CN112125673B - 一种基于先驱体浸渍裂解工艺制备直角形长桁的方法 - Google Patents
一种基于先驱体浸渍裂解工艺制备直角形长桁的方法 Download PDFInfo
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Abstract
发明提出了一种基于先驱体浸渍裂解工艺制备直角形长桁的方法,针对先驱体浸渍裂解工艺的特点,设计了石墨模具工装,通过浸渍流道设计、高温均匀热传导控制实现了直角形长桁的小批量精确制造。本发明创新性地通过石墨模具工装的设计实现了模压成型载荷的均匀传递,保证了纤维预制体成型过程中均匀受力,厚度可控,避免了因受压不均匀而造成的成型质量不高的问题;通过合理的浸渍流道设计避免了直角形长桁致密化死角;致密化过程中确保直角形长桁整体受热传导方式加热,确保直角形长桁在升温‑裂解过程中的温度均匀性,避免因受热不均而产生热应力,最终导致直角形长桁的扭曲与变形,提高了直角形长桁的制备质量与精度。
Description
技术领域
本发明属于连续纤维增强陶瓷基复合材料的制备技术,具体涉及一种基于先驱体浸渍裂解工艺制备直角形长桁的方法。
背景技术
与传统高温合金相比,先驱体浸渍裂解工艺制备的连续纤维增强陶瓷基复合材料的密度仅为高温合金的1/3~1/4;工作温度可提高150℃以上,是国际公认的替代高温合金作为临近空间飞行器热防护系统的理想材料。
在飞行器总体结构中,长桁类结构件作为飞行器纵向承力构件,被广泛应用于机翼、机身等飞行器结构当中,是重要的构件之一,该类结构件受装配环境制约,外形大多扭曲复杂。
与采用高温合金制备长桁包括的合金选材、冲压、铣削、制孔等工序不同,采用先驱体浸渍裂解工艺制备直角形长桁的工序主要包括纤维预制体的编织、成型、致密化等工序,需要针对先驱体浸渍裂解工艺的特点和长桁构件的特点设计连续纤维增强陶瓷基复合材料的成型与制备方法,使之满足装配环境约束的要求,目前没有先驱体浸渍裂解工艺制备纤维增强陶瓷基复合材料直角形长桁用于临近空间飞行器高温热端部件的报道。
发明内容
本发明基于上述材料构件的需求和先驱体浸渍裂解工艺及构件的特点,创新性地提出了一种直角形长桁的成型工装、成型方法与致密化方案。
本方明的技术方案如下:
一种基于先驱体浸渍裂解工艺制备直角形长桁的方法,包括以下操作步骤:
(1)采用连续纤维束编织纤维预制体平板,制备纤维预制体;
(2)设计成型工装:依据直角形长桁构件的外形尺寸设计石墨模具工装;
(3)直角形长桁纤维预制体定型:将步骤(1)中得到的纤维预制体放入步骤(2)制得的石墨模具工装中定型并进行模压,得到直角形长桁纤维预制体;
(4)界面层制备:将直角形长桁纤维预制体放入化学气相沉积炉中采用CVI工艺(化学气相渗透工艺)制备界面层;
(5)先驱体溶液浸渍:将沉积界面层的直角形长桁纤维预制体放入石墨模具工装中固定后置于真空浸渍设备中,用真空泵对真空浸渍设备抽真空,真空浸渍设备内腔压力<100Pa时,将先驱体溶液通过不锈钢管路引入真空浸渍设备内腔,最终使沉积界面层的直角形长桁纤维预制体全部淹没于先驱体溶液中,浸渍处理12-48h;
(6)高温裂解:将浸渍先驱体溶液的直角形长桁纤维预制体置于石墨模具工装后一并放入高温裂解炉中进行高温裂解;高温裂解环境为真空环境或气氛环境中的任意一种,升温至先驱体陶瓷化转变点温度后保温0.5-2h;
(7)重复步骤5和步骤6至3-4次循环后,得到多孔的直角形长桁,将多孔的直角形长桁从石墨模具工装中脱模后置于真空浸渍设备中,用真空泵对真空浸渍设备抽真空,真空浸渍设备内腔压力<100Pa时,将陶瓷先驱体浸渍溶液通过不锈钢管路引入真空浸渍设备内腔,将多孔的直角形长桁再次淹没于陶瓷先驱体浸渍溶液,保持12-48h,然后将其放入再次置于石墨模具中并置于高温裂解炉中进行高温裂解,高温裂解环境为真空环境或气氛环境中的任意一种,升温至先驱体陶瓷化转变点温度后保温0.5-2.0h,脱模称重,重复浸渍-装模-高温裂解-脱模过程,待浸渍裂解后直角形长桁的重量与前次浸渍裂解后质量增重小于1%时,完成直角形长桁的基体致密化过程,得到致密化的直角形长桁坯体;
(8)直角形长桁的加工:将步骤7中致密化的直角形长桁坯体按照图纸要求进行加工,得到直角形长桁。
具体地,所述的连续纤维束包括碳纤维束、碳化硅纤维束、氮化硅纤维束、氧化铝纤维束且不限于上述几种。
具体地,所述的纤维预制体结构包括二维叠层结构、2.5维结构、三维四向结构中的任意一种。
具体地,自由状态时纤维预制体的厚度误差与构件的设计厚度正误差不大于10%。
具体地,所述石墨模具工装的上模主要用于外形面控制,芯模用于内形面和角度控制,在上模和芯模的形面外侧设有定位销孔和固定螺栓通孔,以防止因模压过程中造成的相对滑动以及裂解过程中因热膨胀导致的构件变形,芯模的直角形面夹角与水平线呈45度角,即V或倒V字型,以确保直角形纤维预制体的形面均匀受力。
具体地,上述步骤(3)中,模压时,模压压力为2-5MPa,模压时间为0.5h-2.0h,在上模和芯模的外侧形面处设有开孔,开孔大小直径3-5mm,孔间距10-20mm,开孔位置对应直角形长桁形面和直角棱处,以确保浸渍液均匀浸渍到纤维预制体内部,避免致密化死角。
具体地,上述步骤(4)中,界面层包括热解碳界面层或氮化硼界面层中的一种。
具体地,上述步骤(5)中,先驱体溶液包括但不限于碳化硅陶瓷先驱体溶液、氮化硅陶瓷先驱体溶液、硅硼碳氮陶瓷先驱体溶液中的任意一种或多种组合。
由以上的技术方案可知,本发明的有益效果是:
1)本发明创新性地通过上模和芯模的设计,使得纤维预制体在成型过程中均匀受力,厚度可控,实现直角形长桁构件预制体的成型与工程化制备;
2)通过合理的浸渍流道设计,实现了直角形长桁构件的均匀浸渍与致密化,避免了直角形长桁构件的致密化死角;
3)直角形长桁构件在升温-裂解过程中主要受热传导方式为加热,避免了直角形长桁构件在高温环境下的扭曲与变形;
4)本发明制得的直角形复合材料长桁构件较好地满足了临近空间飞行器热端构件对连续纤维增强陶瓷基复合材料直角形长桁的需求,在国防武器装备领域具有广阔的推广前景。
附图说明
图1是基于先驱体浸渍裂解工艺制备直角形长桁工艺路线图。
图2是实施例1中L形直角长桁石墨模具工装的立体结构示意图。
图3是实施例1中L形直角长桁石墨模具工装的剖面结构示意图。
图4是实施例2中Z形直角长桁石墨模具工装的立体结构示意图。
图5是实施例2中Z形直角长桁石墨模具工装的剖面结构示意图。
具体实施方式
下面将结合实施例对本发明的实施方案进行详细描述,但是本领域技术人员将会理解,下列实施例仅用于说明本发明,而不应视为限制本发明的范围。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。
一种基于先驱体浸渍裂解工艺制备直角形长桁的方法,包括以下操作步骤:
(1)采用连续纤维束编织纤维预制体平板,制备纤维预制体,其中连续纤维束包括碳纤维束、碳化硅纤维束、氮化硅纤维束、且不限于上述几种,纤维预制体结构包括二维叠层结构、2.5维结构、三维四向结构中的任意一种,自由状态时纤维预制体的厚度误差与构件的设计厚度正误差不大于10%;
(2)设计成型工装:依据直角形长桁构件的外形尺寸设计石墨模具工装,石墨模具工装包括上模、芯模、定位销和锁紧螺母,其中上模主要用于外形面控制,芯模用于内形面和角度控制,在上模和芯模的形面外侧设有定位销孔和固定螺栓通孔,以防止因模压过程中造成的相对滑动以及裂解过程中因热膨胀导致的构件变形,芯模的直角形面夹角与水平线呈45度角,即V或倒V字型,以确保直角形纤维预制体的形面均匀受力;
(3)直角形长桁纤维预制体定型:将步骤(1)中得到的纤维预制体放入步骤(2)制得的石墨模具工装中定型并进行模压,得到直角形长桁纤维预制体,模压时,模压压力为2-5MPa,模压时间为0.5h-2.0h,在上模和芯模的外侧形面处设有开孔,开孔大小直径3-5mm,孔间距10-20mm,开孔位置对应直角形长桁形面和直角棱处,以确保浸渍液均匀浸渍到纤维预制体内部,避免致密化死角;
(4)界面层制备:将直角形长桁纤维预制体放入化学气相沉积炉中制备界面层,界面层包括热解碳界面层或氮化硼界面层中的一种;
(5)先驱体溶液浸渍:将沉积界面层的直角形长桁纤维预制体放入石墨模具工装中固定后置于真空浸渍设备中,用真空泵对真空浸渍设备抽真空,真空浸渍设备内腔压力<100Pa时,将先驱体溶液通过不锈钢管路引入真空浸渍设备内腔,最终使沉积界面层的直角形长桁纤维预制体全部淹没于先驱体溶液中,浸渍处理12-48h;
(6)高温裂解:将浸渍先驱体溶液的直角形长桁纤维预制体置于石墨模具工装后一并放入高温裂解炉中进行高温裂解;高温裂解环境为真空环境或气氛环境中的一种,升温至先驱体陶瓷化转变点温度后保温0.5-2h,先驱体溶液包括但不限于碳化硅陶瓷先驱体溶液、氮化硅陶瓷先驱体溶液、硅硼碳氮陶瓷先驱体溶液中的任意一种或多种组合;
(7)重复步骤5和步骤6至3-4次循环后,得到多孔的直角形长桁,将多孔的直角形长桁从石墨模具工装中脱模后置于真空浸渍设备中,用真空泵对真空浸渍设备抽真空,真空浸渍设备内腔压力<100Pa时,将陶瓷先驱体浸渍溶液通过不锈钢管路引入真空浸渍设备内腔,将多孔的直角形长桁再次淹没于陶瓷先驱体浸渍溶液,保持12-48h,然后将其再次置于石墨模具中并置于高温裂解炉中进行高温裂解,高温裂解环境为真空环境或气氛环境中的任意一种,升温至先驱体陶瓷化转变点温度后保温0.5-2.0h,脱模称重,重复浸渍-装模-高温裂解-脱模过程,待浸渍裂解后直角形长桁的重量与前次浸渍裂解后质量增重小于1%时,完成直角形长桁的基体致密化过程,得到致密化的直角形长桁坯体;
(8)直角形长桁的加工:将步骤7中致密化的直角形长桁坯体按照图纸要求进行加工,得到直角形长桁。
为了对本发明的技术方案做进一步的解释,本发明提供SiC/SiC复合材料L形直角长桁和SiC/SiC复合材料Z形直角长桁的制备方法。
实施例1
如图2和图3所示,本实施例制备L形直角长桁石墨模具工装,通过L形直角长桁石墨模具工装对SiC纤维预制体进行模压定型,以丙烷和氩气为气源制备PyC界面层,以聚碳硅烷为前躯体,以二甲苯为溶剂制备SiC陶瓷基体,致密化后通过机械加工得到L形直角SiC/SiC复合材料长桁构件,具体的制备方法如下:
(1)碳化硅纤维预制体的制备:以0.5K碳化硅纤维束为增强体,采用编织方式制备2.5维结构碳化硅纤维预制体,2.5维结构纤维预制体的经纱与纬纱比为8:5,依据L形直角长桁的长度与宽度裁剪2.5维结构纤维预制体;
(2)设计L形直角长桁石墨模具工装:包括芯模1、上模2,浸渍流道3,定位销孔4和固定螺栓通孔5,其中L形长桁构件芯模为倒V字形芯模以保证L形长桁构件在模压过程中受力均匀,厚度可控;在上模和芯模的外侧形面处设有开孔,开孔大小直径3mm,孔间距20mm,开孔位置对应直角形长桁形面和直角棱处,以确保浸渍液均匀浸渍到纤维预制体内部,避免致密化死角;
(3)SiC/SiC直角形长桁纤维预制体定型:将步骤(1)中得到的2.5维结构纤维预制体放入步骤(2)制得的L形直角长桁石墨模具工装中定型并进行模压,得到2.5维结构的L形直角碳化硅纤维预制体,模压时,模压压力为4MPa,模压时间为0.5h,(4)PyC(热解碳界面层)界面层的制备:将步骤三中模压后的2.5维结构的L形直角碳化硅纤维预制体放入化学气相沉积炉内,将炉内抽真空,真空度至50Pa,然后升温至300℃,保温1h后继续升温至1000℃,保温1h,通入氩气和丙烷,两者流量比例为1:1,沉积压力为2000Pa,沉积15h后降温至室温,制得PyC界面层的厚度为200nm;
(5)SiC陶瓷先驱体浸渍溶液的配置:以聚碳硅烷先驱体为溶质,以二甲苯为溶剂,聚碳硅烷占先驱体浸渍溶液重量百分比的50%,在室温下均匀搅拌24h,得到SiC陶瓷先驱体浸渍溶液;将沉积热解碳界面层的L形直角SiC纤维预制体放入L形直角长桁石墨模具工装中固定后一并置于真空浸渍设备中,用真空泵对真空浸渍设备抽真空,真空浸渍设备内腔压力50Pa时,SiC陶瓷先驱体浸渍溶液通过不锈钢管路引入真空浸渍设备内腔,最终L形直角长桁石墨模具工装全部淹没于SiC陶瓷先驱体浸渍溶液,浸渍处理24h;
(6)高温裂解:将经过浸渍带L形直角长桁石墨模具工装的L形直角碳化硅纤维预制体放入高温裂解炉中,抽真空至小于1000Pa,以10℃/min的升温速率加热到1200℃,保温1h;
(7)重复步骤5和步骤6至4次循环后,得到多孔的SiC/SiC复合材料L形直角长桁,多孔的SiC/SiC复合材料L形直角长桁从L形直角长桁石墨模具工装中脱模后,用毛刷刷去表面裂解产物以打开构件表面孔隙,同时对L形直角长桁石墨模具工装进行表面清理,而后将多孔的SiC/SiC复合材料L形直角长桁重新置于真空浸渍设备中,用真空泵对真空浸渍设备抽真空,真空浸渍设备内腔压力为50Pa时,将SiC陶瓷先驱体浸渍溶液通过不锈钢管路引入真空浸渍设备内腔,最终L形直角长桁全部淹没于SiC陶瓷先驱体浸渍溶液,保持16小时;再将浸渍后的L形直角SiC/SiC复合材料长桁置于石墨模具工装后一并放入高温裂解炉中,抽真空至小于100Pa,以10℃/min的升温速率从室温加热到1200℃,保温1h;脱模称重,重复浸渍-装模-高温裂解-脱模过程,至多孔的SiC/SiC复合材料L形直角长桁的增重率较前次小于1%时,得到致密的SiC/SiC复合材料L形直角长桁坯体。
(8)对所制得SiC/SiC复合材料L形直角长桁构件进行机械加工,用1200目的水砂纸打磨,之后用无水乙醇将打磨处清洗干净并烘干,完成L形直角SiC/SiC复合材料长桁构件的制备。
实施例2
如图4和图5所示,本实施例制备Z形直角长桁石墨模具,通过Z形直角长桁石墨模具对SiC纤维预制体进行模压定型,以丙烷和氩气为气源制备PyC界面层,以聚碳硅烷为前躯体,以二甲苯为溶剂制备SiC陶瓷基体,致密化后通过机械加工得到Z形直角SiC/SiC复合材料长桁构件,具体的制备方法如下:
(1)碳化硅纤维预制体的制备:以0.5K碳化硅纤维束作为增强体,采用编织方式制备2.5维结构碳化硅纤维预制体,2.5维结构纤维预制体的经纱与纬纱比为8:5,依据Z形直角长桁的长度与宽度裁剪2.5维结构SiC纤维预制体;
(2)设计Z形直角长桁石墨模具工装,包括芯模6、上模7,浸渍流道8,定位销孔9和固定螺栓通孔10,其中Z形长桁构件芯模型面直角与水平线呈45°角以保证Z形长桁构件在模压过程中受力均匀,厚度可控;在上模和芯模的外侧形面处设有开孔,开孔大小直径4mm,孔间距15mm,开孔位置对应直角形长桁形面和直角棱处,以确保浸渍液均匀浸渍到纤维预制体内部,避免致密化死角;
(3)Z形直角碳化硅纤维预制体模压:将步骤(1)中得到的2.5维结构纤维预制体放入步骤(2)制得的Z形直角长桁石墨模具工装中定型并进行模压,得到2.5维结构的Z形直角碳化硅纤维预制体,模压时,模压压力为4MPa,模压时间为0.5h,(4)PyC界面层的制备:将步骤二中模压后的2.5维结构Z形直角碳化硅纤维预制体放入化学气相沉积炉内,将炉内抽真空,真空度至50Pa,然后升温至300℃,保温1h后继续升温至1000℃,保温1h,通入氩气和丙烷,两者流量比例为1:1,沉积压力为2000Pa,沉积15h后降温至室温,制得PyC界面层的厚度为200nm;
(5)SiC陶瓷先驱体浸渍溶液的配置:以聚碳硅烷先驱体为溶质,以二甲苯为溶剂,聚碳硅烷占先驱体浸渍溶液重量百分比的50%,在室温下均匀搅拌24h,得到SiC陶瓷先驱体浸渍溶液;将沉积热解碳界面层的Z形直角碳化硅纤维预制体放入Z形直角长桁石墨模具工装中固定后一并置于真空浸渍设备中,用真空泵对真空浸渍设备抽真空,真空浸渍设备内腔压力为50Pa时,将SiC陶瓷先驱体浸渍溶液通过不锈钢管路引入真空浸渍设备内腔,最终Z形直角长桁石墨模具工装全部淹没于SiC陶瓷先驱体浸渍溶液中,保持24h。
(6)高温裂解:将经过浸渍带Z形直角长桁石墨模具工装的Z形直角碳化硅纤维预制体放入高温裂解炉中,抽真空至小于1000Pa,以10℃/min的升温速率从室温加热到1200℃,保温1h。
(6)重复步骤5和步骤6至4循环后,得到多孔的SiC/SiC复合材料Z形直角长桁,将多孔的SiC/SiC复合材料从Z形直角长桁石墨模具工装中脱模后,用毛刷刷去表面裂解产物以打开构件表面孔隙,同时对Z形直角长桁石墨模具工装进行表面清理,而后将多孔的SiC/SiC复合材料Z形直角长桁置于真空浸渍设备中,用真空泵对真空浸渍设备抽真空,真空浸渍设备内腔压力50Pa时,将SiC陶瓷先驱体浸渍溶液通过不锈钢管路引入真空浸渍设备内腔,最终多孔的SiC/SiC复合材料Z形直角长桁全部淹没于SiC陶瓷先驱体浸渍溶液保持16小时;再次将多孔的SiC/SiC复合材料Z形直角长桁置于Z形直角长桁石墨模具后一并放入高温裂解炉中,抽真空50Pa,以10℃/min的升温速率从室温加热到1200℃,保温1h;脱模称重,重复浸渍-装模-高温裂解-脱模过程,至多孔的多孔的SiC/SiC复合材料Z形直角长桁的增重率较前次小于1%时,得到致密的SiC/SiC复合材料Z形直角长桁坯体;
(7)对所制SiC/SiC复合材料Z形直角长桁进行机械加工,用1200目的水砂纸打磨,之后用无水乙醇将打磨处清洗干净并烘干,完成SiC/SiC复合材料Z形直角长桁的制备。
以上所描述的实施例是本发明一部分实施例,而不是全部的实施例。本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围,而是仅仅表示本发明的选定实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
Claims (6)
1.一种基于先驱体浸渍裂解工艺制备直角形长桁的方法,其特征在于,包括以下操作步骤:
(1)采用连续纤维束编织纤维预制体平板,制备纤维预制体;
(2)设计成型工装:依据直角形长桁构件的外形尺寸设计石墨模具工装;所述石墨模具工装的上模主要用于外形面控制,芯模用于内形面和角度控制,在上模和芯模的形面外侧设有定位销孔和固定螺栓通孔,芯模的直角形面夹角与水平线呈45度角,即V或倒V字型;
(3)直角形长桁纤维预制体定型:将步骤(1)中得到的纤维预制体放入步骤(2)制得的石墨模具工装中定型并进行模压,得到直角形长桁纤维预制体;模压时,模压压力为2-5MPa,模压时间为0.5h-2.0h,在上模和芯模的外侧形面处设有开孔,开孔直径3-5mm,孔间距10-20mm,开孔位置对应直角形长桁形面和直角棱处;
(4)界面层制备:将直角形长桁纤维预制体放入化学气相沉积炉中制备界面层;
(5)先驱体溶液浸渍:将沉积界面层的直角形长桁纤维预制体放入石墨模具工装中固定后置于真空浸渍设备中,用真空泵对真空浸渍设备抽真空,真空浸渍设备内腔压力<100Pa时,将先驱体溶液通过不锈钢管路引入真空浸渍设备内腔,最终使沉积界面层的直角形长桁纤维预制体全部淹没于先驱体溶液中,浸渍处理12-48小时;
(6)高温裂解:将浸渍先驱体溶液的直角形长桁纤维预制体连同石墨模具工装一并放入高温裂解炉中进行高温裂解;高温裂解环境为真空环境或气氛环境中的任意一种,升温至先驱体陶瓷化转变点温度后保温0.5-2小时;
(7)重复步骤(5)和步骤(6)至3-4次循环后,得到多孔的直角形长桁,将多孔的直角形长桁从石墨模具工装中脱模后置于真空浸渍设备中,用真空泵对真空浸渍设备抽真空,真空浸渍设备内腔压力<100Pa时,将陶瓷先驱体浸渍溶液通过不锈钢管路引入真空浸渍设备内腔,将多孔的直角形长桁再次淹没于陶瓷先驱体浸渍溶液,保持12-48h,然后将其再次放入石墨模具工装中并置于高温裂解炉中进行高温裂解,高温裂解环境为真空环境或气氛环境中的任意一种,升温至先驱体陶瓷化转变点温度后保温0.5-2.0h,脱模称重,重复浸渍-装模-高温裂解-脱模过程,待浸渍裂解后直角形长桁的重量与前次浸渍裂解后质量增重小于1%时,完成直角形长桁的基体致密化过程,得到致密化的直角形长桁坯体;
(8)直角形长桁的加工:将步骤(7)中致密化的直角形长桁坯体按照图纸要求进行加工,得到直角形长桁。
2.根据权利要求1所述一种基于先驱体浸渍裂解工艺制备直角形长桁的方法,其特征在于,所述的连续纤维束包括碳纤维束、碳化硅纤维束、氮化硅纤维束、氧化铝纤维束中的任意一种。
3.根据权利要求1所述一种基于先驱体浸渍裂解工艺制备直角形长桁的方法,其特征在于,所述的纤维预制体结构包括二维叠层结构、2.5维结构、三维四向结构中的任意一种。
4.根据权利要求3所述一种基于先驱体浸渍裂解工艺制备直角形长桁的方法,其特征在于,自由状态时纤维预制体的厚度误差与构件的设计厚度正误差不大于10%。
5.根据权利要求1所述一种基于先驱体浸渍裂解工艺制备直角形长桁的方法,其特征在于,上述步骤(4)中,界面层包括热解碳界面层或氮化硼界面层中的一种。
6.根据权利要求1所述的一种基于先驱体浸渍裂解工艺制备直角形长桁的方法,其特征在于,上述步骤(5)中,先驱体溶液包括但不限于碳化硅陶瓷先驱体溶液、氮化硅陶瓷先驱体溶液、硅硼碳氮陶瓷先驱体溶液中的任意一种或多种组合。
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