CN110255492A - A kind of super-hydrophobic super hydrophilic area distribution surface of silicon base and its preparation method and application - Google Patents
A kind of super-hydrophobic super hydrophilic area distribution surface of silicon base and its preparation method and application Download PDFInfo
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Abstract
This disclosure relates to which a kind of super-hydrophobic super hydrophilic area distribution surface of silicon base and its preparation method and application, method includes the following steps: the surface to silicon base laser machines, obtains the first surface with micrometer-submicrometer grade coarse structure；Hydroxylating processing is carried out to first surface, obtains second surface；Under conditions of condensation reaction, so that second surface and organic solution is carried out condensation reaction, obtain third surface；Ultraviolet irradiation processing in constituency is carried out to third surface, obtains the super-hydrophobic super hydrophilic area distribution surface of silicon base.The silicon substrate surface that disclosed method is prepared has excellent super hydrophilic/super-hydrophobic area distribution characteristic.
Description
Technical field
This disclosure relates to material surface processing technique field, and in particular, to a kind of super-hydrophobic super hydrophilic region of silicon base
It is distributed surface and its preparation method and application.
Background technique
Super hydrophobic surface refers to that water droplet is greater than 150 degree of the surface of solids in surface of solids contact angle, its own has anti-
The excellent properties such as dirty corrosion resistant, fluid drag-reduction, automatically cleaning.Ultra-hydrophilic surface refers to that water droplet drop can be in the short period in the surface of solids
Interior complete drawout makes contact angle be equal or close to 0 °, has in various fields such as antifouling antifog, water-oil separatings very wide
The two advantage concentration can be widely applied to the fields such as construction material, biological medicine, communications and transportation by wealthy application prospect.
Silicon is widely used in daily life, changes its surface microstructure and surface free energy for different substrates
Method is all not quite similar, and the surface prepared often only has a kind of super-hydrophobic or super hydrophilic surface characteristic, in the prior art
Also lack a kind of method for preparing the super-hydrophobic super hydrophilic area distribution surface of silicon base.
Summary of the invention
The purpose of the disclosure is to overcome the prior art that can not prepare while having the silicon of super-hydrophobicity and Superhydrophilic
The problem of substrate, provides a kind of super-hydrophobic super hydrophilic area distribution surface of silicon base and its preparation method and application.
To achieve the goals above, disclosure first aspect, which provides, a kind of prepares the super-hydrophobic super hydrophilic area distribution of silicon base
The method on surface, method includes the following steps:
(1) surface of silicon base is laser machined, obtains first table with micrometer-submicrometer grade coarse structure
Face；
(2) hydroxylating processing is carried out to the first surface, obtains second surface；
(3) under conditions of condensation reaction, so that the second surface and organic solution is carried out condensation reaction, obtain third table
Face；
(4) ultraviolet irradiation processing in constituency is carried out to the third surface, obtains the super-hydrophobic super hydrophilic region of the silicon base
It is distributed surface.
Optionally, the condition of the laser processing are as follows: speed 100-1000mm/s, spot size 0.05-0.10mm,
Power is 5-50W, dotting time 0.05-0.5ms.
Optionally, this method further include: before hydroxylating processing, remove the impurity of the first surface, and optionally
First is carried out to the first surface to be dried；And/or
Before the third surface carries out the processing of constituency ultraviolet irradiation, the described organic molten of the third surface is removed
Liquid, and second optionally is carried out to the third surface and is dried.
Optionally, removing organic solution and/or the method for the impurity includes: by the first surface and/or third table
Face is placed in solvent and is cleaned by ultrasonic；The time of the ultrasonic cleaning is 1-10min, supersonic frequency 20-90kHz, temperature
Degree is 15-25 DEG C, and the solvent includes at least one of acetone, dehydrated alcohol and ultrapure water；
The condition of first drying process and second drying process includes: at room temperature, to use nitrogen each independently
The first surface and/or third surface 1-5min are swept in air-blowing, then carry out isothermal holding；The time of the isothermal holding is 30-
60min, temperature are 80-100 DEG C.
Optionally, this method further include: the first surface is irradiated using the first ultraviolet light and carries out the hydroxylating processing,
Obtain the second surface；The first ultraviolet irradiation time is 60-120min, and the wavelength of the ultraviolet light is 200-
300nm。
Optionally, the preparation method of the organic solution includes: to make perfluoro decane base trichlorosilane under conditions of hydrolysis
With water in the presence of 2,2,4- trimethylpentanes haptoreaction, obtain the organic solution；The 2,2,4- trimethylpentane
Volume ratio with the perfluoro decane base trichlorosilane is 1:(0.01-0.02).
Optionally, this method further include: the third is irradiated using ultraviolet light in the third surface described in exposure mask covering part
Surface carries out the constituency ultraviolet irradiation processing, obtains the super-hydrophobic super hydrophilic area distribution surface of the silicon base；The constituency
The time of ultraviolet irradiation is 60-120min, and the wavelength of second ultraviolet light is 200-300nm.
It is super-hydrophobic that disclosure second aspect provides a kind of silicon base that the method that disclosure first aspect provides is prepared
Super hydrophilic area distribution surface.
Optionally, the first surface of the micrometer-submicrometer grade coarse structure includes micron-sized coarse structure and distribution
In the coarse structure of the submicron order on the micron-sized coarse structure.
The disclosure third aspect provides a kind of super-hydrophobic super hydrophilic area distribution of silicon base that disclosure second aspect provides
Application of the surface at least one of construction material, biological medicine and traffic and transport field.
Through the above technical solutions, the silicon substrate surface that is prepared of disclosed method have it is excellent super hydrophilic/super
Hydrophobic region distribution character.Specifically, micrometer-submicrometer is constructed in silicon substrate surface by the laser processing of ad hoc fashion
The coarse structure of grade, obtains the first surface for being covered with the microstructure of irregular arrangement；By carrying out hydroxylating to first surface
Processing obtains second surface, and makes gained second surface and organic solvent that condensation reaction occur, and silicon base can be effectively reduced
Surface free energy, to obtain the third surface with super-hydrophobicity；Ultraviolet irradiation processing in constituency is carried out to third surface again, is made
Selected area is converted into ultra-hydrophilic surface, and selected region is not still super hydrophobic surface.Wherein, selected area refers in silicon base
Can be by ultraviolet light direct irradiation, and the region to react under action of ultraviolet radiation, refer to cannot be not purple in selected region
The region that outside line is irradiated to.Super hydrophobic surface has the excellent properties such as antifouling corrosion resistant, fluid drag-reduction, automatically cleaning, ultra-hydrophilic surface
Have excellent properties with antifouling antifog, water-oil separating etc., by the silicon substrate surface that the two advantage is concentrated can satisfy construction material,
Demand of the fields such as biological medicine, communications and transportation to material.
Other feature and advantage of the disclosure will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
Attached drawing is and to constitute part of specification for providing further understanding of the disclosure, with following tool
Body embodiment is used to explain the disclosure together, but does not constitute the limitation to the disclosure.In the accompanying drawings:
Fig. 1 is the SEM photograph (amplification factor 2000 on the super-hydrophobic super hydrophilic area distribution surface of the silicon base of the disclosure
Times).
Fig. 2 is the Contact-angle measurement figure on the super-hydrophobic super hydrophilic area distribution surface of the silicon base of the disclosure.
Fig. 3 is the Contact-angle measurement figure on the super-hydrophobic super hydrophilic area distribution surface of the silicon base of the disclosure.
Specific embodiment
It is described in detail below in conjunction with specific embodiment of the attached drawing to the disclosure.It should be understood that this place is retouched
The specific embodiment stated is only used for describing and explaining the disclosure, is not limited to the disclosure.
Disclosure first aspect provides a kind of method for preparing the super-hydrophobic super hydrophilic area distribution surface of silicon base, this method
The following steps are included:
(1) surface of silicon base is laser machined, obtains first table with micrometer-submicrometer grade coarse structure
Face；
(2) hydroxylating processing is carried out to the first surface, obtains second surface；
(3) under conditions of condensation reaction, so that the second surface and organic solution is carried out condensation reaction, obtain third table
Face；
(4) ultraviolet irradiation processing in constituency is carried out to the third surface, obtains the super-hydrophobic super hydrophilic region of the silicon base
It is distributed surface.
Wherein, silicon base is well known to those skilled in the art, such as can be silicon plate of the surface through sanding and polishing,
Polishing can be used the sand paper that abrasive grain degree is 400 mesh, 800 mesh, 1200 mesh, 1500 mesh and 2000 mesh and successively polish, then to table
Face is polished again, obtains smooth silicon substrate surface.
The silicon substrate surface of the disclosure forms the surface with micrometer-submicrometer grade coarse structure after laser machining, empty
Gas can be stored in microscopic gaps, to form solid-liquid-gas three-phase composite contact interface, can reduce silicon substrate surface oneself
By energy；By making the surface with micrometer-submicrometer coarse structure successively carry out hydroxylating processing and condensation reaction, can reduce
The surface free energy of silicon substrate surface, and then the friction between solid-liquid interface is effectively reduced and sticks, increase water droplet in solid table
The contact angle in face, so that silicon substrate surface has good hydrophobicity；Ultraviolet irradiation processing in constituency is carried out to silicon substrate surface again
Afterwards, so that the third surface conversion of selected areas is water-wetted surface, so as to obtain with hydrophily and hydrophobic region
The silicon substrate surface of distribution.The silicon substrate surface that disclosed method is prepared has excellent hydrophily and hydrophobicity.
A kind of specific embodiment, the condition of laser processing can be with are as follows: speed 100-1000mm/s, spot size are
0.05-0.1mm, power 5-50W, dotting time 0.05-0.5ms.Preferably, speed 500-800mm/s, spot size
For 0.05mm, power 18-30W, dotting time 0.2-0.35ms.Other conditions of laser processing can be according to actual needs
It is selected, such as the frequency of laser can be 10-15KHz.Under the above conditions, laser processing can be on the surface of silicon base
Circular array is formed, the adjacent circular and circle of every row are tangent, and the adjacent circular and circle of each column are also tangent, round and round
The tangent can be repeated processing, thus can produce largely overlapping circle, being formed has micrometer-submicrometer coarse structure
Surface, the surface irregularity, in silicon substrate surface having a size of being also attached on micron-sized coarse structure having a size of sub-micron
The smaller coarse structure of grade, structure is irregular, and the surface of the disclosure can be made to have more excellent hydrophily and hydrophobic
Property.Wherein, laser processing can be to carry out, for example, by using laser marking in the conventional use of equipment of those skilled in the art institute
Machine is laser machined.
A kind of specific embodiment, this method can also include: to remove the miscellaneous of first surface before hydroxylating processing
Matter, and first optionally is carried out to first surface and is dried.It removes impurity and the first drying process can be using this field
The method that technical staff routinely uses, it is preferable that first surface can be placed in solvent and be cleaned by ultrasonic；It is ultrasonic clear
The time washed can be 1-10min, and supersonic frequency can be 20-90kHz, and temperature can be 15-25 DEG C, and solvent may include third
At least one of ketone, dehydrated alcohol and ultrapure water, it is preferable that can successively use acetone, dehydrated alcohol and ultrapure water to
One surface is cleaned by ultrasonic.Preferably, the first drying process can be at room temperature, to purge first surface 1- with nitrogen
5min, then carry out isothermal holding.Wherein, isothermal holding can carry out in the equipment that those skilled in the art routinely use,
Such as isothermal holding can be carried out in a vacuum drying oven, the time of isothermal holding can be 30-60min, and temperature can be 80-
100 DEG C, pressure can be normal pressure.It can make the dry free from admixture of first surface by above-mentioned processing, be conducive to hydroxylating processing
Go on smoothly, to guarantee that second surface has good hydrophobicity.
Another specific embodiment, this method can also include: to remove the before carrying out the processing of constituency ultraviolet irradiation
The organic solution on three surfaces, and optionally third surface is dried.It can be using the impurity for removing first surface
Method removes the organic solution on third surface, can use to the withering method of first surface and condition to third table
Face is dried, and details are not described herein for other methods.
A kind of specific embodiment, this method can also include: to carry out hydroxyl using the first ultraviolet light irradiation first surface
Change processing, obtains second surface；The ultraviolet irradiation time can be 60-120min, and the wavelength of ultraviolet light can be 200-
300nm.Ultraviolet light irradiation is well known to those skilled in the art, such as can carry out ultraviolet light irradiation using ultraviolet lamp.
Within the above range, the abundant hydroxylating of first surface can be made, and then make it have good hydrophily.
According to the disclosure, the preparation method of organic solution may include: to make perfluoro decane base trichlorine under conditions of hydrolysis
Silane and the water haptoreaction in the presence of 2,2,4- trimethylpentanes, obtain organic solution；2,2,4- trimethylpentane and complete
The volume ratio of fluorine decane base trichlorosilane can be 1:(0.01-0.02), preferably 1:(0.014-0.016), so that perfluor
Decane base trichlorosilane can be hydrolyzed thoroughly, to form the organic solution of excellent in physical and chemical performance, may advantageously facilitate the second table
Face and organic solution carry out condensation reaction, generate the good third surface of hydrophobicity.
A kind of specific embodiment, this method can also include: to be shone using ultraviolet light with exposure mask covering part third surface
It penetrates third surface and carries out the processing of constituency ultraviolet irradiation, obtain the super-hydrophobic super hydrophilic area distribution surface of silicon base；The ultraviolet photograph in constituency
The time for penetrating processing can be 60-120min, and wavelength can be 200-300nm.The silicon base covered to exposure mask carries out hydroxyl
Change processing so that be exposed to outer silicon base is converted into ultra-hydrophilic surface under ultraviolet irradiation, and capped silicon base according to
Old is super hydrophobic surface.What exposure mask was well known to those skilled in the art, the material of exposure mask can be metal material, for example,
TC4 titanium alloy, thickness can be 0.1-0.5mm, and the machine that can be cut by laser is cut on metallic substrates, to have obtained not
With the mask plate of hole shape.Such as can be cut into edge width on metallic substrates is 3-5mm, line width 3-5mm, spacing
The linear pattern of 1-10mm, completely removes pitch portions, obtains the exposure mask, specific line width and spacing can according to the actual situation into
Row change.
It is super-hydrophobic that disclosure second aspect provides a kind of silicon base that the method that disclosure first aspect provides is prepared
Super hydrophilic area distribution surface.The super-hydrophobic ultra-hydrophilic surface of the silicon base of the disclosure has excellent hydrophily and hydrophobicity, surpasses
Hydrophobic surface has the excellent properties such as antifouling corrosion resistant, fluid drag-reduction, automatically cleaning, and ultra-hydrophilic surface is with antifouling antifog, grease point
From etc. have excellent properties, by the two advantage concentrate to meet the fields such as construction material, biological medicine, communications and transportation to the need of material
It asks.
According to the disclosure, the first surface of micrometer-submicrometer grade coarse structure may include micron-sized coarse structure and
It is distributed in the coarse structure of the submicron order on micron-sized coarse structure.Wherein, the coarse structure of micrometer-submicrometer grade be by
Silicon substrate surface is generated in the presence of repetition processing under specific operating parameter in laser.It is thick with micrometer-submicrometer grade
The first surface of rough structure is more coarse, close to the random arrangement state in nature, silicon substrate surface can be made to have more
Excellent hydrophobicity and hydrophily.
The disclosure third aspect provides a kind of super-hydrophobic super hydrophilic area distribution of silicon base that disclosure second aspect provides
Application of the surface at least one of fields such as construction material, biological medicine and communications and transportation.
The disclosure is further illustrated below by embodiment, but therefore the disclosure is not any way limited.
Embodiment 1
Silicon substrate surface is laser machined, the condition of laser processing are as follows: speed 500mm/s, spot size are
0.05mm, power 18W, frequency 10KHz, dotting time 0.2ms obtain having micrometer-submicrometer grade coarse structure
First surface；
First surface is successively cleaned by ultrasonic with acetone, dehydrated alcohol and ultrapure water, scavenging period 5min, then
At room temperature, first surface 2min is purged with nitrogen.Ultraviolet treatment with irradiation is carried out to first surface, the power of ultraviolet lamp is 75W,
Irradiation time is 60min, and the wavelength of ultraviolet light is 254nm, obtains second surface；
By volume it is 1.5:100, perfluoro decane base trichlorosilane is instilled in 2,2,4- trimethylpentanes, the perfluor last of the ten Heavenly stems is made
Alkyltrichlorosilanes occur hydrolysis and obtain organic solution, and second surface and organic solution is made to carry out condensation reaction, obtain the
Three surfaces；
Successively third surface is cleaned by ultrasonic with acetone, ethyl alcohol and ultrapure water, purges third surface 2min, and 90
30min is kept the temperature under conditions of DEG C in a vacuum drying oven.Third surface is covered with exposure mask, ultraviolet treatment with irradiation is carried out to it,
The power of ultraviolet lamp is 75W, and the wavelength of irradiation time 60min, ultraviolet light are 254nm, and it is super-hydrophobic super hydrophilic to obtain silicon base
Area distribution surface.Wherein, mask plate is TC4 titanium alloy, with a thickness of the plate of 0.5mm.Using laser cutting machine on substrate
Being cut into edge width is 3mm, and line width 5mm, spacing is the linear pattern of 5mm, and pitch portions completely remove.
Super hydrophilic area distribution surface super-hydrophobic to silicon base obtained carries out SEM characterization, and uses contact angle measurement
Contact angle is surveyed, characterization and measurement result are shown in Fig. 1-3.
By Fig. 1-3 it is found that the silicon substrate surface of the disclosure has micrometer-submicrometer grade coarse structure, water in hydrophilic region
Contact angle with silicon substrate surface is 0 °, and the contact angle of water and silicon substrate surface is 159.3 ° in hydrophobic region, the silicon of the disclosure
Substrate surface has excellent hydrophily and hydrophobicity.
Embodiment 2
Silicon substrate surface is prepared using method same as Example 1, the difference is that only, the item of the laser processing
Part are as follows: speed 700mm/s, spot size 0.05mm, power 16W, frequency 15KHz, dotting time 0.1ms.
The silicon substrate surface of the disclosure has micrometer-submicrometer grade coarse structure, water and silicon substrate surface in hydrophilic region
Contact angle be 0 °, in hydrophobic region the contact angle of water and silicon substrate surface be 149.6 °, the silicon substrate surface of the disclosure has
Hydrophily and hydrophobicity.
Embodiment 3
Silicon substrate surface is prepared using method same as Example 1, the difference is that only, first surface is carried out purple
Outside line treatment with irradiation, the power of ultraviolet lamp are 75W, and the wavelength of irradiation time 65min, ultraviolet light are 300nm, obtain the second table
Face.
The silicon substrate surface of the disclosure has micrometer-submicrometer grade coarse structure, water and silicon substrate surface in hydrophilic region
Contact angle be 0 °, in hydrophobic region the contact angle of water and silicon substrate surface be 151.4 °, the silicon substrate surface of the disclosure has
Excellent hydrophily and hydrophobicity.
Embodiment 4
Third surface is covered with exposure mask, ultraviolet treatment with irradiation is carried out to it, the power of ultraviolet lamp is 75W, irradiation time
Wavelength for 70min, ultraviolet light is 200nm, obtains the super-hydrophobic super hydrophilic area distribution surface of silicon base.
The silicon substrate surface of the disclosure has micrometer-submicrometer grade coarse structure, water and silicon substrate surface in hydrophilic region
Contact angle be 0 °, in hydrophobic region the contact angle of water and silicon substrate surface be 150.3 °, the silicon substrate surface of the disclosure has
Excellent hydrophily and hydrophobicity.
Comparative example 1
Silicon substrate surface is prepared using method same as Example 1, the difference is that only, silicon substrate surface is carried out
Laser processing, the condition of laser processing are as follows: speed 1500mm/s, spot size 0.05mm, power 10W, frequency are
20KHz, dotting time 0.01ms obtain the first surface with micron order coarse structure.
The silicon base of the disclosure has micron order coarse structure, and the contact angle of water and silicon substrate surface is in hydrophilic region
4 °, the contact angle of water and silicon substrate surface is 109.9 ° in hydrophobic region, and the silicon substrate surface of the disclosure does not have excellent parent
Aqueous and hydrophobicity.
The preferred embodiment of the disclosure is described in detail in conjunction with attached drawing above, still, the disclosure is not limited to above-mentioned reality
The detail in mode is applied, in the range of the technology design of the disclosure, a variety of letters can be carried out to the technical solution of the disclosure
Monotropic type, these simple variants belong to the protection scope of the disclosure.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the disclosure to it is various can
No further explanation will be given for the combination of energy.
In addition, any combination can also be carried out between a variety of different embodiments of the disclosure, as long as it is without prejudice to originally
Disclosed thought equally should be considered as disclosure disclosure of that.
Claims (10)
1. a kind of method for preparing the super-hydrophobic super hydrophilic area distribution surface of silicon base, which is characterized in that this method includes following
Step:
(1) surface of silicon base is laser machined, obtains the first surface with micrometer-submicrometer grade coarse structure；
(2) hydroxylating processing is carried out to the first surface, obtains second surface；
(3) under conditions of condensation reaction, so that the second surface and organic solution is carried out condensation reaction, obtain third surface；
(4) ultraviolet irradiation processing in constituency is carried out to the third surface, obtains the super-hydrophobic super hydrophilic area distribution of the silicon base
Surface.
2. the method according to claim 1, wherein the condition of the laser processing are as follows: speed 100-
1000mm/s, spot size 0.05-0.1mm, power 5-50W, dotting time 0.05-0.5ms.
3. the method according to claim 1, wherein this method further include: before hydroxylating processing, remove
The impurity of the first surface is removed, and first optionally is carried out to the first surface and is dried；And/or
Before the third surface carries out the processing of constituency ultraviolet irradiation, the organic solution on the third surface is removed, and
Optionally second is carried out to the third surface to be dried.
4. according to the method described in claim 3, it is characterized in that, the method for removing the organic solution and/or the impurity
It include: that the first surface and/or third surface are placed in solvent and are cleaned by ultrasonic；The time of the ultrasonic cleaning is
1-10min, supersonic frequency 20-90kHz, temperature are 15-25 DEG C, and the solvent includes in acetone, dehydrated alcohol and ultrapure water
At least one；
The condition of first drying process and second drying process includes: at room temperature, to be blown with nitrogen each independently
The first surface and/or third surface 1-5min are swept, then carries out isothermal holding；The time of the isothermal holding is 30-
60min, temperature are 80-100 DEG C.
5. the method according to claim 1, wherein this method further include: using described in the irradiation of the first ultraviolet light
First surface carries out the hydroxylating processing, obtains the second surface；The first ultraviolet irradiation time is 60-
120min, the wavelength of the ultraviolet light are 200-300nm.
6. the method according to claim 1, wherein the preparation method of the organic solution includes: in hydrolysis
Under the conditions of, make perfluoro decane base trichlorosilane and the water haptoreaction in the presence of 2,2,4- trimethylpentanes, obtains described having
Machine solution；
The volume ratio of the 2,2,4- trimethylpentane and the perfluoro decane base trichlorosilane is 1:(0.01-0.02).
7. the method according to claim 1, wherein this method further include: the third described in exposure mask covering part
Surface irradiates the third surface using ultraviolet light and carries out the constituency ultraviolet irradiation processing, it is super-hydrophobic to obtain the silicon base
Super hydrophilic area distribution surface；The time of the constituency ultraviolet irradiation processing is 60-120min, the wavelength of second ultraviolet light
For 200-300nm.
8. the super-hydrophobic super hydrophilic area distribution table of the silicon base that method described in any one of claim 1-7 is prepared
Face.
9. surface according to claim 8, which is characterized in that the first surface of the micrometer-submicrometer grade coarse structure
Coarse structure including micron-sized coarse structure and the submicron order being distributed on the micron-sized coarse structure.
10. the super-hydrophobic super hydrophilic area distribution surface of silicon base as claimed in claim 9 is in construction material, biological medicine and traffic
Application at least one of transport field.
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