其通过在900℃至1900℃的温度下,在感应电炉中由金属氧化物与纤维状或球形纳米碳前体的反应产生。
9.如权利要求8所述的合成物,其中所得到的金属碳化物为高结晶的纤维状纳米金属碳化物。
10.如权利要求8所述的合成物,其中所得到的向金属碳化物的转化基本上是完全的。
11.如权利要求8所述的合成物,其中所述纳米金属碳化物基本保持所述碳前体的大小和形态。
12.如权利要求8所述的合成物,其中所述金属氧化物选自Si、Ti、W、Hf、Zr、Cr、Ta、B、V、Nb、Al、Mn、Ni、Fe、Co和Mo的金属氧化物。
13.产生金属碳化物的方法,其包括如下步骤:将金属氧化物与碳前体混合,在感应电炉中加热所述混合物以便使所得到的金属氧化物从MOx完全转化,而没有任何残余的氧。
14.如权利要求13所述的方法,其中将所述的金属氧化物和纳米碳前体感应加热到900℃至1900℃。
15.如权利要求13所述的方法,其中所述方法是连续法。
16.产生金属碳化物的方法,包括如下步骤:
(a)提供金属氧化物;
(b)将所述金属氧化物与纳米碳前体混合;
(c)将所述混合物在感应电炉中加热到900℃至1900℃;
(d)在加热过程中向所述混合物引入惰性气体;
(e)在加热周期结束时收集所得到的金属碳化物;
(f)作为连续法,重复步骤“a”至“e”。
17.产生金属碳化物的方法,包括如下步骤:
(a)提供金属氧化物;
(b)将所述金属氧化物与纳米碳前体混合;
(c)将所述混合物在感应电炉中加热到900℃至1900℃并维持少于30分钟;
(d)在加热过程中向所述混合物引入惰性气体;
(e)在加热周期结束时收集所得到的金属碳化物;
(f)作为连续法,重复步骤“a”至“e”。
18.如权利要求17所述的方法,其中将所得到的金属碳化物应用于高温热电装置。
19.如权利要求17所述的方法,其中将所得到的金属碳化物应用于量子阱。
20.如权利要求17所述的方法,其中将所得到的金属碳化物应用于光电装置。
21.如权利要求17所述的方法,其中将所得到的金属碳化物应用于半导体。
22.如权利要求17所述的方法,其中将所得到的金属碳化物应用于装甲。
23.如权利要求17所述的方法,其中将所得到的金属碳化物应用于催化剂。
24.如权利要求23所述的方法,其中所述在催化剂中的应用包括氢化、脱氢、重整、脱氮和脱硫。
25.如权利要求17所述的方法,其中将所得到的金属碳化物应用于不连续补强剂。
26.如权利要求17所述的方法,其中将所得到的金属碳化物应用于结构补强。
27.如权利要求17所述的方法,其中将所得到的金属碳化物应用于改善耐磨性。
28.如权利要求17所述的方法,其中将所得到的金属碳化物应用于提供耐腐蚀性。
29.如权利要求17所述的方法,其中将所得到的金属碳化物应用于提高高温稳定性。
30.如权利要求17所述的方法,其中将所得到的金属碳化物应用于提供抗辐射性。
31.如权利要求17所述的方法,其中将所得到的金属碳化物应用于提供增强的导热性。
32.基本上如所述及公开的发明。
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CN (1) | CN101027251A (zh) |
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WO2020057095A1 (zh) * | 2018-09-20 | 2020-03-26 | 东北大学 | 一种利用感应炉制备碳化硅粉体的方法 |
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EP2125663A4 (en) * | 2007-02-22 | 2012-05-23 | Boron Compounds Ltd | PROCESS FOR PRODUCING CERAMIC MATERIALS |
US20100069223A1 (en) * | 2007-03-07 | 2010-03-18 | Emanual Prilutsky | Method for the preparation of ceramic materials |
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CN103553043A (zh) * | 2013-09-30 | 2014-02-05 | 陕西科技大学 | 一种制备高比表面积SiC纳米微球的方法 |
CN103553043B (zh) * | 2013-09-30 | 2015-04-22 | 陕西科技大学 | 一种制备高比表面积SiC 纳米微球的方法 |
WO2020057095A1 (zh) * | 2018-09-20 | 2020-03-26 | 东北大学 | 一种利用感应炉制备碳化硅粉体的方法 |
CN114574892A (zh) * | 2022-03-11 | 2022-06-03 | 电子科技大学长三角研究院(湖州) | 一种以氧化物为模板瞬时高温合成过渡金属碳化物纳米阵列的方法 |
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