Method and device for processing microstructure arrays of polystyrene-graphene nanocomposites

Abstract

A device for processing microstructure arrays of polystyrene-graphene nanocomposites, including a laser generator, a vacuum chamber, an object stage, an ultraviolet filter and a gas flow control unit. The object stage is detachably fixed to a bottom of the vacuum chamber with a passage that can be opened or closed. The ultraviolet filter is provided in the vacuum chamber. A laser light emitted by the laser generator arrives at the object stage through the ultraviolet filter. The object stage is configured to place a sample to be processed. The gas flow control unit is communicated with the vacuum chamber and is configured to control the flow of the gas entering the vacuum chamber. The vacuum chamber is fixed on a three-axis precision positioning platform via a vacuum chamber clamp. The device disclosed herein aims to solve the existing difficulty in processing microstructure arrays of polystyrene-graphene nanocomposites.

Claims

1. A method for processing microstructure arrays of polystyrene-graphene nanocomposites, the method comprising: (1) mixing polystyrene microsphere powders and absolute ethanol at a ratio of 1:1 to obtain a mixture, and then stirring the mixture by a magnetic stirrer for 10 min so as to uniformly disperse the polystyrene microsphere powders in the absolute ethanol to obtain a polystyrene microsphere ethanol solution; (2) placing a silicon wafer with a size of 2 cm2 cm on a workbench of a spin coater, dropwise adding the polystyrene microsphere ethanol solution obtained in step (1) on the silicon wafer by a pipettor, and spin coating the solution, wherein low and high rotation speeds of the spin coater are respectively set to 400 rpm and 1000 rpm and a spin-coating time is 50 seconds so that the polystyrene microsphere ethanol solution is uniformly coated on the silicon wafer; (3) drying the silicon wafer coated with the polystyrene microsphere ethanol solution obtained in step (2) in a vacuum drying oven at a vacuum degree of 0.1 KPa at 60 C. for 1 h to obtain a sample, wherein an ethanol solution in the polystyrene microsphere ethanol solution volatilizes by said drying and polystyrene microspheres thereof form a compact monolayer structure; (4) placing the sample dried in step (3) on an object stage in a vacuum chamber of a laser processing system, and locking the vacuum chamber to prevent outside gases from entering the vacuum chamber, the vacuum chamber being arranged on a three-axis precision positioning platform; (5) controlling a movement of the three-axis precision positioning platform by a computer software control interface so as to position the sample below a laser generator, wherein an ultraviolet filter is located directly below the laser generator, and only ultraviolet light can pass through the ultraviolet filter, but light of other wavelengths is blocked, so that the sample is not damaged by the light of other wavelengths during laser processing; (6) switching on a vacuum pump to reduce a pressure of the vacuum chamber to 0.1 KPa, and keeping the vacuum pump operating for more than 1 min, so that an oxygen content in the vacuum chamber is minimized to avoid burning of the sample when the sample is heated during the processing; (7) introducing a shielding gas at a flow rate of 300 mL/min for 3 min while keeping the vacuum pump operating for more than 3 min, wherein the shielding gas is introduced to remove residual oxygen in the vacuum chamber so that free carbon and graphene generated during the processing are not oxidized and the sample does not burn when the sample is heated during the processing; (8) turning off the vacuum pump, continuing to introduce the shielding gas until the pressure of the vacuum chamber is 100 KPa, and then shutting off the shielding gas so that the vacuum chamber is filled with the shielding gas to further dilute the residual oxygen in the vacuum chamber, thereby forming a shielding gas atmosphere in the vacuum chamber with a certain pressure preventing movements and damage of the sample due to sudden influx of external air; (9) repeating steps (6)-(8) three times to remove a residual gas in the vacuum chamber, thereby preventing an adverse impact of the residual gas on the processing; (10) turning on the vacuum pump and introducing the shielding gas, controlling a flow rate of the shielding gas to be 300 mL/min and the pressure of the vacuum chamber at 0.1 KPa, and maintaining a stable shielding gas atmosphere in the vacuum chamber until the processing is finished; (11) performing the processing to form a pattern by using a laser drawing lines on the sample, wherein a spacing between the lines in the pattern is 0.03-0.05 mm; (12) during said processing, adjusting parameters of the laser generator and adjusting a location of a laser focus to make a distance between the position of the sample being processed and the laser focus appropriate, and continuing the processing according to a predesigned pattern, wherein the distance is set so as not to be so close that high energy damages occur in the sample and is set so as not to be so far as to fail to convert a surface of the polystyrene microspheres into graphene by said processing; and (13) controlling the three-axis precision positioning platform to a discharging point after said finishing of the processing and opening the vacuum chamber to take out a finished product, wherein a surface of the finished product has microstructure arrays of the graphene/polystyrene microsphere composites formed by said processing.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 schematically shows a processing flow of microstructure arrays of polystyrene-graphene nanocomposites according to an embodiment of the invention;

(2) FIG. 2 is a schematic view of a device for processing the microstructure arrays of the polystyrene-graphene nanocomposites according to an embodiment of the invention;

(3) FIG. 3 is a schematic view of a nanoscale pattern processed by a laser according to an embodiment of the invention;

(4) FIG. 4 schematically shows graphene converted from a surface of polystyrene according to an embodiment of the invention; and

(5) FIG. 5 is a simplified diagram of the device for processing the microstructure arrays of the polystyrene-graphene nanocomposites according to an embodiment of the invention.

(6) Reference numerals: 1laser generator; 2incident laser beam; 3ultraviolet filter; 4vacuum chamber; 5gas flow control unit; 6vacuum chamber clamp; 7vacuum gauge; 8silicon wafer coated with polystyrene microspheres; 9object stage; 10three-axis precision positioning platform; 11vacuum pump; 12polystyrene microspheres; and 14graphene/polystyrene microsphere composite.

DETAILED DESCRIPTION OF EMBODIMENTS

(7) The technical solutions of this invention will be further described below with reference to the accompanying drawings and specific embodiments.

(8) FIGS. 1-5 schematically show a device for processing microstructure arrays of polystyrene-graphene nanocomposites, including: a laser generator 1, a vacuum chamber 4, an object stage 9, an ultraviolet filter 3 and a gas flow control unit 5.

(9) The object stage is detachably fixed to a bottom of the vacuum chamber 4, and the vacuum chamber 4 has a passage that can be opened or closed.

(10) The ultraviolet filter 3 is provided in the vacuum chamber 4. A laser light emitted by the laser generator 1 arrives at the object stage through the ultraviolet filter 3. The object stage is configured to place a sample to be processed.

(11) The gas flow control unit 5 is communicated with the vacuum chamber 4 and is configured to control the flow of the gas entering the vacuum chamber 4.

(12) The vacuum chamber 4 is fixed on the three-axis precision positioning platform 10 via a vacuum chamber clamp 6.

(13) The polystyrene microspheres 12 are efficiently processed by the laser to realize surface reconstruction, so as to generate graphene. That's why the laser generator 1 and the vacuum chamber 4 are utilized in this embodiment. Moreover, in order to process various patterns on a surface of the sample and form various microstructure arrays, the vacuum chamber 4 is fixed on the three-axis precision positioning platform 10, so that the vacuum chamber 4 and an object fixed in the vacuum chamber 4 can be precisely positioned along the movement of the three-axis precision positioning platform 10.

(14) In this embodiment, the gas flow control unit 5 includes a gas flow meter and a flow controller.

(15) One end of the flow controller is connected to the vacuum chamber 4, and the other end of the flow controller is connected to a gas source. The gas flow meter is communicated to a pipeline between the flow controller and the gas source.

(16) A device for processing the microstructure arrays of the polystyrene-graphene nanocomposites of this invention further includes a vacuum gauge 7 and a vacuum pump 11. The vacuum gauge 7 is communicated with the vacuum chamber 4. The vacuum pump 11 is connected to an interface of the vacuum chamber 4 via a connecting pipe to discharge gases in the vacuum chamber.

(17) In this embodiment, the gas flow control unit is configured to accurately control the amount of the gas entering the vacuum chamber, and the vacuum pump 11 and the vacuum gauge 7 are configured to precisely control a vacuum degree of the vacuum chamber, thereby improving product quality and yield.

(18) In some embodiments, the connecting pipe is a vacuum bellows made of 304 stainless steel KF16.

(19) The vacuum bellows readily bends without deformation, benefits the efficiency in building a vacuum environment and has ease in the installation and dismantling.

(20) In addition, the gas flow meter has a maximum measurement range of 300 mL/min, and the vacuum pump can achieve the vacuum degree of the vacuum chamber 4 to 0.1 KPa or more.

(21) A method for processing the microstructure arrays of the polystyrene-graphene nanocomposites provided herein has the following steps.

(22) (1) Polystyrene microsphere powders and absolute ethanol were mixed at a ratio of 1:1 to obtain a mixture, and then the mixture was stirred by a magnetic stirrer for 10 min to prepare a polystyrene microsphere ethanol solution.

(23) (2) A silicon wafer with a size of 2 cm2 cm was placed on a workbench of a spin coater, and the polystyrene microsphere solution obtained in step (1) was dropwise added on the silicon wafer by a pipettor, where low and high rotation speeds were respectively set to 400 rpm and 1000 rpm, and a spin-coating time was 50 seconds.

(24) (3) The silicon wafer coated with the polystyrene microsphere ethanol solution obtained in step (2) was dried in a vacuum drying oven at a vacuum degree of 0.1 KPa at 60 C. for 1 h to obtain a sample.

(25) (4) The sample dried in step (3) was placed on an object stage in a vacuum chamber of a laser processing system and then the vacuum chamber was locked.

(26) (5) A movement of a three-axis precision positioning platform was controlled by a computer software control interface to enable a position to be processed of the sample to locate directly below a laser generator, where an ultraviolet filter was located directly below the laser generator.

(27) (6) A vacuum pump was switched on to reduce a vacuum degree of the vacuum chamber to 0.1 KPa, and the vacuum pump was kept operating for more than 1 min.

(28) (7) A shielding gas was introduced at a flow rate of 300 mL/min, and the vacuum pump was kept operating for more than 3 min; and the shielding gas was continuously introduced for 3 min, where the shielding gas was introduced to remove a residual oxygen and the like in the vacuum chamber, so that free carbon and graphene generated during processing are not be oxidized.

(29) (8) The vacuum pump was turned off, and the shielding gas was continuously introduced until the vacuum degree of the vacuum chamber was 100 KPa, after that, the shielding gas was shut off and the vacuum chamber 4 was filled with the shielding gas to further dilute the residual oxygen in the vacuum chamber 4.

(30) (9) The procedures of the gas removal and the shielding gas intake were repeated three times to remove a residual gas in the vacuum chamber, preventing an adverse impact of the residual gas on the processing.

(31) (10) The vacuum pump was turned on and the shielding gas was introduced, and a flow rate of the shielding gas was controlled to be 300 mL/min, simultaneously, the vacuum degree of the vacuum chamber was maintained at 0.1 KPa until the processing was finished.

(32) (11) A pattern was processed by using a laser to draw lines on the sample, where a spacing between the lines in the pattern was 0.03-0.05 mm.

(33) (12) The parameters of the laser generator 1 were set to have the number of markings of 1, a marking speed of 100 mm/s, the number of separators of 1, a power percentage of 40%, a calibration power of 1.8 W; and then a distance from a laser focus to a surface of silicon wafer coated with polystyrene microspheres 8 was adjusted to a range of 3-5 mm; the laser generator 1 was switched on for processing.

(34) (13) After the processing was completed, the three-axis precision positioning platform 10 arrived at a discharging point, and a finished product could be took out from the vacuum chamber 4, where microstructure arrays of the graphene/polystyrene microsphere composites were obtained on a surface of the finished product.

(35) The polystyrene microspheres were efficiently processed by the laser to realize surface reconstruction, so as to generate graphene. The graphene generated herein was firmly attached to surfaces of the polystyrene microspheres, thereby greatly improving the composites in the bonding strength of polystyrene and graphene. The various patterns could be quickly processed by the laser to form various microstructure arrays. This processing method has a simple and rapid operation with high processing efficiency, having great application prospects.

(36) The technical principles of the invention are described above with reference to specific embodiments. These descriptions are merely illustration of the principles and not intended to limit the scope of the invention. All other embodiments made by those skilled in the art based on the explanation disclosed herein without sparing any creative efforts, should fall within the scope of the invention.