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1. 发明授权

US07786253B2 Apparatus and method for oxidation and stabilization of polymeric materials 有权
标题翻译：用于氧化和稳定聚合材料的装置和方法
公开(公告)号：US07786253B2
公开(公告)日：2010-08-31
申请号：US12466092
申请日：2009-05-14
申请人： Felix L. Paulauskas , Terry L. White , Daniel M. Sherman
发明人： Felix L. Paulauskas , Terry L. White , Daniel M. Sherman
IPC分类号： C08G64/00 , C08G63/02
CPC分类号： B29C59/14 , B29C2059/145 , B29K2033/20 , C08J3/24 , C08J2333/20 , D01F9/14 , D01F9/225 , D06M10/06 , D06M2101/28 , Y10T428/24942 , Y10T428/31663
摘要： An apparatus for treating polymeric materials comprises a treatment chamber adapted to maintain a selected atmosphere; a means for supporting the polymeric material within the chamber; and, a source of plasma-derived gas containing at least one reactive oxidative species whereby the polymer is stabilized and cross linked through exposure to the oxidative species in the chamber at a selected temperature. The polymer may be directly exposed to the plasma, or alternatively, the plasma may be established in a separate volume from which the reactive species may be extracted and introduced into the vicinity of the polymer. The apparatus may be configured for either batch-type or continuous-type processing. The apparatus and method are especially useful for preparing polymer fibers, particularly PAN fibers, for later carbonization treatments.
摘要翻译：一种用于处理聚合材料的设备包括适于保持选定气氛的处理室; 用于在腔室内支撑聚合材料的装置; 以及含有至少一种反应性氧化物质的等离子体衍生气体的来源，由此聚合物通过在选定温度下暴露于室中的氧化物质而稳定并交联。聚合物可以直接暴露于等离子体，或者，等离子体可以建立在单独的体积中，反应物质可以从该体积中提取并引入到聚合物附近。该装置可以被配置为分批式或连续型处理。该设备和方法特别适用于制备聚合物纤维，特别是PAN纤维，用于后续的碳化处理。

2. 发明申请

US20090263295A1 APPARATUS AND METHOD FOR OXIDATION AND STABILIZATION OF POLYMERIC MATERIALS 有权
标题翻译：聚合材料氧化和稳定化的装置和方法
公开(公告)号：US20090263295A1
公开(公告)日：2009-10-22
申请号：US12466092
申请日：2009-05-14
申请人： Felix L. Paulauskas , Terry L. White , Daniel M. Sherman
发明人： Felix L. Paulauskas , Terry L. White , Daniel M. Sherman
IPC分类号： G21C1/00 , B01J19/08 , B01J19/12
CPC分类号： B29C59/14 , B29C2059/145 , B29K2033/20 , C08J3/24 , C08J2333/20 , D01F9/14 , D01F9/225 , D06M10/06 , D06M2101/28 , Y10T428/24942 , Y10T428/31663
摘要： An apparatus for treating polymeric materials comprises a treatment chamber adapted to maintain a selected atmosphere; a means for supporting the polymeric material within the chamber; and, a source of plasma-derived gas containing at least one reactive oxidative species whereby the polymer is stabilized and cross linked through exposure to the oxidative species in the chamber at a selected temperature. The polymer may be directly exposed to the plasma, or alternatively, the plasma may be established in a separate volume from which the reactive species may be extracted and introduced into the vicinity of the polymer. The apparatus may be configured for either batch-type or continuous-type processing. The apparatus and method are especially useful for preparing polymer fibers, particularly PAN fibers, for later carbonization treatments.
摘要翻译：一种用于处理聚合材料的设备包括适于保持选定气氛的处理室; 用于在腔室内支撑聚合材料的装置; 以及含有至少一种反应性氧化物质的等离子体衍生气体的来源，由此聚合物通过在选定温度下暴露于室中的氧化物质而稳定并交联。聚合物可以直接暴露于等离子体，或者，等离子体可以建立在单独的体积中，反应物质可以从该体积中提取并引入到聚合物附近。该装置可以被配置为分批式或连续型处理。该设备和方法特别适用于制备聚合物纤维，特别是PAN纤维，用于后续的碳化处理。

3. 发明授权

US07534854B1 Apparatus and method for oxidation and stabilization of polymeric materials 有权
标题翻译：用于氧化和稳定聚合材料的装置和方法
公开(公告)号：US07534854B1
公开(公告)日：2009-05-19
申请号：US11344573
申请日：2006-01-31
申请人： Felix L. Paulauskas , Terry L. White , Daniel M. Sherman
发明人： Felix L. Paulauskas , Terry L. White , Daniel M. Sherman
IPC分类号： C08F6/00 , C08J3/00
CPC分类号： B29C59/14 , B29C2059/145 , B29K2033/20 , C08J3/24 , C08J2333/20 , D01F9/14 , D01F9/225 , D06M10/06 , D06M2101/28 , Y10T428/24942 , Y10T428/31663
摘要： An apparatus for treating polymeric materials comprises a treatment chamber adapted to maintain a selected atmosphere; a means for supporting the polymeric material within the chamber; and, a source of plasma-derived gas containing at least one reactive oxidative species whereby the polymer is stabilized and cross linked through exposure to the oxidative species in the chamber at a selected temperature. The polymer may be directly exposed to the plasma, or alternatively, the plasma may be established in a separate volume from which the reactive species may be extracted and introduced into the vicinity of the polymer. The apparatus may be configured for either batch-type or continuous-type processing. The apparatus and method are especially useful for preparing polymer fibers, particularly PAN fibers, for later carbonization treatments.
摘要翻译：一种用于处理聚合材料的设备包括适于保持选定气氛的处理室; 用于在腔室内支撑聚合材料的装置; 以及含有至少一种反应性氧化物质的等离子体衍生气体的来源，由此通过在所选择的温度下暴露于室中的氧化物质来稳定和交联聚合物。聚合物可以直接暴露于等离子体，或者，等离子体可以建立在单独的体积中，反应物质可以从该体积中提取并引入到聚合物附近。该装置可以被配置为分批式或连续型处理。该设备和方法特别适用于制备聚合物纤维，特别是PAN纤维，用于后续的碳化处理。

4. 发明授权

US07824495B1 System to continuously produce carbon fiber via microwave assisted plasma processing 有权
标题翻译：系统通过微波辅助等离子体处理连续生产碳纤维
公开(公告)号：US07824495B1
公开(公告)日：2010-11-02
申请号：US11270065
申请日：2005-11-09
申请人： Terry L. White , Felix L. Paulauskas , Timothy S. Bigelow
发明人： Terry L. White , Felix L. Paulauskas , Timothy S. Bigelow
IPC分类号： C23C16/00 , C23F1/00
CPC分类号： B01J19/126 , D01F9/32 , D06M10/025 , H01J37/32192 , H01J37/32229
摘要： A system to continuously produce fully carbonized or graphitized carbon fibers using microwave-assisted plasma (MAP) processing comprises an elongated chamber in which a microwave plasma is excited in a selected gas atmosphere. Fiber is drawn continuously through the chamber, entering and exiting through openings designed to minimize in-leakage of air. There is a gradient of microwave power within the chamber with generally higher power near where the fiber exits and lower power near where the fiber enters. Polyacrylonitrile (PAN), pitch, or any other suitable organic/polymeric precursor fibers can be used as a feedstock for the inventive system. Oxidized or partially oxidized PAN or pitch or other polymeric fiber precursors are run continuously through a MAP reactor in an inert, non-oxidizing atmosphere to heat the fibers, drive off the unwanted elements such as oxygen, nitrogen, and hydrogen, and produce carbon or graphite fibers faster than conventionally produced carbon fibers.
摘要翻译：使用微波辅助等离子体（MAP）处理连续生产完全碳化或石墨化的碳纤维的系统包括其中微波等离子体在所选择的气体气氛中被激发的细长室。纤维被连续地抽吸通过室，通过设计成最小化空气泄漏的开口进入和离开。室内具有微波功率的梯度，在光纤出口附近具有通常较高的功率，在纤维进入附近的功率较低。聚丙烯腈（PAN），沥青或任何其它合适的有机/聚合物前体纤维可用作本发明体系的原料。氧化或部分氧化的PAN或沥青或其它聚合物纤维前体在惰性非氧化气氛中连续通过MAP反应器，以加热纤维，驱除不需要的元素如氧，氮和氢，并产生碳或石墨纤维比常规生产的碳纤维更快。

5. 发明授权

US06514449B1 Microwave and plasma-assisted modification of composite fiber surface topography 有权
标题翻译：复合纤维表面形貌的微波和等离子体辅助改性
公开(公告)号：US06514449B1
公开(公告)日：2003-02-04
申请号：US09668246
申请日：2000-09-22
申请人： Felix L. Paulauskas , Terry L. White , Timothy S. Bigelow
发明人： Felix L. Paulauskas , Terry L. White , Timothy S. Bigelow
IPC分类号： B29C5916
CPC分类号： B29C70/16 , B29C70/54 , D01D10/00 , D06M10/003 , D06M10/025
摘要： The present invention introduces a novel method for producing an undulated surface on composite fibers using plasma technology and microwave radiation. The undulated surface improves the mechanical interlocking of the fibers to composite resins and enhances the mechanical strength and interfacial sheer strength of the composites in which they are introduced.
摘要翻译：本发明引入了使用等离子体技术和微波辐射在复合纤维上制造起伏表面的新颖方法。波纹表面改善了纤维与复合树脂的机械互锁，并提高了其引入复合材料的机械强度和界面剪切强度。

6. 发明授权

US08679592B2 System to continuously produce carbon fiber via microwave assisted plasma processing 有权
标题翻译：系统通过微波辅助等离子体处理连续生产碳纤维
公开(公告)号：US08679592B2
公开(公告)日：2014-03-25
申请号：US12897372
申请日：2010-10-04
申请人： Terry L. White , Felix L. Paulauskas , Timothy S. Bigelow
发明人： Terry L. White , Felix L. Paulauskas , Timothy S. Bigelow
IPC分类号： H05H1/46 , B05D3/02 , B05D3/06 , C01B31/02 , C01B31/04
CPC分类号： B01J19/126 , D01F9/32 , D06M10/025 , H01J37/32192 , H01J37/32229
摘要： A method for continuously processing carbon fiber including establishing a microwave plasma in a selected atmosphere contained in an elongated chamber having a microwave power gradient along its length defined by a lower microwave power at one end and a higher microwave power at the opposite end of the elongated chamber. The elongated chamber having an opening in each of the ends of the chamber that are adapted to allow the passage of the fiber tow while limiting incidental gas flow into or out of said chamber. A continuous fiber tow is introduced into the end of the chamber having the lower microwave power. The fiber tow is withdrawn from the opposite end of the chamber having the higher microwave power. The fiber to is subjected to progressively higher microwave energy as the fiber is being traversed through the elongated chamber.
摘要翻译：一种用于连续处理碳纤维的方法，包括在包含在具有微波功率梯度的细长室中的选定气氛中建立微波等离子体，该微波功率梯度沿着其长度由一端的较低微波功率限定，并且在细长的另一端具有较高的微波功率房间。细长室具有在室的每个端部中的开口，其适于允许纤维束的通过，同时限制偶然的气体流入或流出所述室。将连续的纤维束引入具有较低微波功率的室的端部。纤维束从具有较高微波功率的腔室的相对端排出。当纤维穿过细长室时，纤维经受逐渐更高的微波能量。

7. 发明申请

US20110079505A1 SYSTEM TO CONTINUOUSLY PRODUCE CARBON FIBER VIA MICROWAVE ASSISTED PLASMA PROCESSING 有权
标题翻译：通过微波辅助等离子体处理连续生产碳纤维的系统
公开(公告)号：US20110079505A1
公开(公告)日：2011-04-07
申请号：US12897372
申请日：2010-10-04
申请人： Terry L. White , Felix L. Paulauskas , Timothy S. Bigelow
发明人： Terry L. White , Felix L. Paulauskas , Timothy S. Bigelow
IPC分类号： D01F11/16
CPC分类号： B01J19/126 , D01F9/32 , D06M10/025 , H01J37/32192 , H01J37/32229
摘要： A method for continuously processing carbon fiber including establishing a microwave plasma in a selected atmosphere contained in an elongated chamber having a microwave power gradient along its length defined by a lower microwave power at one end and a higher microwave power at the opposite end of the elongated chamber. The elongated chamber having an opening in each of the ends of the chamber that are adapted to allow the passage of the fiber tow while limiting incidental gas flow into or out of said chamber. A continuous fiber tow is introduced into the end of the chamber having the lower microwave power. The fiber tow is withdrawn from the opposite end of the chamber having the higher microwave power. The fiber to is subjected to progressively higher microwave energy as the fiber is being traversed through the elongated chamber.
摘要翻译：一种用于连续处理碳纤维的方法，包括在包含在具有微波功率梯度的细长室中的选定气氛中建立微波等离子体，该微波功率梯度沿着其长度由一端的较低微波功率限定，并且在细长的另一端具有较高的微波功率房间。细长室具有在室的每个端部中的开口，其适于允许纤维束的通过，同时限制偶然的气体流入或流出所述室。将连续的纤维束引入具有较低微波功率的室的端部。纤维束从具有较高微波功率的腔室的相对端排出。当纤维穿过细长室时，纤维经受逐渐更高的微波能量。

8. 发明授权

US08227051B1 Apparatus and method for carbon fiber surface treatment 有权
标题翻译：碳纤维表面处理设备及方法
公开(公告)号：US08227051B1
公开(公告)日：2012-07-24
申请号：US11159006
申请日：2005-06-22
申请人： Felix L. Paulauskas , Daniel M. Sherman
发明人： Felix L. Paulauskas , Daniel M. Sherman
IPC分类号： H05H1/24 , B05D3/06
CPC分类号： H05H1/2406 , C04B35/62844 , C04B2235/5248 , C04B2235/6585 , D06M10/025 , D06M10/06 , D06M11/34 , D06M2101/40 , H05H2001/2412
摘要： An apparatus and method for enhancing the surface energy and/or surface chemistry of carbon fibers involves exposing the fibers to direct or indirect contact with atmospheric pressure plasma generated using a background gas containing at least some oxygen or other reactive species. The fiber may be exposed directly to the plasma, provided that the plasma is nonfilamentary, or the fiber may be exposed indirectly through contact with gases exhausting from a plasma discharge maintained in a separate volume. In either case, the process is carried out at or near atmospheric pressure, thereby eliminating the need for vacuum equipment. The process may be further modified by moistening the fibers with selected oxygen-containing liquids before exposure to the plasma.
摘要翻译：用于增强碳纤维的表面能和/或表面化学性质的装置和方法包括将纤维暴露于使用含有至少一些氧或其它反应性物质的背景气体产生的大气压等离子体的直接或间接接触。光纤可以直接暴露于等离子体，只要等离子体是非离子的，或者纤维可以通过与维持在单独体积中的等离子体放电排出的气体接触而间接暴露。在任一情况下，该过程在大气压或接近大气压下进行，从而不需要真空设备。可以通过在暴露于等离子体之前用选择的含氧液体润湿纤维来进一步修饰该方法。

9. 发明授权

US07649078B1 Apparatus and method for stabilization or oxidation of polymeric materials 有权
标题翻译：用于稳定或氧化聚合材料的装置和方法
公开(公告)号：US07649078B1
公开(公告)日：2010-01-19
申请号：US11391615
申请日：2006-03-28
申请人： Felix L. Paulauskas , Daniel M. Sherman
发明人： Felix L. Paulauskas , Daniel M. Sherman
IPC分类号： C08G63/02 , B32B27/06
CPC分类号： B29C59/14 , B29C2059/145 , B29K2033/20 , C01B13/10 , C08J7/12 , D01F9/328 , D06M10/06 , D06M11/34 , Y10T428/2904
摘要： An apparatus for treating polymeric materials comprises a treatment chamber adapted to maintain a selected atmosphere at a selected temperature; a means for supporting the polymeric material within the chamber; and, a source of ozone-containing gas, which decomposes at the selected temperature yielding at least one reactive oxidative species whereby the polymer is stabilized and cross linked through exposure to the oxidative species in the chamber at the selected temperature. The ozone may be generated by a plasma discharge or by various chemical processes. The apparatus may be configured for either batch-type or continuous-type processing. The apparatus and method are especially useful for preparing polymer fibers, particularly PAN fibers, for later carbonization treatments as well as to make flame-retardant fabrics.
摘要翻译：一种用于处理聚合材料的设备包括适于将选定气氛保持在选定温度的处理室; 用于在腔室内支撑聚合材料的装置; 以及含有臭氧的气体源，其在所选择的温度下分解，产生至少一种反应性氧化物质，由此通过在所选择的温度下暴露于室中的氧化物质使聚合物稳定并交联。臭氧可以通过等离子体放电或各种化学过程产生。该装置可以被配置为分批式或连续型处理。该装置和方法特别适用于制备聚合物纤维，特别是PAN纤维，用于后续的碳化处理以及制备阻燃织物。

10. 发明授权

US08741395B2 Apparatus and method for carbon fiber surface treatment 有权
标题翻译：碳纤维表面处理设备及方法
公开(公告)号：US08741395B2
公开(公告)日：2014-06-03
申请号：US13555476
申请日：2012-07-23
申请人： Felix L. Paulauskas , Daniel M. Sherman
发明人： Felix L. Paulauskas , Daniel M. Sherman
IPC分类号： H05H1/24 , H05H1/00
CPC分类号： H05H1/2406 , C04B35/62844 , C04B2235/5248 , C04B2235/6585 , D06M10/025 , D06M10/06 , D06M11/34 , D06M2101/40 , H05H2001/2412
摘要： An apparatus and method for enhancing the surface energy and/or surface chemistry of carbon fibers involves exposing the fibers to direct or indirect contact with atmospheric pressure plasma generated using a background gas containing at least some oxygen or other reactive species. The fiber may be exposed directly to the plasma, provided that the plasma is nonfilamentary, or the fiber may be exposed indirectly through contact with gases exhausting from a plasma discharge maintained in a separate volume. In either case, the process is carried out at or near atmospheric pressure, thereby eliminating the need for vacuum equipment. The process may be further modified by moistening the fibers with selected oxygen-containing liquids before exposure to the plasma.
摘要翻译：用于增强碳纤维的表面能和/或表面化学性质的装置和方法包括将纤维暴露于使用含有至少一些氧或其它反应性物质的背景气体产生的大气压等离子体的直接或间接接触。光纤可以直接暴露于等离子体，只要等离子体是非离子的，或者纤维可以通过与维持在单独体积中的等离子体放电排出的气体接触而间接暴露。在任一情况下，该过程在大气压或接近大气压下进行，从而不需要真空设备。可以通过在暴露于等离子体之前用选择的含氧液体润湿纤维来进一步修饰该方法。

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