CN109954987B - Method for processing nano blind holes on surface of single silk by femtosecond laser - Google Patents
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Abstract
The invention provides a method for processing a nano blind hole on the surface of single silk by using femtosecond laser, belonging to the field of femtosecond laser application. The method comprises the steps of firstly focusing a femtosecond laser pulse sequence on the surface of silk through a lens or a microscope objective, and preparing the independent single elliptic nano blind hole on the surface of the silk by regulating the number, energy flux and polarization direction of the femtosecond laser pulse incident on the surface of the silk. The method provided by the invention is based on the principle of near-field optical modulation, and realizes that a single nano blind hole far smaller than the diffraction limit is processed on the surface of silk. Compared with the traditional method, the method has the advantages of high processing precision, flexibility and convenience, and provides a feasible method for preparing the high-sensitivity sensor.
Description
Technical Field
The invention relates to a method for processing a nano blind hole on the surface of a single silk by using femtosecond laser, belonging to the technical field of femtosecond laser application.
Background
Silk is an ancient biomaterial, is applied to human beings for thousands of years together with natural materials such as cotton, animal fur and the like, and has important application in the textile industry due to the special structural form and excellent mechanical property. In addition, since fibroin has excellent biocompatibility and has good optical transmission performance in the visible light band of 400nm to 700nm, it is regarded as a photoelectric sensor for monitoring living bodies. For example, silk has been applied to dental bacteria sensors, edible fruit maturity monitoring sensors, and the like.
The implementation of the above device requires first the processing of silk. At present, the processing method of the fibroin device mainly obtains a pure fibroin solution by degumming, dialysis and other processes of natural silkworm cocoons, and further obtains a structure with corresponding functions by casting, spin coating, soft etching, nano imprinting, ink jet printing and the like. However, the silk has small size (about 10 μm) and strong mechanical property, so that the direct micro-nano processing of the natural silk is very difficult.
Disclosure of Invention
The invention aims to provide a method for processing a nano blind hole on the surface of a single silk by using femtosecond laser, aiming at the lack of a method for directly processing the nano blind hole on the single silk at present, the method utilizes the near-field modulation principle and the multiphoton nonlinear absorption effect in the action process of the femtosecond laser and silk fibroin, and generates an independent elliptical blind hole structure with the minor axis length less than 100nm by reasonably regulating and controlling the parameters of the femtosecond laser.
The invention provides a method for processing nano blind holes on the surface of silk by using femtosecond laser, which comprises the following steps:
(1) the ablation threshold of the silk to be processed is determined by an epitaxial method, and the process is as follows:
(1-1) the N energy fluxes are F0The femtosecond laser pulse is focused on the surface of silk through a lens according to the incident femtosecond laser wavelength lambda and the spot diameter DLQuality factor M2Calculating the focal length f of the lens to obtain the beam waist radius omega at the focal point0，
(1-2) measuring the radius r of the silk surface ablation circular spots obtained in the step (1-1);
(1-3) calculating silk ablation threshold F under N pulsesth，
(2) Focusing the femtosecond laser pulse sequence on the surface of the single silk through a lens or a microscope objective;
(3) the parameters of the femtosecond laser are controlled as follows: the number of femtosecond laser pulses is 300-800, the energy flux of the femtosecond laser is 1.05-1.15 times of the silk ablation threshold value under the corresponding number of pulses, the polarization direction of the femtosecond laser is axially vertical to the silk, and the independently existing nano oval blind holes are processed on the surface of the silk.
The method for processing the nano blind holes on the surface of the silk comprises the following specific steps:
(2-1) constructing a femtosecond laser processing system, which comprises a femtosecond laser, a half-wave plate, a neutral density attenuation plate, an electric control shutter, an illumination light source, a semi-transmitting and semi-reflecting mirror, a dichroic mirror, a lens or a microscope objective and a translation stage; the femtosecond laser emitted by the femtosecond laser forms a first light path through a half-wave plate, a neutral density attenuation plate and an electric control shutter in turn, the visible light emitted by the illumination light source forms a second light path through a half-mirror, a dichroic mirror, a lens or a microscope objective in turn and irradiates on the translation stage, and the charge coupling element and the imaging lens form a third light path; the first light path and the second light path are mutually vertical and are intersected at the dichroic mirror, and the second light path and the third light path are mutually vertical and are intersected at the semi-transmitting and semi-reflecting mirror;
(2-2) debugging the femtosecond laser processing system: starting a femtosecond laser device, generating femtosecond laser pulses, reducing the repetition frequency to 10Hz, setting an electric control shutter to be a single exposure mode, setting exposure time, enabling the number of the femtosecond laser pulses passing through the shutter to be 1, adjusting the height of a translation table, enabling the diameter of an ablation circular spot generated on the surface of silk by the single pulse under fixed energy to be minimum, completing debugging of a femtosecond laser processing system, and enabling the femtosecond laser to be accurately focused on the surface of the silk;
and (2-3) adjusting the polarization direction of the femtosecond laser pulse through a half-wave plate to ensure that the polarization direction of the femtosecond laser pulse irradiated on the surface of the silk is vertical to the axial direction of the silk.
(2-4) adjusting the neutral density attenuation sheet to enable the energy flux of the single pulse incident to the surface of the silk to be 1.05-1.15 times of the silk ablation threshold value under the corresponding number of pulses;
and (2-5) setting the repetition frequency of the femtosecond laser and the exposure time of the electrically controlled shutter, and enabling the number of femtosecond laser pulses passing through the shutter to be N to finish processing. The purpose of the invention is realized by the following technology:
the invention provides a method for processing nano blind holes on the surface of single silk by using femtosecond laser, which has the advantages that:
1. compared with the prior art in which silk protein aqueous solution is prepared and then casting, spin coating, soft etching, nano imprinting, ink jet printing and other methods are adopted, the femtosecond laser micro-nano manufacturing method is a non-contact mask-free processing method, has the characteristics of ultrafast, superstrong and high precision, and can be used for preparing a high-sensitivity protein sensor by directly utilizing natural silk.
2. The method provided by the invention has the advantages that when the energy flux of the single pulse incident to the surface of the silk is determined to be 1.05-1.15 times of the silk ablation threshold under the corresponding pulse number, the independent preparation of the elliptical blind hole with the minor axis length less than 100nm can be realized, and the processing precision is high.
3. The silk with the nano-pores processed on the surface, which is processed and prepared by the method, directly processes single natural silk by using femtosecond laser, and has the advantages of simple process, good flexibility and the like.
Drawings
Fig. 1 is a femtosecond laser processing system employed in an embodiment of the present invention.
In fig. 1, 1 is a femtosecond laser, 2 is a half-wave plate, 3 is a neutral density attenuation plate, 4 is an electrically controlled shutter, 5 is an illumination light source, 6 is a half-mirror, 7 is a dichroic mirror, 8 is a lens or a microscope objective, 9 is silk, 10 is a translation stage, 11 is a Charge Coupled Device (CCD), and 12 is an imaging lens.
Detailed Description
The invention provides a method for processing nano blind holes on the surface of silk by using femtosecond laser, which comprises the following steps:
(1) the ablation threshold of the silk to be processed is determined by an epitaxial method, and the process is as follows:
(1-1) the N energy fluxes are F0The femtosecond laser pulse is focused on the surface of silk through a lens according to the incident femtosecond laser wavelength lambda and the spot diameter DLQuality factor M2Calculating the focal length f of the lens to obtain the beam waist radius omega at the focal point0，
(1-2) measuring the radius r of the silk surface ablation circular spots obtained in the step (1-1);
(1-3) calculating silk ablation threshold F under N pulsesth，
(2) Focusing the femtosecond laser pulse sequence on the surface of the single silk through a lens or a microscope objective;
(3) the parameters of the femtosecond laser are controlled as follows: the number of femtosecond laser pulses is 300-800, the energy flux of the femtosecond laser is 1.05-1.15 times of the silk ablation threshold value under the corresponding number of pulses, the polarization direction of the femtosecond laser is axially vertical to the silk, and the independently existing nano oval blind holes are processed on the surface of the silk.
The invention provides a method for processing nano blind holes on the surface of silk, which specifically comprises the following steps:
(2-1) constructing a femtosecond laser processing system, wherein the structure of the femtosecond laser processing system is shown in figure 1, and the femtosecond laser processing system comprises a femtosecond laser 1, a half-wave plate 2, a neutral density attenuation plate 3, an electric control shutter 4, an illumination light source 5, a half-transmitting and half-reflecting mirror 6, a dichroic mirror 7, a lens or a microscope objective 8 and a translation stage 10; the femtosecond laser emitted by the femtosecond laser 1 forms a first optical path sequentially through a half-wave plate 2, a neutral density attenuation plate 3 and an electric control shutter 4, the visible light emitted by the illumination light source 5 sequentially passes through a half-wave mirror 6, a dichroic mirror 7, a lens or a microscope objective 8 to irradiate on a translation stage 10 to form a second optical path, and the charge coupling element 11 and the imaging lens 12 form a third optical path; the first light path and the second light path are mutually vertical and are intersected at the dichroic mirror 7, and the second light path and the third light path are mutually vertical and are intersected at the semi-transparent and semi-reflective mirror 6;
(2-2) debugging the femtosecond laser processing system: starting a femtosecond laser 1, generating femtosecond laser pulses, reducing the repetition frequency to 10Hz, setting an electric control shutter 4 to be a single exposure mode, setting exposure time, enabling the number of the femtosecond laser pulses passing through the shutter to be 1, adjusting the height of a translation table 10, enabling the diameter of an ablation circular spot generated on the surface of silk by the single pulse under fixed energy to be minimum, completing debugging of a femtosecond laser processing system, and then accurately focusing the femtosecond laser on the surface of the silk 9;
(2-3) adjusting the polarization direction of the femtosecond laser pulse through the half-wave plate 2 to ensure that the polarization direction of the femtosecond laser pulse irradiated on the surface of the silk 9 is vertical to the axial direction of the silk.
(2-4) adjusting the neutral density attenuation sheet 3 to enable the energy flux of the single pulse incident to the surface of the silk 9 to be 1.05-1.15 times of the silk ablation threshold value under the corresponding pulse number;
(2-5) setting the repetition frequency of the femtosecond laser and the exposure time of the electric control shutter 4, and enabling the number of femtosecond laser pulses passing through the shutter to be N to finish the processing.
The invention will be further described with reference to the following figures and examples:
the present invention is implemented in a femtosecond laser processing system as shown in fig. 1, which includes two parts, a processing subsystem and an observation subsystem. The processing subsystem comprises a femtosecond laser 1, a half-wave plate 2, a neutral density attenuation plate 3, an electric control shutter 4, a dichroic mirror 7, a lens or a microscope objective 8 and a translation stage 10. The observation subsystem comprises an illumination light source 5, a half-mirror 6, a lens or a microscope objective 8, a Charge Coupled Device (CCD)11 and an imaging lens 12.
In the processing subsystem, a femtosecond laser pulse sequence output by the femtosecond laser sequentially penetrates through the half-wave plate 2 to adjust the polarization direction, the neutral density attenuation plate 3 to adjust the energy, then is reflected by the dichroic mirror 7, and is focused on the surface of silk 9 through the lens or the microscope objective lens 8. An electric control shutter 4 is arranged between the neutral density attenuation sheet 3 and the dichroic mirror 7 and used for accurately regulating and controlling the number of pulses irradiated to the surface of the silk 9. The silk 9 is fixed on a translation table 10 and used for accurately controlling the position of the processed nano blind hole. The parameters of the femtosecond laser 1 in the example are: the center wavelength of the femtosecond laser is 800nm, the repetition frequency is 1 Hz-1 kHz, and the pulse width is 35 fs.
In the observation subsystem, the illumination light emitted by the illumination light source 5 is transmitted by the half-transmitting mirror 6 and the dichroic mirror 7 and then focused on the surface of silk 9 by a lens or a microscope objective 8 for illuminating the processing area. The real-time image of the processing area is amplified by a lens or a microscope objective 8, then penetrates through a dichroic mirror 7, and is reflected by a half-transmitting and half-reflecting mirror 6 to enter an imaging lens 12. The imaging lens 12 is used to image the magnified real-time image onto a Charge Coupled Device (CCD)11 and transmit to a display for viewing the process.
The invention discloses a method for processing nano blind holes on the surface of silk by using femtosecond laser, which comprises the following steps:
step one, focusing the femtosecond laser pulse sequence on the surface of the silk through a lens or a microscope objective. The first step specifically comprises the following steps:
step 1.1), the femtosecond laser 1 is started to generate femtosecond laser pulses. The polarization direction is adjusted through the half-wave plate 2, so that the polarization direction irradiated to the surface of the silk 9 is vertical to the axial direction of the silk.
And step 1.2), adjusting the neutral density attenuation sheet 3 to enable the energy flux of the single pulse incident to the surface of the silk 9 to be 1.05-1.15 times of the silk ablation threshold value under the corresponding pulse number.
And step two, the processing of the nano-holes is realized by regulating and controlling femtosecond laser parameters and utilizing the local near-field light modulation principle. The second step specifically comprises:
and 2.1) selecting a lens or a microscope objective 8, fixing the silk 9 on a translation stage 10, and adjusting the relative positions of the working surfaces of the lens or the microscope objective 8 and the translation stage 10 to focus the femtosecond laser passing through the lens or the microscope objective 8 on the designated processing position on the surface of the silk 9.
And 2.2) controlling the number N of pulse sequences irradiated on the silk 9 by coordinately regulating and controlling the femtosecond laser repetition frequency and the single exposure time of the electric control shutter 4 to finish the processing.
The nano holes formed on the surface of the silk by the method are independent elliptical blind holes with the minor axis length less than 100 nm.
The following are examples of the process of the invention:
example 1:
the neutral density attenuation sheet 3 is adjusted to set the single pulse energy to be 48.7nJ (4.34J/cm)2，1.13Fth) The method comprises the steps of arranging a lens or a microscope objective 8 as a 50 × long working distance flat field semi-apochromatic lens (NA is 0.5), controlling the number N of pulse sequences irradiated on silk 9 to be 350 through an electric control shutter 4, and preparing an independently-existing elliptic blind hole with the minor axis length of 74nm on the silk 9.
Example 2:
the neutral density attenuation sheet 3 was adjusted to set the single pulse energy at 43.1nJ (3.84J/cm)2，1.07Fth) The method comprises the steps of arranging a lens or a microscope objective 8 as a 50 × long working distance flat field semi-apochromatic lens (NA is 0.5), controlling the number N of pulse sequences irradiated on silk 9 to be 450 through an electric control shutter 4, and preparing an independently-existing elliptic blind hole with the minor axis length of 22nm on the silk 9.
Example 3:
the neutral density attenuation sheet 3 is adjusted, and the single pulse energy is set to be 40.1nJ (3.58J/cm)2，1.06Fth) The method comprises the steps of arranging a lens or a microscope objective 8 as a 50 × long working distance flat field semi-apochromatic lens (NA is 0.5), controlling the number N of pulse sequences irradiated on silk 9 to be 650 through an electric control shutter 4, and preparing an independently-existing elliptic blind hole with the minor axis length of 66nm on the silk 9.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (1)
1. A method for processing nano blind holes on the surface of single silk by femtosecond laser is characterized in that: the method comprises the following steps:
(1) the ablation threshold of the silk to be processed is determined by an epitaxial method, and the process is as follows:
(1-1) the N energy fluxes are F0The femtosecond laser pulse is focused on the surface of silk through a lens according to the incident femtosecond laser wavelength lambda and the spot diameter DLQuality factor M2Calculating the focal length f of the lens to obtain the beam waist radius omega at the focal point0，
(1-2) measuring the radius r of the silk surface ablation circular spots obtained in the step (1-1);
(1-3) calculating silk ablation threshold F under N pulsesth，
(2) Constructing a femtosecond laser processing system, which comprises a femtosecond laser, a half-wave plate, a neutral density attenuation plate, an electric control shutter, an illumination light source, a semi-transparent and semi-reflective mirror, a dichroic mirror, a lens or a microscope objective and a translation stage; the femtosecond laser emitted by the femtosecond laser forms a first light path through a half-wave plate, a neutral density attenuation plate and an electric control shutter in turn, the visible light emitted by the illumination light source forms a second light path through a half-mirror, a dichroic mirror, a lens or a microscope objective in turn and irradiates on the translation stage, and the charge coupling element and the imaging lens form a third light path; the first light path and the second light path are mutually vertical and are intersected at the dichroic mirror, and the second light path and the third light path are mutually vertical and are intersected at the semi-transmitting and semi-reflecting mirror;
(3) debugging the femtosecond laser processing system: starting a femtosecond laser device, generating femtosecond laser pulses, reducing the repetition frequency to 10Hz, setting an electric control shutter to be a single exposure mode, setting exposure time, enabling the number of the femtosecond laser pulses passing through the shutter to be 1, adjusting the height of a translation table, enabling the diameter of an ablation circular spot generated on the surface of silk by a single pulse under fixed energy to be minimum, completing debugging of a femtosecond laser processing system, and focusing the femtosecond laser pulse sequence on the surface of the single silk through a lens or a microscope objective;
(4) adjust femtosecond laser pulse's polarization direction through half-wave plate, make the femtosecond laser pulse polarization direction of irradiation to the silk surface perpendicular with silk axis direction, through adjusting neutral density attenuator, make the monopulse energy flux of inciding the silk surface for corresponding under the pulse number between the 1.05 ~ 1.15 times of silk ablation threshold value, the parameter of control femtosecond laser is: the number of femtosecond laser pulses is 300-800, the polarization direction of the femtosecond laser is vertical to the axial direction of the silk, the repetition frequency of the femtosecond laser and the exposure time of an electric control shutter are set, the number of the femtosecond laser pulses passing through the shutter is N, and the independent nano elliptical hole is processed on the surface of the silk.
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| CN1063805C (en) * | 1997-12-16 | 2001-03-28 | 柳启瑞 | Method for making multi-microporous hollow fibre by using laser processing technology |
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