WO2019127335A1 - 一种氧化石墨烯过滤膜制造方法 - Google Patents

一种氧化石墨烯过滤膜制造方法 Download PDF

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WO2019127335A1
WO2019127335A1 PCT/CN2017/119757 CN2017119757W WO2019127335A1 WO 2019127335 A1 WO2019127335 A1 WO 2019127335A1 CN 2017119757 W CN2017119757 W CN 2017119757W WO 2019127335 A1 WO2019127335 A1 WO 2019127335A1
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graphene
copper foil
graphene oxide
foil substrate
sccm
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PCT/CN2017/119757
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French (fr)
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袁志山
杨武斌
王成勇
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广东工业大学
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Priority to PCT/CN2017/119757 priority Critical patent/WO2019127335A1/zh
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means

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  • the invention belongs to the micro-nano manufacturing and application technology, in particular to a method for manufacturing a graphene oxide filter membrane.
  • the oil-water separation technology has been receiving much attention from people to solve the problem of crude oil exploitation, marine oil leakage, industrial and domestic oily sewage, which have caused great harm to the environment and ecological balance.
  • membrane technology has been widely used in the field of oil-water separation.
  • the principle of oil-water separation based on membrane technology is to achieve separation by utilizing the super-hydrophilic/super-oleophobic and super-hydrophobic/super-lipophilic properties of the membrane surface.
  • Membrane technology is an effective and simple method for the treatment of oily wastewater.
  • the metal film has good mechanical properties and can carry a large amount of oil-water mixture.
  • the metal itself is hydrophilic, oleophilic and the chemical nature of the metal itself is relatively active. Therefore, the use of a metal film for oil-water separation requires modification of the surface to improve the surface properties of the metal.
  • the object of the present invention is to provide a method for detecting molecular markers of tumor markers, which is used for solving the drawbacks of the existing nanopore detection technology, and can effectively reduce the complexity of the detection method.
  • the present invention provides a method for producing a graphene oxide filter membrane, the method comprising the steps of:
  • the copper foil substrate is a double-sided polished copper foil substrate, and the copper foil substrate has a thickness of 50 ⁇ m to 500 ⁇ m.
  • the laser used in the laser processing is one of a nanosecond laser, a picosecond laser, and a femtosecond laser.
  • the laser has a laser wavelength of 532 nm or 775 nm or 1064 nm or 1550 nm.
  • the average power of the nanosecond laser is 15W-30W
  • the average power of the picosecond laser is 10W-20W
  • the average power of the femtosecond laser is 0.5W-2W.
  • the laser engraving frequency is 15 to 75 times during laser processing, the laser scanning speed is 40 to 1000 mm/s, and the laser frequency is 1 Hz to 100 MHz.
  • the micro-hole array is 50 ⁇ 50-100 ⁇ 100
  • the micro-hole array spacing is 100 ⁇ m-200 ⁇ m
  • the micro-hole array aperture diameter is 50 ⁇ m-100 ⁇ m
  • the micro-hole array occupies an area of 25 mm 2 . ⁇ 400mm2.
  • the machine is manufactured by using a drilling machine, and the feeding speed of the drilling machine is 0.8 m/min to 1.2 m/min, and the retracting speed is 5 m/min to 7 m/min.
  • the step S3 further includes the following steps:
  • the cleaned copper foil substrate is placed in the center of the tube furnace, and argon gas is introduced to discharge the air in the furnace tube;
  • the temperature is raised, the heating rate is 10 ° C / min, and the argon flow rate is maintained at 100 sccm to 200 sccm.
  • methane is introduced, the flow rate of methane is from 20 sccm to 25 sccm, graphene is grown on the surface of the copper foil substrate and the inner pore wall, and the growth time is 5 min to 10 min;
  • the hydrogen gas and methane are turned off, and the argon gas flow rate is adjusted to 100 sccm to 200 sccm until cooling to room temperature.
  • the step S4 further includes the following steps:
  • the surface of the graphene copper foil substrate is placed in the center of the tube furnace, air is introduced, and the air flow rate is 100 sccm to 200 sccm;
  • heating temperature is 300 ° C ⁇ 600 ° C, maintaining the temperature in the interval of 300 ° C ⁇ 600 ° C 5 min ⁇ 10 min;
  • the detection method is simple and fast.
  • the concentration of the tumor marker is determined by detecting the magnitude of the blockage current drop in the nanopore array.
  • the detection time is short, which improves the detection efficiency.
  • the nanopore sensor has a detection accuracy of a single molecule level. Therefore, the tumor marker molecule of the present invention has a high level of detection and is suitable for early detection of cancer.
  • FIG. 1 is a schematic view showing the process flow of a method for producing a graphene oxide filter membrane of the present invention.
  • FIG 2 is a schematic view of a copper foil substrate in the present invention.
  • FIG. 3 is a schematic view showing the structure of a series of micro-hole arrays in the present invention.
  • Figure 4 is a schematic view showing the structure of the graphene surface and the inner wall of the graphene in the present invention.
  • Fig. 5 is a partially enlarged schematic view showing a portion A in Fig. 4.
  • Figure 6 is a schematic view showing the structure of the surface of the graphene oxide copper foil substrate and the inner wall of the graphene oxide in the present invention.
  • Fig. 7 is a partially enlarged schematic view showing a portion B in Fig. 6.
  • Figure 8 is a microscopic view of the graphene oxide filter membrane of the present invention.
  • microporous array 100, microporous array inner pore wall, 2, graphene, 20, graphene pore array, 200, graphene pore inner wall, 3, graphene oxide, 30, graphite oxide Olefin array, 300, graphene oxide inner pore wall.
  • the present invention provides a method for molecular detection of tumor markers, the method comprising the steps of:
  • S2 a series of micro-hole arrays 10 are disposed on the copper foil substrate 1 by laser processing or machining;
  • the graphene 2 includes a graphene hole array 20 and a graphene pore inner wall 200 disposed on the graphene hole array 20.
  • the copper foil substrate 1 is a double-sided polished copper foil having a thickness of 50 ⁇ m to 500 ⁇ m.
  • a series of microporous arrays 10 are fabricated on the copper foil substrate 1 by laser processing.
  • the laser used for laser processing may be a nanosecond laser, and the picosecond laser may also be a fly. Second laser.
  • the micropore array 10 is 50 ⁇ 50 ⁇ m to 100 ⁇ 100 ⁇ m, the micropore array 10 has a pitch of 100 ⁇ m to 200 ⁇ m, the micropore array 10 has a pore diameter of 50 ⁇ m to 100 ⁇ m, and the micropore array 10 occupies an area of 25 mm 2 to 400 mm 2 , and the laser wavelength is For 532 nm or 775 nm or 1064 nm or 1550 nm, the average power of the nanosecond laser is 15W to 30W, the average power of the picosecond laser is 10W to 20W, and the average power of the femtosecond laser is 0.5W to 2W.
  • the number of laser engravings is 15 to 75, the laser scanning speed is 40 to 1000 mm/s, and the
  • a series of microwell arrays 10 are fabricated on a copper foil substrate 1 by mechanical processing, and the machining is performed using a drill press.
  • the micro-hole array 10 is 50 ⁇ 50-100 ⁇ 100, the micro-hole array 10 has a pitch of 100 ⁇ m-200 ⁇ m, the micro-hole array 10 has a hole diameter of 50 ⁇ m-100 ⁇ m, and the micro-hole array 10 occupies an area of 25 mm 2 to 400 mm 2 , and the drilling speed is
  • the feed rate is from 200000 r/min to 300,000 r/min, the feed rate is from 0.8 m/min to 1.2 m/min, and the retraction speed is from 5 m/min to 7 m/min.
  • the step of growing the graphene 2 on the surface of the copper foil substrate 1 and the inner pore wall by the chemical vapor deposition method in the S3 step to obtain the graphene surface and the graphene inner pore wall 200 further includes the following steps:
  • the cleaned copper foil substrate is placed in the center of the tube furnace, and argon gas is introduced to discharge the air in the furnace tube;
  • the temperature is raised, the heating rate is 10 ° C / min, and the argon flow rate is maintained at 100 sccm to 200 sccm.
  • methane is introduced, the flow rate of methane is from 20 sccm to 25 sccm, graphene is grown on the surface of the copper foil substrate 1 and the inner pore wall, and the growth time is 5 min to 10 min;
  • the hydrogen gas and methane are turned off, and the argon gas flow rate is adjusted to 100 sccm to 200 sccm until cooling to room temperature.
  • the surface of the graphene copper foil substrate and the graphene inner pore wall 200 are heated and oxidized in the air to obtain the surface of the graphene oxide copper foil substrate and the graphene oxide inner pore wall 300 in the step S4. :
  • the surface of the graphene copper foil substrate is placed in the center of the tube furnace, air is introduced, and the air flow rate is 100 sccm to 200 sccm;
  • heating temperature is 300 ° C ⁇ 600 ° C, maintaining the temperature in the interval of 300 ° C ⁇ 600 ° C 5 min ⁇ 10 min;
  • a method for producing a graphene oxide filter membrane according to an embodiment of the invention.
  • a copper foil substrate 1 is first provided.
  • a series of microwell arrays 10 are fabricated on the copper foil substrate 1 by laser processing.
  • graphene is grown on the surface of the copper foil substrate 1 and the inner pore walls by chemical vapor deposition to obtain a graphene surface and a graphene inner pore wall 200.
  • the surface of the graphene copper foil substrate 1 and the graphene inner pore wall 200 are heated and oxidized in the air to obtain the surface of the graphene oxide copper foil substrate 1 and the graphene oxide inner pore wall 300.
  • the method for preparing the graphene oxide filter membrane is simple, easy to perform, has the ability to prevent oil clogging, has high durability, and can realize high-efficiency oil-water mixture separation.
  • the method for detecting molecular markers of tumor markers provided by the present invention solves the problems of the types of blocking current signals encountered by the former using nanopore to detect tumor markers, complex components, and long detection period. Moreover, the method for detecting molecular markers of tumor markers proposed by the invention is easy to integrate, realizes multi-channel parallel detection, and improves detection efficiency. In addition, the invention has simple operation, good expandability and wide application range. Therefore, the present invention effectively overcomes various shortcomings in the prior art and has high industrial utilization value.

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Abstract

一种氧化石墨烯过滤膜制造方法。包括：首先提供一铜箔基板（1）。接着，通过激光加工或者机械加工的方法在铜箔基板（1）上制造出一系列微米孔阵列（2）。接着，利用化学气相沉积法在铜箔基板（1）表面与内孔壁上生长石墨烯（2）得到石墨烯（2）表面与石墨烯内孔壁（200）。最后，将石墨烯铜箔基板表面与石墨烯内孔壁（200）在空气中加热氧化得到氧化石墨烯铜箔基板表面与氧化石墨烯内孔壁（300）。

Description

一种氧化石墨烯过滤膜制造方法 技术领域
本发明属于微纳制造与应用技术，特别是一种氧化石墨烯过滤膜的制造方法。
背景技术
油水分离技术一直备受人们关注，期以解决原油开采，海洋石油泄漏，工业、生活含油污水等对环境和生态平衡带来极大的危害。随着膜技术的迅速发展以及表面湿润状态理论建立使得膜技术在油水分离领域得到广泛的应用。基于膜技术的油水分离原理是利用膜表面超亲水/超疏油和超疏水/超亲油的性质实现分离。膜技术是对含油污水处理的有效、简单的方法。
金属膜具有良好的力学性能，可以承载大量的油水混合物。但是金属本身是亲水，亲油的而且金属本身化学性质较为活泼，因此利用金属膜进行油水分离需要对表面进行修饰，改善金属表面性质。
中国发明专利申请(公开号CN105268326A)中，提出了一种在超亲水疏油金属网膜上修饰长链烷酸或长链长链烷基硫醇制造超疏水亲油金属网膜的方法。由于长链烷酸或长链长链烷基利用化学键连接在金属网上，但化学键容易受到外部环境的影响，如温度，PH值等影响，最终使得表面的修饰物脱落，失去油水分离的能力。
发明内容
鉴于以上所述现有技术的缺点，本发明的目的在于提供一种肿瘤标志物分子检测的方法，用于解决现有纳米孔检测技术的弊端，能有效降低检测方法的复杂程度问题。
为实现上述目的及其他相关目的，本发明提供一种氧化石墨烯过滤膜制造方法，所述制作方法包括如下步骤：
S1：提供一铜箔基板；
S2：通过激光加工或机械加工的方法在铜箔基板上设置一系列微米孔阵列；
S3：利用化学气相沉积法在铜箔基板表面与微米孔阵列的内孔壁上生长石墨烯获得石墨烯表面与石墨烯内孔壁；
S4：将石墨烯铜箔基板表面与石墨烯内孔壁在空气中加热氧化获得氧化石墨烯铜箔基板表面与氧化石墨烯内孔壁。
优选地，所述S1步骤中，铜箔基板为双面抛光的铜箔基板，铜箔基板的厚度为50μm～500μm。
优选地，所述S2步骤中，激光加工时使用的激光器为纳秒激光器、皮秒激光器、飞秒激光器的其中一种。
优选地，所述激光器的激光波长为532nm或775nm或1064nm或1550nm。
优选地，所述纳秒激光器平均功率为15W～30W，皮秒激光器平均功率为10W～20W，飞秒激光器平均功率为0.5W～2W。
优选地，所述S2步骤中，激光加工时激光器的雕刻次数为15次～75次，激光器扫描速度为40～1000mm/s，激光频率为1Hz～100MHz。
优选地，所述S2步骤中，微米孔阵列为50×50～100×100，微米孔阵列间距为100μm～200μm，微米孔阵列孔直径为50μm～100μm，微米孔阵列所占据的区域面积为25mm2～400mm2。
优选地，所述S2步骤中，机械加工时采用钻床制造，所述钻床的进给速度为0.8米/分钟～1.2米/分钟，退刀速度为5米/分钟～7米/分钟。
优选地，所述S3步骤中还包括如下步骤：
A1、将清洗后的铜箔衬底放入管式炉中央，通入氩气，将炉管内空气排出后；
A2、开始升温，升温速率10℃/min，保持氩气流量100sccm～200sccm。
A3、当炉管温度加热到800℃-1000℃时，通入氢气，氢气的流量为850sccm～950sccm，使衬底在氢气和氩气的气氛下退火20min～30min；
A4、退火结束后，通入甲烷，甲烷的流量为20sccm～25sccm，铜箔基板表面和内孔壁上开始生长石墨烯，生长时间为5min～10min；
A5、生长结束后，关闭氢气和甲烷，将氩气流量调整为100sccm～200sccm直到冷却到室温。
优选地，所述S4步骤中还包括如下步骤：
B1、将所述石墨烯铜箔基板表面放入管式炉中央，通入空气，空气流量为100sccm～200sccm；
B2、加热温度为300℃～600℃，保持温度在300℃～600℃的区间内5min～10min；
B3、氧化结束后，停止加热，保持空气流量为100sccm～200sccm直到冷却到室温。
本发明具有以下有益效果：
1.检测方法简单，快速。通过检测纳米孔阵列阻塞电流下降的幅值，判断肿瘤标志物的浓度。此外，检测时间短，提高了检测效率。
2.检测精度高。纳米孔传感器检测精度达到单分子级别。因此，本发明的肿瘤标志物分子检测水平高，适用于癌症早期检测。
附图说明
图1为本发明氧化石墨烯过滤膜制造方法的工艺流程示意图。
图2为本发明中的铜箔基板示意图。
图3为本发明中设置系列微米孔阵列结构示意图。
图4为本发明中石墨烯表面与石墨烯内孔壁的结构示意图。
图5为图4中A处的局部放大示意图。
图6为本发明中氧化石墨烯铜箔基板表面与氧化石墨烯内孔壁的结构示意图。
图7为图6中B处的局部放大示意图。
图8为本发明中氧化石墨烯过滤膜的显微实物图。
图中附图标记说明：
1、铜箔基板，10、微米孔阵列，100、微米孔阵列内孔壁，2、石墨烯，20、石墨烯孔阵列，200、石墨烯孔内壁，3、氧化石墨烯，30、氧化石墨烯孔阵列，300、氧化石墨烯内孔壁。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式，本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用，本说明书中的各项细节也可以基于不同观点与应用，在没有背离本发明的精神下进行各种修饰或改变。
需要说明的是，本实施例中所提供的图示仅以示意方式说明本发明的基本构想，遂图式中仅显示与本发明中有关的组件而非按照实际实施时的组件数目、形状及尺寸绘制，其实际实施时各组件的型态、数量及比例可为一种随意的改变，且其组件布局型态也可能更为复杂。
如图1-8所示，本发明提供一种肿瘤标志物分子检测的方法，所述制作方法包括如下步骤：
S1：提供一铜箔基板1；
S2：通过激光加工或机械加工的方法在铜箔基板1上设置一系列微米孔阵列10；
S3：利用化学气相沉积法在铜箔基板1表面与微米孔阵列10的微米孔阵列内孔壁100上生长石墨烯2获得石墨烯表面与石墨烯内孔壁200；具体地，如图4、图5所示，所述石墨烯2包括石墨烯孔阵列20以及设置于石墨烯孔阵列20上的石墨烯孔内壁200。
S4：将铜箔基板1表面与石墨烯内孔壁200在空气中加热氧化获得氧化石墨烯铜箔基板表面与氧化石墨烯内孔壁300。具体地，如图6、图7所示，氧化石墨烯内孔壁300设置于氧化石墨烯孔阵列30上，并且氧化石墨烯内孔壁300与氧化石墨烯孔阵列30相互组成氧化石墨烯3.
铜箔基板1为双面已经抛光的铜箔，铜箔厚度为50μm～500μm。
一种实施例中，所述S2步骤中，通过激光加工的方法在铜箔基板1上制造出一系列微米孔阵列10，激光加工所用的激光器可以是纳秒激光器，皮秒激光器也可以是飞秒激光器。微米孔阵列10为50×50μm～100×100μm，微米孔阵列10间距为100μm～200μm，微米孔阵列10孔直径为50μm～100μm，微米孔阵列10所占据的区域面积为25mm2～400mm2，激光波长为532nm或775nm或1064nm或1550nm，纳秒激光器平均功率为15W～30W，皮秒激光器平均功率为10W～20W，飞秒激光器平均功率为0.5W～2W。激光器雕刻次数为15次～75次，激光器扫描速度为40～1000mm/s，激光频率为1Hz～100MHz。
一种实施例中，通过机械加工的方法在铜箔基板1上制造出一系列微米孔阵列10，机械加工采用钻床制造。微米孔阵列10为50×50～100×100，微米孔阵列10间距为100μm～200μm，微米孔阵列10孔直径为50μm～100μm，微米孔阵列10所占据的区域面积为25mm2～400mm2，钻床转速为200000r/min～300000r/min，进给速度为0.8米/分钟～1.2米/分钟，退刀速度为5米/分钟～7米/分钟。
一种实施例中，所述S3步骤中利用化学气相沉积法在铜箔基板1表面与内孔壁上生长石墨烯2得到石墨烯表面与石墨烯内孔壁200还包括如下步骤：
A1、将清洗后的铜箔衬底放入管式炉中央，通入氩气，将炉管内空气排出后；
A2、开始升温，升温速率10℃/min，保持氩气流量100sccm～200sccm。
A3、当炉管温度加热到800℃-1000℃时，通入氢气，氢气的流量为850sccm～950sccm，使衬底在氢气和氩气的气氛下退火20min～30min；
A4、退火结束后，通入甲烷，甲烷的流量为20sccm～25sccm，铜箔基板1表面和内孔壁上开始生长石墨烯，生长时间为5min～10min；
A5、生长结束后，关闭氢气和甲烷，将氩气流量调整为100sccm～200sccm直到冷却到室温。
一种实施例中，所述S4步骤中将石墨烯铜箔基板表面与石墨烯内孔壁200在空气中加热氧化得到氧化石墨烯铜箔基板表面与氧化石墨烯内孔壁300还包括如下步骤：
B1、将所述石墨烯铜箔基板表面放入管式炉中央，通入空气，空气流量为100sccm～200sccm；
B2、加热温度为300℃～600℃，保持温度在300℃～600℃的区间内5min～10min；
B3、氧化结束后，停止加热，保持空气流量为100sccm～200sccm直到冷却到室温。
本发明实施例的一种氧化石墨烯过滤膜制造方法。在具体实施时：首先提供一铜箔基板1。接着，通过激光加工的方法，在铜箔基板1上制造出一系列微米孔阵列10。接着，利用化学气相沉积法在铜箔基板1表面与内孔壁上生长石墨烯得到石墨烯表面与石墨烯内孔壁200。最后，将石墨烯铜箔基板1表面与石墨烯内孔壁200在空气中加热氧化得到氧化石墨烯铜箔基板1表面与氧化石墨烯内孔壁300。
该氧化石墨烯过滤膜的制备方法简单，易行，具有防止油堵塞能力，有极高的耐用性，可实现高效油水混合物分离。
综上所述，本发明提供的一种肿瘤标志物分子检测的方法，解决了前人使用纳米孔检测肿瘤标志物遇到的阻塞电流信号种类多，成分复杂，检测周期长等难题。且本发明提出的肿瘤标志物分子检测的方法易于集成，实现多通道并行检测，提高检测效率。此外，本发明操作简单，具有较好的扩展性和较广的使用范围。所以，本发明有效克服了现有技术中的种种缺点而具高度产业利用价值。
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。

Claims (10)

  1. 一种氧化石墨烯过滤膜制造方法，其特征在于，所述制作方法包括如下步骤：
    S1：提供一铜箔基板；
    S2：通过激光加工或机械加工的方法在铜箔基板上设置一系列微米孔阵列；
    S3：利用化学气相沉积法在铜箔基板表面与微米孔阵列的内孔壁上生长石墨烯获得石墨烯表面与石墨烯内孔壁；
    S4：将石墨烯铜箔基板表面与石墨烯内孔壁在空气中加热氧化获得氧化石墨烯铜箔基板表面与氧化石墨烯内孔壁。
  2. 根据权利要求1所述的氧化石墨烯过滤膜制造方法，其特征在于：所述S1步骤中，铜箔基板为双面抛光的铜箔基板，铜箔基板的厚度为50μm～500μm。
  3. 根据权利要求1所述的氧化石墨烯过滤膜制造方法，其特征在于：所述S2步骤中，激光加工时使用的激光器为纳秒激光器、皮秒激光器、飞秒激光器的其中一种。
  4. 根据权利要求3所述的氧化石墨烯过滤膜制造方法，其特征在于：所述激光器的激光波长为532nm或775nm或1064nm或1550nm。
  5. 根据权利要求3所述的氧化石墨烯过滤膜制造方法，其特征在于：所述纳秒激光器平均功率为15W～30W，皮秒激光器平均功率为10W～20W，飞秒激光器平均功率为0.5W～2W。
  6. 根据权利要求1或3所述的氧化石墨烯过滤膜制造方法，其特征在于：所述S2步骤中，激光加工时激光器的雕刻次数为15次～75次，激光器扫描速度为40～1000mm/s，激光频率为1Hz～100MHz。
  7. 根据权利要求1所述的氧化石墨烯过滤膜制造方法，其特征在于：所述S2步骤中，微米孔阵列为50×50～100×100，微米孔阵列间距为100μm～200μm，微米孔阵列孔直径为50μm～100μm，微米孔阵列所占据的区域面积为25mm2～400mm2。
  8. 根据权利要求1所述的氧化石墨烯过滤膜制造方法，其特征在于：所述S2步骤中，机械加工时采用钻床制造，所述钻床的进给速度为0.8米/分钟～1.2米/分钟，退刀速度为5米/分钟～7米/分钟。
  9. 根据权利要求1所述的氧化石墨烯过滤膜制造方法，其特征在于：所述S3步骤中还包括如下步骤：
    A1、将清洗后的铜箔衬底放入管式炉中央，通入氩气，将炉管内空气排出后；
    A2、开始升温，升温速率10℃/min，保持氩气流量100sccm～200sccm。
    A3、当炉管温度加热到800℃-1000℃时，通入氢气，氢气的流量为850sccm～950sccm，使衬底在氢气和氩气的气氛下退火20min～30min；
    A4、退火结束后，通入甲烷，甲烷的流量为20sccm～25sccm，铜箔基板表面和内孔壁上开始生长石墨烯，生长时间为5min～10min；
    A5、生长结束后，关闭氢气和甲烷，将氩气流量调整为100sccm～200sccm直到冷却到室温。
  10. 根据权利要求1所述的氧化石墨烯过滤膜制造方法，其特征在于：所述S4步骤中还包括如下步骤：
    B1、将所述石墨烯铜箔基板表面放入管式炉中央，通入空气，空气流量为100sccm～200sccm；
    B2、加热温度为300℃～600℃，保持温度在300℃～600℃的区间内5min～10min；
    B3、氧化结束后，停止加热，保持空气流量为100sccm～200sccm直到冷却到室温。
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