CN105060239A - Preparation method of super-hydrophobic porous silicon - Google Patents
Preparation method of super-hydrophobic porous silicon Download PDFInfo
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Abstract
The invention discloses a preparation method of super-hydrophobic porous silicon. The method comprises the following steps: radiating and ablating a micro-nano structure on a monocrystalline silicon surface with ultra-short pulse laser; and corroding the surface with a mixed solution prepared from hydrofluoric acid, nitric acid and distilled water in a certain ratio to obtain a porous silicon surface. The porous silicon surface prepared with the method has excellent super-hydrophobic characteristic.
Description
Technical field
The present invention relates to super hydrophobic porous silicon, particularly utilize the micro-nano structure of induced by ultrashort pulse laser silicon face.
Technical background
The wettability of material surface causes people huge and interest widely in nearest decades, because its huge applications in daily life and industrial production is worth, especially has the surfacing of super-drainage structure.First, we have found super-hydrophobicity on occurring in nature lotus leaf, and this ultra-hydrophobicity has automatic cleaning action, leaf surfaces can be kept not by contamination by dust, keep it photosyntheticly to carry out smoothly, meanwhile, we are also referred to as this phenomenon " lotus leaf effect ".Due to the plurality of advantages of this super-hydrophobicity, people have attempted multiple method and have prepared this surfacing with ultra-hydrophobicity, such as, chemical vapor infiltration, sol-gal process, from spin-coating method, chemical synthesis, beam-plasma method, method of electrostatic spinning etc.In recent years, in retrofit field, ultra-short pulse laser is widely used.This new technology has good spatial selectivity on micro-meter scale, is a kind of technology had great advantage at retrofit field tool.Utilize this technology to prepare the surfacing with different wetting characteristic to have huge application background.
Summary of the invention
The invention provides a kind of method preparing super hydrophobic porous silicon structure.Do not need to utilize low-surface energy substance to process material surface, only utilize the method for ultra-short pulse laser and the super hydrophobic porous silicon structure of mixed acid corrosion preparation.
A preparation method for super hydrophobic porous silicon, its feature is, step is as follows:
1) ultrasonic process: the acetone solvent that the monocrystalline silicon piece content of acetone being first (111) the crystal orientation of twin polishing is greater than 99.5% carries out ultrasonic process five minutes, takes out afterwards and dries;
2) pulse laser scanning: through the monocrystalline silicon piece of ultrasonic process, be placed in computer-controlled three-dimensional mobile platform, the pulse width of ultra-short pulse laser used is that 10 femtoseconds are to 10 psecs.Utilize focusing system that the ultra-short pulse laser with constant power is focused on monocrystalline silicon surface, and three-dimensional mobile platform carries out laser scanning with fixing rate travel to monocrystalline silicon surface at every turn, obtain a series of being parallel to each other, and set adjacent between there is the micron trenches of same intervals, wherein, the mean power of ultra-short pulse laser in single sample preparation process, the interval of sweep speed and adjacent scanning lines remains unchanged respectively, in different Sample Preparation Procedure, the mean power of described laser, the setting range at the interval between sweep speed and adjacent scanning lines is respectively: 5mW to 200mW, 1mm/s to 20mm/s, 5 μm to 30 μm,
3) mixed acid process: nitric acid and hydrofluoric acid concentration is before mixing respectively 68% and 40%, and before mixing, the volume ratio of nitric acid and hydrofluoric acid is 2 ~ 3, the volume ratio of distilled water and hydrofluoric acid is 3 ~ 6, after mixing, in fume hood, the monocrystalline silicon piece handled well with ultra-short pulse laser is placed in this mixed acid solution, the time of corrosion is 60 ~ 120 minutes;
4) from mixed acid, take out the absolute ethyl alcohol that sample with ethanol content is greater than 99.7% rinse well, dry, contact angle measurement is utilized to measure itself and the contact angle distilling the globule, select the sample that wherein contact angle is greater than 150 °, recycling SEM picks out the porous monocrystalline silicon chip that surface has micro-nano honeycomb shape from the sample of about 150 ° of contact angle.
The porous silica material of prepared by the present invention have ultra-hydrophobicity possesses following advantage:
Utilize focusing system that ultra-short pulse laser is focused on material surface, focal spot radius is several microns, can realize the spatial selectivity of ultra-short pulse laser processing at micro-meter scale, and fuel factor is negligible, produces very little fire damage around material effects.
Sample after this ultrashort pulse irradiation, after mixed acid corrosion, obtain Porous Silicon structures, and this monocrystalline silicon surface with Porous Silicon structures has very strong hydrophobic property on its surface.
Detailed description of the invention
Below by embodiment, the present invention is described in further detail, but should not be construed as the restriction of scope.
Embodiment 1: the preparation method of super hydrophobic porous silicon, comprises the following steps:
1) twin polishing, crystal orientation is (111), and diameter is 50.4-51.2mm, thickness is the monocrystalline silicon piece that the silicon chip of 325-375 μm cuts into the blockage of 1cmX1cm, then utilizes acetone solvent to clean five minutes in ultrasonic pond, the impurity on removing surface, take out, dry;
2) monocrystalline silicon piece through processing in ultrasonic pond, be fixed in three-dimensional mobile platform, then, be 800nm by wavelength, repetition rate is 1kHz, pulse width is that the femtosecond pulse of 120fs focuses on described monocrystalline silicon sheet surface through microcobjective, power setting is 5mW, and sweep speed is 1mm/s, and focusing objective len multiplication factor is 5, be spaced apart 5 μm between adjacent scanning striped, obtain the groove structure of a series of micro-meter scale be parallel to each other;
3) hydrofluoric acid solution that 3mL concentration is 40% is got, 9mL concentration is 68% salpeter solution, 18mL distilled water, is blended in a small container and prepares mixed acid solution, then be placed on by the monocrystalline silicon piece through femtosecond pulse process and wherein corrode, the time of corrosion is decided to be 60 minutes;
4) from mixed acid, described monocrystalline silicon piece is taken out with tweezers, and rinse with absolute ethyl alcohol, dry, utilize contact angle measurement measure described in monocrystalline silicon piece and the static contact angle of water be 143 °, achieve the sub-super-hydrophobicity on surface, and through scanning electron microscopy measurement, select to obtain the porous silicon wafer that its surface defines similar cellular loose structure.
Embodiment 2: the preparation method of super hydrophobic porous silicon, comprises the following steps:
1) twin polishing, crystal orientation is (111), and diameter is 50.4-51.2mm, thickness is the blockage that the silicon chip of 325-375 μm cuts into 2cmx2cm, then utilizes acetone solvent to clean five minutes in ultrasonic pond, the impurity on removing surface, take out, dry;
2) monocrystalline silicon piece through processing in ultrasonic pond, be fixed in three-dimensional mobile platform, then, be 800nm by wavelength, repetition rate is 200kHz, pulse width is that the femtosecond pulse of 120fs focuses on described monocrystalline silicon sheet surface through microcobjective, power setting is 5mW, and sweep speed is 10mm/s, and focusing objective len multiplication factor is 10, be spaced apart 5 μm between adjacent scanning striped, obtain a series of groove structure be parallel to each other;
3) hydrofluoric acid solution that 2mL concentration is 40% is got, 5mL concentration is 68% salpeter solution, 10mL distilled water, is placed in a small container and prepares mixed acid solution, then be placed in mixed acid solution by the monocrystalline silicon piece through pulse laser processing and corrode, the time of corrosion is decided to be 60 minutes;
4) through step 3) mixed acid corrosion monocrystalline silicon piece, take out with tweezers, and rinse with absolute ethyl alcohol, dry, the static contact angle utilizing contact angle measurement to measure itself and water is 150 °, achieve the super-hydrophobicity on surface, and through scanning electron microscopy measurement, obtain its surface and define similar cellular loose structure.
Embodiment 3: the preparation method of super hydrophobic porous silicon, comprises the following steps:
1) twin polishing, crystal orientation is (111), and diameter is 50.4-51.2mm, thickness is the blockage that the silicon chip of 325-375 μm cuts into 3cmx3cm, then utilizes acetone solvent to clean five minutes in ultrasonic pond, the impurity on removing surface, take out, dry;
2) monocrystalline silicon piece through processing in ultrasonic pond, be fixed in three-dimensional mobile platform, then, wavelength is 1064nm, and repetition rate is 500kHz, pulse width is that the picosecond pulse laser of 10ps focuses on monocrystalline silicon surface through field lens, power setting is 5mW, and by vibration mirror scanning, sweep speed is 20mm/s, be spaced apart 5 μm between adjacent scanning, obtain a series of groove structure be parallel to each other;
3) prepare mixed acid solution, get the hydrofluoric acid solution that 3mL concentration is 40%, 9mL concentration is 68% salpeter solution, 18mL distilled water, be blended in a small container, be then placed on through the monocrystalline silicon piece of pulse laser processing and wherein corrode, the time of corrosion is decided to be 60 minutes;
4) through step 3) mixed acid corrosion monocrystalline silicon piece, take out with tweezers, and rinse with absolute ethyl alcohol, dry, the static contact angle utilizing contact angle measurement to measure itself and water is 155 °, achieve the ultra-hydrophobicity on surface, and through scanning electron microscopy measurement, obtain its surface and define similar cellular loose structure.
Embodiment 4: the preparation method of super hydrophobic porous silicon, comprises the following steps:
1) twin polishing, crystal orientation is (111), and diameter is 50.4-51.2mm, thickness is 325-375 μm, silicon chip cut into the blockage of 3cmx3cm, then utilize acetone solvent to clean five minutes in ultrasonic pond, the impurity on removing surface, takes out, dries;
2) monocrystalline silicon piece through processing in ultrasonic pond, be fixed in three-dimensional mobile platform, then, wavelength is 800nm, and repetition rate is 1kHz, pulse width is that the femtosecond pulse regular menstruation during early pregnancy microcobjective of 120fs focuses on monocrystalline silicon surface, power setting is 100mW, and sweep speed is 20mm/s, and focusing objective len multiplication factor is 5, be spaced apart 5 μm between adjacent scanning, obtain a series of groove structure be parallel to each other;
3) prepare mixed acid solution, get the hydrofluoric acid solution that 3mL concentration is 40%, 9mL concentration is 68% salpeter solution, 18mL distilled water, be blended in a small container, be then placed on through the monocrystalline silicon piece of pulse laser processing and wherein corrode, the time of corrosion is decided to be 100 minutes;
4) through step 3) mixed acid corrosion monocrystalline silicon piece, take out with tweezers, and rinse with absolute ethyl alcohol, dry, the static contact angle utilizing contact angle measurement to measure itself and water is 151 °, achieve the ultra-hydrophobicity on surface, and through scanning electron microscopy measurement, obtain its surface and define similar cellular loose structure.
Embodiment 5: the preparation method of super hydrophobic porous silicon, comprises the following steps:
1) twin polishing, crystal orientation is (111), and diameter is 50.4-51.2mm, thickness is 325-375 μm, silicon chip cut into the blockage of 3cmx3cm, then utilize acetone solvent to clean five minutes in ultrasonic pond, the impurity on removing surface, takes out, dries;
2) monocrystalline silicon piece through processing in ultrasonic pond, be fixed in three-dimensional mobile platform, then, wavelength is 800nm, and repetition rate is 200kHz, pulse width is that the femtosecond pulse of 120fs focuses on monocrystalline silicon surface through microcobjective, power setting is 200mW, and sweep speed is 20mm/s, and focusing objective len multiplication factor is 5, be spaced apart 5 μm between adjacent scanning, obtain a series of groove structure be parallel to each other;
3) prepare mixed acid solution, get the hydrofluoric acid solution that 3mL concentration is 40%, 9mL concentration is 68% salpeter solution, 18mL distilled water, be blended in a small container, be then placed on through the monocrystalline silicon piece of pulse laser processing and wherein corrode, the time of corrosion is decided to be 120 minutes;
4) through step 3) mixed acid corrosion monocrystalline silicon piece, take out with tweezers, and rinse with absolute ethyl alcohol, dry, the static contact angle utilizing contact angle measurement to measure itself and water is 152 °, achieve the ultra-hydrophobicity on surface, and through scanning electron microscopy measurement, obtain its surface and define similar cellular loose structure.
Embodiment 6: the preparation method of super hydrophobic porous silicon, comprises the following steps:
1) twin polishing, crystal orientation is (111), and diameter is 50.4-51.2mm, thickness is 325-375 μm, silicon chip cut into the blockage of 3cmx3cm, then utilize acetone solvent to clean five minutes in ultrasonic pond, the impurity on removing surface, takes out, dries;
2) monocrystalline silicon piece through processing in ultrasonic pond, be fixed in three-dimensional mobile platform, then, wavelength is 1064nm, and repetition rate is 500kHz, pulse width is that the picosecond pulse laser of 10ps focuses on monocrystalline silicon surface through field lens, power setting is 200mW, and by vibration mirror scanning, sweep speed is 20mm/s, be spaced apart 5 μm between adjacent scanning, obtain a series of groove structure be parallel to each other;
3) prepare mixed acid solution, get the hydrofluoric acid solution that 3mL concentration is 40%, 9mL concentration is 68% salpeter solution, 18mL distilled water, be blended in a small container, be then placed on through the monocrystalline silicon piece of pulse laser processing and wherein corrode, the time of corrosion is decided to be 120 minutes;
4) through step 3) mixed acid corrosion monocrystalline silicon piece, take out with tweezers, and rinse with absolute ethyl alcohol, dry, the static contact angle utilizing contact angle measurement to measure itself and water is 153 °, achieve the ultra-hydrophobicity on surface, and through scanning electron microscopy measurement, obtain its surface and define similar cellular loose structure.
Embodiment 7: the preparation method of super hydrophobic porous silicon, comprises the following steps:
1) twin polishing, crystal orientation is (111), and diameter is 50.4-51.2mm, thickness is 325-375 μm, silicon chip cut into the blockage of 3cmx3cm, then utilize acetone solvent to clean five minutes in ultrasonic pond, the impurity on removing surface, takes out, dries;
2) monocrystalline silicon piece through processing in ultrasonic pond, be fixed in three-dimensional mobile platform, then, wavelength is 800nm, repetition rate 1kHz, pulse width is that the femtosecond pulse of 120fs focuses on monocrystalline silicon surface through microcobjective, power setting is 200mW, and sweep speed is 20mm/s, and focusing objective len multiplication factor is 5, be spaced apart 10 μm between adjacent scanning, obtain a series of groove structure be parallel to each other;
3) prepare mixed acid solution, get the hydrofluoric acid solution that 3mL concentration is 40%, 9mL concentration is 68% salpeter solution, 18mL distilled water, be blended in a small container, be then placed on through the monocrystalline silicon piece of pulse laser processing and wherein corrode, the time of corrosion is decided to be 120 minutes;
4) through step 3) mixed acid corrosion monocrystalline silicon piece, take out with tweezers, and rinse with absolute ethyl alcohol, dry, the static contact angle utilizing contact angle measurement to measure itself and water is 156 °, achieve the ultra-hydrophobicity on surface, and through scanning electron microscopy measurement, obtain its surface and define similar cellular loose structure.
Embodiment 8: the preparation method of super hydrophobic porous silicon, comprises the following steps:
1) twin polishing, crystal orientation is (111), and diameter is 50.4-51.2mm, thickness is 325-375 μm, silicon chip cut into the blockage of 3cmx3cm, then utilize acetone solvent to clean five minutes in ultrasonic pond, the impurity on removing surface, takes out, dries;
2) monocrystalline silicon piece through processing in ultrasonic pond, be fixed in three-dimensional mobile platform, then, wavelength is 800nm, and repetition rate is 200kHz, pulse width is that the femtosecond pulse of 120fs focuses on monocrystalline silicon surface through microcobjective, power setting is 200mW, and sweep speed is 20mm/s, and focusing objective len multiplication factor is 5, be spaced apart 30 μm between adjacent scanning, obtain a series of groove structure be parallel to each other;
3) prepare mixed acid solution, get the hydrofluoric acid solution that 3mL concentration is 40%, 9mL concentration is 68% salpeter solution, 18mL distilled water, be blended in a small container, be then placed on through the monocrystalline silicon piece of pulse laser processing and wherein corrode, the time of corrosion is decided to be 120 minutes;
4) through step 3) mixed acid corrosion monocrystalline silicon piece, take out with tweezers, and rinse with absolute ethyl alcohol, dry, the static contact angle utilizing contact angle measurement to measure itself and water is 151 °, achieve the ultra-hydrophobicity on surface, and through scanning electron microscopy measurement, obtain its surface and define similar cellular loose structure.
Embodiment 9: the preparation method of super hydrophobic porous silicon, comprises the following steps:
1) twin polishing, crystal orientation is (111), and diameter is 50.4-51.2mm, thickness is 325-375 μm, silicon chip cut into the blockage of 3cmx3cm, then utilize acetone solvent to clean five minutes in ultrasonic pond, the impurity on removing surface, takes out, dries;
2) monocrystalline silicon piece through processing in ultrasonic pond, be fixed in three-dimensional mobile platform, then, wavelength is 1064nm, and repetition rate is 500kHz, pulse width is that the picosecond pulse laser of 10ps focuses on monocrystalline silicon surface through field lens, power setting is 200mW, and by vibration mirror scanning, sweep speed is 20mm/s, be spaced apart 30 μm between adjacent scanning, obtain a series of groove structure be parallel to each other.
3) prepare mixed acid solution, get the hydrofluoric acid solution that 3mL concentration is 40%, 9mL concentration is 68% salpeter solution, 18mL distilled water, be blended in a small container, be then placed on through the monocrystalline silicon piece of pulse laser processing and wherein corrode, the time of corrosion is decided to be 120 minutes.
4) through step 3) mixed acid corrosion monocrystalline silicon piece, take out with tweezers, and rinse with absolute ethyl alcohol, dry, the static contact angle utilizing contact angle measurement to measure itself and water is 153 °, achieve the ultra-hydrophobicity on surface, and through scanning electron microscopy measurement, obtain its surface and define similar cellular loose structure.
Claims (1)
1. a preparation method for super hydrophobic porous silicon, is characterized in that, step is as follows:
1) ultrasonic process: the acetone solvent that the monocrystalline silicon piece content of acetone being first (111) the crystal orientation of twin polishing is greater than 99.5% carries out ultrasonic process five minutes, takes out afterwards and dries;
2) pulse laser scanning: through the monocrystalline silicon piece of ultrasonic process, be placed in computer-controlled three-dimensional mobile platform, the pulse width of ultra-short pulse laser used is that 10 femtoseconds are to 10 psecs.Utilize focusing system that the ultra-short pulse laser with constant power is focused on monocrystalline silicon surface, and three-dimensional mobile platform carries out laser scanning with fixing rate travel to monocrystalline silicon surface at every turn, obtain a series of being parallel to each other, and set adjacent between there is the micron trenches of same intervals, wherein, the mean power of ultra-short pulse laser in single sample preparation process, the interval of sweep speed and adjacent scanning lines remains unchanged respectively, in different Sample Preparation Procedure, the mean power of described laser, the setting range at the interval between sweep speed and adjacent scanning lines is respectively: 5mW to 200mW, 1mm/s to 20mm/s, 5 μm to 30 μm,
3) mixed acid process: nitric acid and hydrofluoric acid concentration is before mixing respectively 68% and 40%, and before mixing, the volume ratio of nitric acid and hydrofluoric acid is 2 ~ 3, the volume ratio of distilled water and hydrofluoric acid is 3 ~ 6, after mixing, in fume hood, the monocrystalline silicon piece handled well with ultra-short pulse laser is placed in this mixed acid solution, the time of corrosion is 60 ~ 120 minutes;
4) from mixed acid, take out the absolute ethyl alcohol that sample with ethanol content is greater than 99.7% rinse well, dry, contact angle measurement is utilized to measure itself and the contact angle distilling the globule, select the sample that wherein contact angle is greater than 150 °, recycling SEM picks out the porous monocrystalline silicon chip that surface has micro-nano honeycomb shape from the sample of about 150 ° of contact angle.
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| CN105609572A (en) * | 2016-03-22 | 2016-05-25 | 中利腾晖光伏科技有限公司 | Texturing method for monocrystalline cell, monocrystalline cell and monocrystalline photovoltaic module |
| CN107021449A (en) * | 2016-04-19 | 2017-08-08 | 北京航空航天大学 | Prepare the preparation method and applications at ordered micro-configuration and controllable chemical composition interface |
| CN108314993A (en) * | 2017-12-28 | 2018-07-24 | 肇庆市华师大光电产业研究院 | A kind of preparation method of large area flexible hydrophobic porous silicon fiml |
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