CN107546102A - A kind of method for preparing micro-nano-scale periodically or non-periodically structure in material surface - Google Patents
A kind of method for preparing micro-nano-scale periodically or non-periodically structure in material surface Download PDFInfo
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- CN107546102A CN107546102A CN201610475697.7A CN201610475697A CN107546102A CN 107546102 A CN107546102 A CN 107546102A CN 201610475697 A CN201610475697 A CN 201610475697A CN 107546102 A CN107546102 A CN 107546102A
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Abstract
The invention discloses a kind of method for preparing micro-nano-scale periodically or non-periodically structure in material surface, the particularly method in diamond surface manufacturing cycle structure, this method comprises the following steps：(1) the coating impressing glue on substrate；The demoulding after the template with periodically or non-periodically structure is stamped on substrate using stamping technique, impressing glue is set to be formed in substrate surface with periodically raised；(2) be stripped after on substrate deposited metal layer, metal level is only deposited at the raised surface；(3) plasma etching；(4) metal level of deposition and impressing glue are peeled off from substrate, obtaining surface has the material of periodically or non-periodically structure.The preparation process of the present invention is simple, one-shot forming；Pollution-free, low power consuming, low noise, without sewage discharge, product life cycle length.This method has universality, is generally applicable to the cycle of various different micro-/ nano yardsticks or the preparation of aperiodic structure device.
Description
Technical field
The present invention relates to a kind of method for preparing micro-nano-scale periodically or non-periodically structure in material surface.
Background technology
Diamond is hardness highest material in nature, and as a kind of " jewel " truly, diamond provides
A series of special performance, including translucency, heat conductivity, rigidity, wearability and its characteristic electron.Particularly diamond
When size and purity reach certain level, numerous performances particularly optics and semiconducting behavior of diamond is preferably played
Be widely applied.
In backing material, silicon and sapphire are more commonly used backing materials.From the seventies, with the preparation of silicon materials
Technique and semiconductor surface technique are updated, and silicon detector has obtained development quickly.But in strong radiation environment, silicon crystal lattice
It is vulnerable to radiation injury, makes the increase of detector leakage current, hydraulic performance decline.Because intrinsic conductivity caused by thermal excitation is with temperature
Exponentially increase, and the energy gap of silicon is smaller, therefore the device of silicon materials manufacture is not suitable for being operated in 150 DEG C of environment
In.Sapphire Substrate has production technology maturation when light-emitting diode chip for backlight unit makes, device quality is good, stability is good, mechanical
The features such as intensity is high.But there is also the problem of lattice mismatch and thermal stress mismatch.Sapphire poor thermal conductivity（100 DEG C about
25W/(m·K)）, when using LED component, substantial amounts of heat can be transferred out, high power device particularly larger to area,
Thermal conductivity is a very important Consideration.
The content of the invention
It is an object of the invention to provide one kind micro-nano-scale periodically or non-periodically structure is prepared in material surface
Method, by the substrate of large scale high cleanliness use nano impression, growth the skill such as metal level and plasma etching
The material with periodic structure is made in art.By further selecting diamond to be used as backing material, prepared has cycle knot
The material of structure, it can be used for preparing all kinds of reflections under high radiation condition and transmission grating, photonic crystal light-emitting diode, phenanthrene
Nie Er lens etc., and can apply in medical treatment, the outer space, nuclear power station etc. used in high-radiation field in sensitive detection parts.Together
When, in order to expand the radiation hardness diamond Meta Materials with periodic structure, we take new preparation technology, reduce preparation
Cost, reduce environmental pollution while improve the product precision of gained diamond.
The technical scheme is that, there is provided one kind prepares micro-nano-scale in material surface and periodically or non-periodically tied
The method of structure, comprises the following steps：
(1) the coating impressing glue on substrate；The template with periodically or non-periodically structure is stamped into using stamping technique
It is stripped after on substrate, impressing glue is formed in substrate surface with projection periodically or non-periodically；
(2) the deposited metal layer on substrate, metal level is made to be only deposited at the raised surface；
(3) plasma etching is carried out；
(4) metal level of deposition and impressing glue are peeled off from substrate, obtains surface with periodically or non-periodically structure
Material.
Further, step（1）In, the stamping technique refers to nanometer embossing；The stamping technique is hot padding
Or ultraviolet light solidification stamping technique；Preferably, the resolution ratio of impressing is less than 10nm.
Further, step（2）In, the step of removing cull is not included before deposited metal.Optionally, walked in deposited metal
Included after rapid and go cull step.
Further, periodic structure refers to the microstructure of micron order, Nano grade, particularly size less than 10nm's
Structure.
Further, step（2）In, the metal level is Cr layers；Preferably, the thickness of the Cr layers is 5-20nm；Institute
Cr layers are stated as technology growths such as electron beam evaporation or magnetron sputterings.
Further, step（3）In, the plasma etching is reactive plasma etching or inductively coupled plasma
Etching.
Further, step（1）In, the substrate is diamond；Preferably, the diamond is monocrystalline or polycrystalline gold
Hard rock.
Further, the projection periodically or non-periodically for rectangular, aciculiform, inverted V-shaped, inverted pyramid
The one or more of the micron and nano periodic structure of shape or various irregular shapes.
The present invention, which further provides surface prepared by described method, has the material of periodically or non-periodically structure.
The diamond that the present invention further relates to surface and has periodic structure is being prepared in high radiation condition
Under all kinds of reflections and transmission grating, photonic crystal light-emitting diode, Fresnel Lenses in application, and in medical treatment, outside too
Application in detector used in the high radiation field such as sky, nuclear power station.
The present invention will be further described by taking diamond as an example below：The present invention prepares a kind of resistance to spoke with periodic structure
Radioglold hard rock Meta Materials,, can due to excellent radiation resistance first in the exceedingly odious radiation field of environmental condition
Using as radiation-resistant window, such as all kinds of reflections under X-ray window, radiation condition and transmission grating, the pole of photonic crystal light-emitting two
Pipe, Fresnel Lenses, radiation detector etc..Secondly, diamond energy gap is（5.5eV）, resistivity is high, and dielectric constant is small,
These electrical properties ensure that diamond is small as device noise, and signal to noise ratio is high.And because energy gap is big, diamond is near
Ultraviolet to infra-red range is nearly all transparent, and influence of the veiling glare to diamond is minimum in use.Because band gap is wide,
Diamond device is compared with silicon transistor can be at a much higher temperature（500℃）Work, in electronic application field diamond
Device will substitute the silicon device in adverse circumstances.In addition, diamond thermal conductivity is high so that diamond detector can be in room
Temperature, even normal work under high temperature, it is not necessary to the additional cooling system as silicon detector.Finally, the high rigidity of diamond also makes
It has be not easy to be scratched in use damage this it is unique the advantages of.
The nanometer embossing of the process to the present invention and prior art makees some contrasts below：In the prior art,
The flow of nanometer embossing can be divided into：Impressing preparation-impressing-is stripped-gone cull-evaporation-stripping-etching, sees accompanying drawing 1.
Accordingly, the process step of the invention is：Impressing-the demoulding-evaporation-etching-stripping.Can save to steam goes cull to walk before crossing
Suddenly, its it is of the prior art go cull step, can cause imprint glue be brokenly corroded, so as to cause obtained periodicity
The shape of structure is destroyed to a certain degree.
Being explained further for present invention process is as follows：By taking rectangular preiection as an example, ferryman's skill is steamed using orientation, gold can be caused
Category is only in the site deposition of projection, and groove is interior due to non-deposited metal layer, so be just selectively removed, and under groove
The substrate of side is also etched away.Meanwhile in plasma etching, the superposition of polymeric layer and metal deposition layer significantly increases
Mask thicknesses, reduce the difficulty of follow-up stripping technology, technique is simple, and effect is more excellent.
Compared to nano impression of the prior art, the common process for being stripped, going cull, steaming to cross, peel off, etch, this hair
Bright preparation process is simple, operability is stronger, technology difficulty is lower, pollution-free, low power consuming, low noise, without sewage arrange
Put, product life cycle length.This method has universality, is generally applicable to the cycle of various different micro-/ nano yardsticks or non-week
The preparation of phase component；Layout by changing impression block can manufacture the Meta Materials of different diamond substrates.
Preparation of the above-mentioned technique particularly suitable for diamond Meta Materials, general work can be overcome using above-mentioned preparation technology
Skill is difficult to be prepared on a diamond substrate the technical barrier of the product with excellent surface smoothness, steep property.It is prepared into
To the diamond with periodic structure have extremely strong radiation resistance, can be used under high radiation condition, product surface
Smooth, regularity is good, and steep property is good；The radiation hardness diamond Meta Materials application field of the periodic structure of preparation is wide, can be used for
Prepare all kinds of reflections and transmission grating, photonic crystal light-emitting diode, Fresnel Lenses under high radiation condition etc., Yi Jike
To apply in medical treatment, the outer space, nuclear power station etc. used in high-radiation field in sensitive detection parts.
Brief description of the drawings
Fig. 1 represents nanometer embossing schematic diagram of the prior art（Derive from《Sub-wavelength based on nanometer embossing
Anti-reflection structure optics is studied》, Jiang Keming, University Of Suzhou, master thesis）；
Fig. 2 represents to prepare the process chart for the diamond that surface has periodic structure.
Wherein, the polymer in accompanying drawing is exactly finger pressure print glue, and photoresist is the most frequently used impressing glue.
Embodiment
With reference to embodiment, the invention will be further described.
To make the object, technical solutions and advantages of the present invention clearer, the embodiments of the present invention are carried out below
Detailed elaboration.The given examples are served only to explain the present invention, is not intended to limit the scope of the present invention.
Following embodiment 1-4 are prepared using the preparation technology flow described in Fig. 2.
Embodiment 1
The preparation high-purity single-crystal diamond for the microwave plasma chemical vapor deposition apparatus for being 75KW with power, and by its size
Be processed as 20mm × 20mm × 10mm high-purity diamond substrate, imprinted by ultraviolet solidified nano, electron beam evaporation, etc. from
The steps such as sub- lithographic technique produce the periodic pattern for the rectangular that resolution ratio is 10nm, and gained sample surfaces are smooth, steep property
Good, etching trench bottom is close to square.The diamond Meta Materials of this periodic structure can be used for preparing under high radiation condition
All kinds of reflections and transmission grating, photonic crystal light-emitting diode, Fresnel Lenses etc., and can apply medical treatment, the outer space,
Nuclear power station etc. is used in high-radiation field in sensitive detection parts.
Embodiment 2
The preparation high-purity single-crystal diamond for the microwave plasma chemical vapor deposition apparatus for being 75KW with power, and by its size
Be processed as 20mm × 20mm × 6mm high-purity diamond substrate, imprinted by ultraviolet solidified nano, electron beam evaporation, etc. from
The steps such as sub- lithographic technique produce the periodic pattern of 5nm rectangulars, and gained sample surfaces are smooth, and steep property is good, etching groove bottom
Portion is close to square.The diamond Meta Materials of this periodic structure can be used for preparing all kinds of reflections under high radiation condition and thoroughly
Grating, photonic crystal light-emitting diode, Fresnel Lenses etc. are penetrated, and can be applied in medical treatment, the outer space, nuclear power station etc. in height
Used in radiation field in sensitive detection parts.
Embodiment 3
The preparation high-purity single-crystal diamond for the microwave plasma chemical vapor deposition apparatus for being 75KW with power, and by its size
Be processed as 20mm × 20mm × 6mm high-purity diamond substrate, imprinted by ultraviolet solidified nano, electron beam evaporation, etc. from
Sub- lithographic technique produces the periodic pattern of 50nm inverted V-shapeds, and gained sample surfaces are smooth, and steep property is good, and etching trench bottom approaches
It is square.The diamond Meta Materials of this periodic structure can be used for preparing all kinds of reflections and transmitted light under high radiation condition
Grid, photonic crystal light-emitting diode, Fresnel Lenses etc., and can apply and be radiated in medical treatment, the outer space, nuclear power station etc. in height
Used in sensitive detection parts.
Embodiment 4
The preparation high-purity single-crystal diamond for the microwave plasma chemical vapor deposition apparatus for being 75KW with power, and by its size
Be processed as 20mm × 20mm × 10mm high-purity diamond substrate, imprinted by ultraviolet solidified nano, electron beam evaporation, etc. from
Sub- lithographic technique produces the periodic pattern of 50nm inverted V-shapeds, and gained sample surfaces are smooth, and steep property is good, and etching trench bottom approaches
It is square.The diamond Meta Materials of this periodic structure can be used for preparing all kinds of reflections and transmitted light under high radiation condition
Grid, photonic crystal light-emitting diode, Fresnel Lenses etc., and can apply and be radiated in medical treatment, the outer space, nuclear power station etc. in height
Used in sensitive detection parts.
Comparative example 1
Using diamond same as Example 1, Fig. 1 is used（Derive from《Sub-wavelength antireflection knot based on nanometer embossing
Structure optics is studied》, Jiang Keming, University Of Suzhou, master thesis）Preparation method, gained sample surfaces are rough, suddenly
Straightforward difference.And preparation technology is complicated, it is big that the later stage peels off difficulty.
The step of various methods divide above, be intended merely to describe it is clear, can be merged into when realizing a step or
Some steps are split, are decomposed into multiple steps, as long as including identical logical relation, all protection domain in this patent
It is interior；To either adding inessential modification in algorithm in flow or introducing inessential design, but its algorithm is not changed
Core design with flow is all in the protection domain of the patent.
It will be understood by those skilled in the art that the respective embodiments described above are to realize the specific embodiment of the present invention,
And in actual applications, can to it, various changes can be made in the form and details, without departing from the spirit and scope of the present invention.
Claims (10)
- A kind of 1. method for preparing micro-nano-scale periodically or non-periodically structure in material surface, it is characterised in that including Following steps：(1) the coating impressing glue on substrate；The template with periodically or non-periodically structure is stamped into using stamping technique It is stripped after on substrate, impressing glue is formed in substrate surface with projection periodically or non-periodically；(2) the deposited metal layer on substrate, metal level is made to be only deposited at the raised surface；(3) plasma etching is carried out；(4) metal level of deposition and impressing glue are peeled off from substrate, obtains surface with periodically or non-periodically structure Material.
- 2. the method as described in claim 1, it is characterised in that step（1）In, the impressing refers to nano impression；Preferably, Imprinted using ultraviolet light solidified imprinting or thermoplastic, the resolution ratio of impressing is less than 10nm.
- 3. the method as described in claim any one of 1-2, it is characterised in that do not include before deposited metal layer and go cull step.
- 4. the method as described in claim any one of 1-3, it is characterised in that step（2）In, the metal level is Cr layers；It is excellent Selection of land, the thickness of the Cr layers is 5-20nm.
- 5. the method as described in claim any one of 1-4, it is characterised in that step（3）In, the plasma etching is reaction Plasma etching or inductively coupled plasma etching.
- 6. the method as described in claim any one of 1-5, it is characterised in that step（1）In, the substrate is diamond；It is excellent Selection of land, the diamond are monocrystalline or polycrystalline diamond.
- 7. the method as described in claim any one of 1-6, it is characterised in that the projection periodically or non-periodically is square The one of formation, aciculiform, inverted V-shaped, reverse pyramid or various irregular shapes micron or nano periodic structure Kind is a variety of.
- 8. surface prepared by a kind of method as described in claim any one of 1-7 has the material of periodically or non-periodically structure Material.
- 9. a kind of diamond with surface periodic structure, it is characterised in that the use of diamond is substrate, using claim Any one preparation method described in 1-7 obtains.
- 10. the surface described in claim 9 has the diamond of periodic structure each under high radiation condition in preparation Application in class reflection and transmission grating, photonic crystal light-emitting diode, Fresnel Lenses, and in medical treatment, the outer space, nuclear power The application stood in detector used in contour radiation field.
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| CN110329985A (en) * | 2019-06-18 | 2019-10-15 | 长沙新材料产业研究院有限公司 | A kind of diamond surface labyrinth and preparation method thereof |
| CN112639575A (en) * | 2018-09-07 | 2021-04-09 | 华为技术有限公司 | High refractive index waveguide for augmented reality |
| WO2022109854A1 (en) * | 2020-11-25 | 2022-06-02 | 苏州晶湛半导体有限公司 | Composite substrate, photoelectric device and preparation method therefor |
| CN116604120A (en) * | 2023-07-21 | 2023-08-18 | 中国科学院宁波材料技术与工程研究所 | Anti-counterfeiting mark welding method, device and application based on diamond substrate |
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| CN112639575A (en) * | 2018-09-07 | 2021-04-09 | 华为技术有限公司 | High refractive index waveguide for augmented reality |
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| CN116604120A (en) * | 2023-07-21 | 2023-08-18 | 中国科学院宁波材料技术与工程研究所 | Anti-counterfeiting mark welding method, device and application based on diamond substrate |
| CN116604120B (en) * | 2023-07-21 | 2023-09-22 | 中国科学院宁波材料技术与工程研究所 | Anti-counterfeiting mark welding method, device and application based on diamond substrate |
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Application publication date: 20180105 |