CN106316468B - The method that the processing of nanometer striped array is carried out to ceramic material using AFM diamond probe - Google Patents
The method that the processing of nanometer striped array is carried out to ceramic material using AFM diamond probe Download PDFInfo
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- CN106316468B CN106316468B CN201610629882.7A CN201610629882A CN106316468B CN 106316468 B CN106316468 B CN 106316468B CN 201610629882 A CN201610629882 A CN 201610629882A CN 106316468 B CN106316468 B CN 106316468B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
- C04B41/5338—Etching
- C04B41/5346—Dry etching
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q70/00—General aspects of SPM probes, their manufacture or their related instrumentation, insofar as they are not specially adapted to a single SPM technique covered by group G01Q60/00
- G01Q70/16—Probe manufacture
Abstract
The method for carrying out the processing of nanometer striped array to ceramic material using AFM diamond probe, it is related to the method that a kind of pair of ultra hard ceramic material locally carries out the processing of superfine nano striped array structure.The present invention is that ultra hard ceramic materials chemistry inertia is high, hardness is big in order to solve, unmanageable technical problem.This method is as follows: one, preparing AFM Diamond tip；Two, AFM Diamond tip delineates ultra hard ceramic material (SiC single crystal) surface.The present invention is the method that a kind of pair of ultra hard ceramic material carries out the processing of superfine nano striped array structure, diamond crystal can intuitively be observed to the delineation situation of ultra hard ceramic material, depicting superfine nano striped array in ultra hard ceramic material surface, (width of fringe has many advantages, such as reproducible, high-efficient down to 15nm).The invention belongs to the field of superfine nano striped array structure processing is carried out to ultra hard ceramic material.
Description
Technical field
The present invention relates to the methods that a kind of pair of ultra hard ceramic material carries out the processing of superfine nano striped array.
Background technique
Ultra hard ceramic material is ceramic material of the hardness close to diamond (10 grades of Mohs' hardness).As silicon carbide, boron carbide,
Boron nitride and tungsten carbide etc. are ceramic.Since ultra hard ceramic material has the characteristics that chemical inertness is high, hardness is big, it is difficult to its surface
Carry out the processing of the micro-structure of nano-precision.Micro-structure with nano-precision using increasingly extensive, especially in optics member
The fields such as part.At present mainly using traditional processings means such as focused ion beam, electron beam and laser processings to ultra hard ceramic material
The processing of micro-structure is carried out, however process equipment is expensive, processing conditions is more harsh.
Atomic force microscope (Atomic Force Microscope, AFM) can both characterize material surface pattern and obtain three
Tie up image, can also by the physics chemical action between needle point and sample, improved on nanoscale metal, polymer and
The material surfaces such as semiconductor.And nowadays AFM has been successfully applied to local anodic oxidation, mechanical removal, chemistry removal and nanometer
The nanoprocessings fields such as etching.
Summary of the invention
The present invention is to solve to be difficult to ask in the technology that ultra hard ceramic material surface carries out the processing of nano-precision micro-structure
Topic provides a kind of method for carrying out the processing of nanometer striped array to ceramic material using AFM diamond probe.
Using AFM diamond probe to ceramic material carry out nanometer striped array processing method according to the following steps into
Row:
One, the preparation of AFM diamond probe:
It is coated with uv-curable glue in the mica upper surface of cleavage, then diamond crystal is dispersed in the mica of cleavage
The AFM probe of no needle point is contacted uv-curable glue, and the surface of mobile diamond crystal in mica surface by upper surface, into
Needle contacts diamond crystal until the AFM probe of no needle point, has the AFM probe of diamond crystal spoke under ultraviolet curing lamp for glutinous
According to 30 minutes, to ultra-violet curing adhesive curing and diamond crystal was firmly adhered on AFM probe, and AFM diamond probe is made；
Two, AFM set voltage value as 2~10V, pressure be 2000~20000nN, scored area is 5 × 5 μm2's
Under the conditions of, AFM diamond probe is carried out in ultra hard ceramic material surface by delineation 10min~4.5h using AFM contact mode, i.e.,
It completes to carry out the processing of nanometer striped array to ceramic material using AFM diamond probe.
Three, it will be swept after step 2 delineates treated ultra hard ceramic material clean using the tapping-mode of AFM
It retouches, observes scored area pattern (information such as nanometer width of fringe, depth).
Present invention mica used in step 1, uv-curable glue and the AFM probe without needle point are commercial product.
The present invention be it is a kind of using AFM diamond probe to ultra hard ceramic material carry out superfine nano striped array processing
Method directly observes diamond crystal to the delineation situation of ultra hard ceramic material using AFM after processing.Utilize AFM diamond
Probe ultra hard ceramic material surface depict superfine nano striped array (width of fringe down to 15nm), have it is reproducible,
The advantages that high-efficient.
It can be effectively by SiC using the method that AFM diamond probe carries out microcell delineation to SiC single crystal in atmospheric environment
The removal of monocrystalline skin-material, it is high-efficient and reproducible in the superfine nano striped array that surface of SiC formation width is 15nm.
The polish abrasive diamond crystal of use has the advantages that nontoxic, harmless, and processing environment is mild, process safety.The present invention mentions
For a kind of material removing rate higher, process control, low cost SiC material micro-nano manufacturing method.
Distinctive feature and beneficial effect of the invention is:
(1) for the features such as ultra hard ceramic material hardness is big, chemical inertness is high, the present invention can be effectively to ultra hard ceramic material
Carry out (processing of the width of fringe down to 15nm) of superfine nano striped array.
(2) ultra hard ceramic material surface is processed using AFM diamond probe, diamond crystal has nontoxic, nothing
Evil advantage, processing environment is mild, process safety, and has many advantages, such as that efficient, repeatability is high.
Detailed description of the invention
Fig. 1 is the optical microscopy shape appearance figure of AFM diamond probe；
Fig. 2 is the scanning electron microscope shape appearance figure of AFM diamond probe；
Fig. 3 is the superfine nano striped array AFM plan view tested in one in scored area；
Fig. 4 is the superfine nano striped array AFM plan view tested in one in scored area.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment
Any combination.
Specific embodiment 1: present embodiment carries out nanometer striped array to ceramic material using AFM diamond probe
The method of processing follows the steps below:
One, the preparation of AFM diamond probe:
It is coated with uv-curable glue in the mica upper surface of cleavage, then diamond crystal is dispersed in the mica of cleavage
The AFM probe of no needle point is contacted uv-curable glue, and the surface of mobile diamond crystal in mica surface by upper surface, into
Needle contacts diamond crystal until the AFM probe of no needle point, has the AFM probe of diamond crystal spoke under ultraviolet curing lamp for glutinous
According to 30 minutes, to ultra-violet curing adhesive curing and diamond crystal was firmly adhered on AFM probe, and AFM diamond probe is made；
Two, AFM set voltage value as 2~10V, pressure be 2000~20000nN, scored area is 5 × 5 μm2's
Under the conditions of, AFM diamond probe is carried out in ultra hard ceramic material surface by delineation 10min~4.5h using AFM contact mode, i.e.,
It completes to carry out the processing of nanometer striped array to ceramic material using AFM diamond probe.
Specific embodiment 2: the present embodiment is different from the first embodiment in that superhard pottery described in step 2
Ceramic material is silicon carbide (SiC) monocrystalline, and Mohs' hardness is 9.5 grades.It is other same as the specific embodiment one.
The purity of diamond crystal used in present embodiment is 99.9%.
It can be effectively by SiC single crystal using the method that AFM diamond probe delineates SiC single crystal microcell in atmospheric environment
Skin-material removal, forming superfine nano striped array in surface of SiC, (width of fringe is delineated high-efficient and is repeated down to 15nm)
Property is good.The polish abrasive diamond crystal (Mohs' hardness is 10 grade) used has many advantages, such as nontoxic, harmless, processing environment temperature
With, process safety, pollution-free.The present invention provide a kind of higher material removing rate, process control, low cost to ultra hard ceramic material
The method that material carries out the processing of superfine nano striped array structure.
Specific embodiment 3: unlike one of present embodiment and specific embodiment one or two described in step 2
Ultra hard ceramic material be boron carbide (B4C), Mohs' hardness is 9.3 grades.It is other identical as one of specific embodiment one or two.
Specific embodiment 4: AFM in step 2 unlike one of present embodiment and specific embodiment one to three
Set voltage value as 3~9V.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: AFM in step 2 unlike one of present embodiment and specific embodiment one to four
Set voltage value as 4~8V.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: AFM in step 2 unlike one of present embodiment and specific embodiment one to five
Set voltage value as 5~7V.It is other identical as one of specific embodiment one to five.
Specific embodiment 7: AFM in step 2 unlike one of present embodiment and specific embodiment one to six
Set voltage value as 6V.It is other identical as one of specific embodiment one to six.
Specific embodiment 8: being used in step 2 unlike one of present embodiment and specific embodiment one to seven
AFM contact mode carries out 10~60min of delineation in ultra hard ceramic material surface.Other phases one of with specific embodiment one to seven
Together.
Specific embodiment 9: being used in step 2 unlike one of present embodiment and specific embodiment one to eight
AFM contact mode carries out 1.5~4h of delineation in ultra hard ceramic material surface.Other phases one of with specific embodiment one to eight
Together.
Specific embodiment 10: being used in step 2 unlike one of present embodiment and specific embodiment one to nine
AFM contact mode carries out delineation 2.5h in ultra hard ceramic material surface.It is other identical as one of specific embodiment one to nine.
Using following experimental verifications effect of the present invention:
Experiment one:
Using AFM diamond probe to ceramic material carry out nanometer striped array processing method according to the following steps into
Row:
One, the preparation of AFM diamond probe:
It is coated with uv-curable glue in the mica upper surface of cleavage, then diamond crystal is dispersed in the mica of cleavage
The AFM probe of no needle point is contacted uv-curable glue, and the surface of mobile diamond crystal in mica surface by upper surface, into
Needle contacts diamond crystal until the AFM probe of no needle point, has the AFM probe of diamond crystal spoke under ultraviolet curing lamp for glutinous
According to 30 minutes, to ultra-violet curing adhesive curing and diamond crystal was firmly adhered on AFM probe, and AFM diamond probe is made；
Two, AFM set voltage value as 10V, pressure 13333nN, scored area be 5 × 5 μm2Under conditions of, it adopts
AFM diamond probe is subjected to 10~60min of delineation on SiC single crystal surface with AFM contact mode, that is, completes to use AFM Buddha's warrior attendant
Stone probe carries out the processing of nanometer striped array to ceramic material.
Three, it will be swept after step 2 delineates treated ultra hard ceramic material clean using the tapping-mode of AFM
It retouches, observes scored area pattern (information such as nanometer width of fringe, depth).
This experiment is in an atmosphere a kind of ultra-fine using the method that AFM diamond probe carries out material removal to SiC single crystal
The method of nanometer striped array processing.After delineating 1h in an atmosphere using AFM diamond probe (AFM contact mode), in SiC table
Face forms (5 × 5 μm of scored area of superfine nano striped array that width is 15nm2).Diamond crystal is used in an atmosphere
The method of SiC single crystal material finish can effectively be removed SiC single crystal skin-material, it is high-efficient and reproducible.
The polish abrasive diamond crystal of use have many advantages, such as it is nontoxic, harmless and from a wealth of sources, polishing environment it is mild, mistake
Journey is safe and pollution-free.The present invention provide a kind of higher material removing rate, process control, low cost ultra hard ceramic material it is super
Thin nanometer striped array structure processing method.
Claims (10)
1. the method for carrying out the processing of nanometer striped array to ceramic material using AFM diamond probe, it is characterised in that use AFM
The method that diamond probe carries out the processing of nanometer striped array to ceramic material follows the steps below:
One, the preparation of AFM diamond probe:
It is coated with uv-curable glue in the mica upper surface of cleavage, diamond crystal is then dispersed in table on the mica of cleavage
The AFM probe of no needle point is contacted uv-curable glue in mica surface, and is moved to the surface of diamond crystal, inserting needle by face
Until the AFM probe contact diamond crystal of no needle point, there is the AFM probe of diamond crystal to irradiate under ultraviolet curing lamp for glutinous
30 minutes, to ultra-violet curing adhesive curing and diamond crystal was firmly adhered on AFM probe, and AFM diamond probe is made；
Two, AFM set voltage value as 2 ~ 10 V, pressure be 2000 ~ 20000 nN, scored area is 5 × 5 μm2Condition
Under, AFM diamond probe is carried out in ultra hard ceramic material surface by delineation 10 min ~ 4.5h using AFM contact mode, obtains item
Line width is completed to carry out nano strip to ceramic material using AFM diamond probe down to the superfine nano striped array of 15 nm
The processing of line array.
2. the method that the processing of nanometer striped array is carried out to ceramic material using AFM diamond probe according to claim 1,
It is characterized in that ultra hard ceramic material described in step 2 is single-crystal silicon carbide, Mohs' hardness is 9.5 grades.
3. the method that the processing of nanometer striped array is carried out to ceramic material using AFM diamond probe according to claim 1,
It is characterized in that ultra hard ceramic material described in step 2 is boron carbide, Mohs' hardness is 9.3 grades.
4. the method that the processing of nanometer striped array is carried out to ceramic material using AFM diamond probe according to claim 1,
It is characterized in that AFM sets voltage value as 3 ~ 9 V in step 2.
5. the method that the processing of nanometer striped array is carried out to ceramic material using AFM diamond probe according to claim 1,
It is characterized in that AFM sets voltage value as 4 ~ 8 V in step 2.
6. the method that the processing of nanometer striped array is carried out to ceramic material using AFM diamond probe according to claim 1,
It is characterized in that AFM sets voltage value as 5 ~ 7 V in step 2.
7. the method that the processing of nanometer striped array is carried out to ceramic material using AFM diamond probe according to claim 1,
It is characterized in that AFM sets voltage value as 6V in step 2.
8. the method that the processing of nanometer striped array is carried out to ceramic material using AFM diamond probe according to claim 1,
It is characterized in that carrying out 10 ~ 60 min of delineation in ultra hard ceramic material surface using AFM contact mode in step 2.
9. the method that the processing of nanometer striped array is carried out to ceramic material using AFM diamond probe according to claim 1,
It is characterized in that carrying out 1.5 ~ 4 h of delineation in ultra hard ceramic material surface using AFM contact mode in step 2.
10. carrying out the side of nanometer striped array processing to ceramic material using AFM diamond probe according to claim 1
Method, it is characterised in that 2.5 h of delineation are carried out in ultra hard ceramic material surface using AFM contact mode in step 2.
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| CN109179313B (en) * | 2018-08-30 | 2020-08-28 | 哈尔滨工业大学 | Preparation method of micro-nanofluidic chip based on AFM |
| CN113466208A (en) * | 2021-07-13 | 2021-10-01 | 哈尔滨工业大学 | Method for preparing Raman substrate by using structured probe |
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| CN101723318A (en) * | 2009-12-03 | 2010-06-09 | 西南交通大学 | Micro-nano manufacturing method for surfaces of quartz and glass materials |
| CN102198927A (en) * | 2011-04-22 | 2011-09-28 | 河南大学 | Method for etching nanometer pattern on surface of crystalline silicon |
| CN105619185A (en) * | 2015-12-30 | 2016-06-01 | 哈尔滨工业大学 | Method for polishing ceramic material partially through artemisinin crystals |
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