CN109234702A - A kind of preparation method of monocrystalline molybdenum disulfide device array - Google Patents
A kind of preparation method of monocrystalline molybdenum disulfide device array Download PDFInfo
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Abstract
A kind of preparation method of monocrystalline molybdenum disulfide device array, first by chemical vapour deposition technique in the continuous polycrystalline molybdenum disulfide of substrate surface growing large-area；It is secondly by etching that molybdenum disulfide is graphical, nucleus array is formed in substrate surface；Later surface is subjected to chemical vapor deposition with the substrate of nucleus array again, monocrystalline molybdenum disulfide is generated at nucleus, the position of monocrystalline molybdenum disulfide growth is accurately controlled by the position of implantation nucleus, forms monocrystalline molybdenum disulfide array；Micro-nano technology technology machined metal electrodes are finally used, single crystal device array is formed；The present invention can avoid by the method for implantation nucleus there are grain boundary defects in molybdenum disulfide device array, and acquisition high quality molybdenum disulfide micro-nano device array lays the foundation for the functionization of molybdenum disulfide device.
Description
Technical field
The present invention relates to MEMS technology field, in particular to a kind of preparation method of monocrystalline molybdenum disulfide device array is led to
It crosses implantation nucleus and realizes that the growth position per a piece of monocrystalline molybdenum disulfide is controllable, to avoid in device that there are grain boundary defects, obtain
Obtain high quality molybdenum disulfide device array.
Background technique
The unique material property of two-dimensional material molybdenum disulfide determines that it is logical in biotechnology, medical treatment, environmental monitoring, intelligence
The multiple fields such as letter, aerospace, artificial intelligence have important research and application prospect.The preparation method of molybdenum disulfide is led at present
There are mechanical stripping method, solwution method, chemical vapour deposition technique.The wherein molybdenum disulfide sample of mechanical stripping method and solwution method preparation
Size is minimum, only micron dimension, it is difficult to realize extensive practical；Chemical vapour deposition technique (Fig. 1) can prepare large area two
Molybdenum sulfide has practical potentiality.
Grain boundary defects are the main bottleneck (Fig. 2) of the two-dimensional materials such as current chemical vapour deposition technique growth molybdenum disulfide, ginseng
See document (Science, 2014,34,286-289).Be randomly formed nucleus in molybdenum disulfide growth course first, nuclei growth at
For monocrystalline, monocrystalline, which continues to grow up, is connected to become the complete molybdenum disulfide of large area.Since the crystal orientation between adjacent nucleus is in the presence of poor
It is different, lead to grain boundary defects occur after final monocrystalline connection.So at present using the large area two of chemical vapour deposition technique preparation
Molybdenum sulfide is polycrystalline structure.The preparation of large area (wafer scale) monocrystalline molybdenum disulfide is not possible to realize at present.
Grain boundary defects make the material properties such as the electricity of molybdenum disulfide, machinery seriously degenerate.Since nucleus is in chemical vapor deposition
It is random during product to occur, cause the position Arbitrary distribution of finally formed crystal boundary, therefore difficult when processing micro-nano device array
To avoid grain boundary defects.Grain boundary defects cause the performance of micro-nano device to be remarkably decreased, and greatly reduce molybdenum disulfide and lead in MEMS
The practical value in domain.Therefore how in molybdenum disulfide micro-nano device grain boundary defects are avoided, realizes extensive monocrystalline molybdenum disulfide
Device array is a problem of urgent need to resolve.
Summary of the invention
In order to overcome the defects of the prior art described above, the purpose of the present invention is to provide a kind of monocrystalline molybdenum disulfide device battle arrays
The preparation method of column breaks through the thinking of conventional growth molybdenum disulfide, the nucleus for replacing nature to be randomly formed using artificial nucleus, energy
Enough accurate positions for controlling the growth per a piece of monocrystalline molybdenum disulfide, making the molybdenum disulfide in prepared device array is monocrystalline knot
Structure avoids grain boundary defects in molybdenum disulfide micro-nano device array.
In order to achieve the above object, the present invention is realized by the following method:
A kind of preparation method of monocrystalline molybdenum disulfide device array, preparation step is successively are as follows:
(1) first by chemical vapour deposition technique in the continuous polycrystalline molybdenum disulfide of substrate surface growing large-area, with true
Pressure in quartzy furnace is evacuated to 10mTorr by sky pump, is then passed through argon gas into quartzy furnace, and 500-700 degrees Celsius of growth temperature,
Growth time 10-30 minutes, the molybdenum disulfide was two-dimensional material, i.e., thickness direction only has single layer atom or a small number of several layers of originals
Son；
(2) the continuous polycrystalline molybdenum disulfide of the large area of generation is graphical by the method for dry etching, in substrate table
Face forms nucleus array, and the oxygen pressure that dry etching uses is 10-15Pa, flow velocity 50-100sccm, power 50-100W, quarter
Erosion time 2-5 minutes；
(3) surface is subjected to chemical vapor deposition with the substrate of nucleus array again, it will be in quartzy furnace with vacuum pump
Pressure is evacuated to 10mTorr, argon gas is then passed through into quartzy furnace, 500-700 degrees Celsius of growth temperature, growth time 2-10 divides
Clock, monocrystalline molybdenum disulfide is only grown in the position of implantation nucleus, therefore the position of monocrystalline molybdenum disulfide growth is by implantation nucleus
Position determines, forms monocrystalline molybdenum disulfide array；
(4) micro-nano technology technology machined metal electrodes are used, monocrystalline molybdenum disulfide device array is formed.
The continuous polycrystalline molybdenum disulfide thickness direction of large area described in step (1) only has single layer atom or a small number of several layers of originals
Son, a small number of several layers of atoms are not more than 10 layers.
Nucleus diameter in nucleus array described in step (2) is 0.2-2 microns, and nucleus spacing is 10-100 microns.
The monocrystalline molybdenum disulfide for carrying out chemical vapor deposition growth described in step (3) again is that single layer or minority are several layers of,
A small number of several layers of atoms are not more than 10 layers.
Metal electrode described in step (4) is formed in table in substrate using the step of electron beam lithography, metal deposit, removing
Face, metal deposit is by sputtering, vapor deposition or other methods, and wherein metal material is selected any one in Au, Ag, Cu, Al, Pt
Kind.
The maximum problem that two-dimensional material molybdenum disulfide functionization encounters is: grain boundary defects make the performance of micro-nano device sharply
It reduces, and grain boundary defects are extremely difficult during Material growth and device fabrication avoids.The beneficial effects of the present invention are: can be real
Existing monocrystalline molybdenum disulfide micro-nano device array, avoids in device that there are grain boundary defects, is obviously improved molybdenum disulfide micro-nano device
Performance lays the foundation for the functionization of molybdenum disulfide device.
Detailed description of the invention
Fig. 1 is the schematic device that chemical vapour deposition technique grows molybdenum disulfide.
Fig. 2 be the two-dimensional materials such as chemical vapour deposition technique growing large-area molybdenum disulfide process schematic (Science,
2014,34,286-289) it, is initially formed nucleus, nuclei growth becomes monocrystalline, and monocrystalline continues to grow up, and connects into large-area polycrystalline
Two-dimensional material.
Fig. 3 is that monocrystalline molybdenum disulfide array of the invention prepares schematic diagram, first in substrate surface growing large-area monocrystalline
Then molybdenum disulfide is etched into nucleus shape, then is carried out second of chemical vapor deposition growth, two sulphur of monocrystalline is formed
Change molybdenum array.
Fig. 4 is monocrystalline molybdenum disulfide micro-nano device array flow process chart of the invention.
Fig. 5 is monocrystalline molybdenum disulfide micro-nano device array schematic diagram of the invention.
Specific embodiment
Technical scheme is described further with reference to the accompanying drawings and embodiments.
Embodiment one
A kind of preparation method of monocrystalline molybdenum disulfide device array, preparation step is successively are as follows:
(1) growing large-area molybdenum disulfide
Referring to Fig.1, using chemical vapour deposition technique, using argon gas as carrier gas, in SiO under high temperature, environment under low pressure2Surface growth
Large area molybdenum disulfide.First by molybdenum disulfide powder and SiO2/ Si substrate is put into quartzy furnace.It will be in quartzy furnace with vacuum pump
Pressure be evacuated to 10mTorr, be then passed through argon gas into quartzy furnace, 600 degrees Celsius of growth temperature, growth time 20 minutes.Material
Expect in preparation process, the molybdenum disulfide molecule that blocky molybdenum disulfide gasification generates is carried by argon gas to SiO2/Si substrate surface, and
Form nucleus.Nucleus continued growth forms monocrystalline and is finally connected to become polycrystalline molybdenum disulfide, referring to Fig. 2.The molybdenum disulfide
For two-dimensional material, i.e. thickness direction only has single layer atom or a small number of several layers of atoms.
(2) nucleus array is formed
Substrate surface is cleaned, and is dried up with nitrogen using acetone, isopropanol first.It is negative at one layer of substrate surface spin coating
Property electron beam resist AR-N7520.073 (spin coating machine speed 1000-4000RPM, time 30-60 second), heats 1 on hot plate
Minute (80-100 DEG C).Pass through electron beam exposure (exposure dose 80-100 μ C/cm2), development (impregnated in AR300-47 developer solution
1-2 minutes) make photoetching offset plate figure.The molybdenum disulfide of glue protection will be photo-etched using argon plasma dry etching technology
Graphical (the general of molybdenum disulfide is realized in removal (oxygen pressure 13Pa, flow velocity 80sccm, power 80W, etch period 4 minutes)
Molybdenum disulfide is etched into nucleus shape, nucleus diameter 200-2000nm).Sample is impregnated to 5-10 points in acetone after dry etching
Clock removes photoresist.
(3) monocrystalline molybdenum disulfide array is grown
Referring to Fig. 3, the substrate with nucleus is placed again into quartzy furnace and carries out chemical vapor deposition growth.Growth temperature
Degree, pressure, the parameters such as gas flow are identical as first time growing large-area molybdenum disulfide before.Due to the defective bit of substrate surface
It sets and is easier to capture molybdenum disulfide molecule, therefore being implanted into nucleus method is substantially by introducing stronger " defect ", with SiO2/ Si base
The defect of bottom surface itself forms the competition mechanism of contention molybdenum disulfide molecule.Final result causes molybdenum disulfide to be only present in plant
At the nucleus entered.The growth position of every a piece of monocrystalline molybdenum disulfide is accurately controlled by being implanted into nucleus.By controlling growth time 8
Minute, it 600 degrees Celsius of growth temperature, stops growing before the interconnection of adjacent single crystalline molybdenum disulfide, obtains monocrystalline curing
Molybdenum array.
(4) monocrystalline molybdenum disulfide device array is processed
Referring to Fig. 4, by common photoetching, metal deposit, removing technique in SiO2/ Si substrate surface processes Subsequent electronic
The centering of beam photoetching marks.Photoetching uses AZ601 positive photoresist, spin coating machine speed 1000-4000RPM, time 30-90 second.
After gluing on hot plate 100-120 DEG C heating 1-2 minutes.Expose 90-100s, after exposure on hot plate 100-120 DEG C plus
Heat 2 minutes.Develop 90-100s in 318 developer solutions.Metal deposit grows 10 nano-titaniums using magnetron sputtering technique and 50-100 receives
The gold of meter Hou Du.Stripping technology, by the metal removal above photoresist and photoresist, makes metallic layer graphic using acetone.
Referring to Fig. 5, in SiO2One layer of positive electronic beam photoresist (spin coating machine speed 1000- of/Si substrate surface spin coating
4000RPM, time 30-90 second), 80-100 DEG C heating 1-2 minutes on hot plate.Make its figure by electron beam exposure and development
Change.Using the gold of magnetron sputtering technique growth 10 nano-titaniums and 50-100 nano thickness.Sample is impregnated in acetone, and is assisted
With sonic oscillation, it is therefore intended that removal photoresist and the metal (stripping technology) of photoresist surface attachment.Pass through stripping technology
It realizes the graphical of metal layer, forms the metal electrode of molybdenum disulfide micro-nano device.Each monocrystalline molybdenum disulfide device is corresponding
Two metal electrodes.
The triangle monocrystalline molybdenum disulfide in device is etched into needed for device by common photoetching, argon gas dry etching
Rectangle.Photoetching uses AZ601 positive photoresist, spin coating machine speed 1000-4000RPM, time 30-90 second.In heat after gluing
100-120 DEG C heating 1-2 minutes on plate.Expose 90-100s, after exposure on hot plate 100-120 DEG C heat 2 minutes.318 is aobvious
Develop 90-100s in shadow liquid.
Embodiment two
A kind of preparation method of monocrystalline molybdenum disulfide device array, preparation step is successively are as follows:
(1) first by chemical vapour deposition technique in the continuous polycrystalline molybdenum disulfide of substrate surface growing large-area, with true
Pressure in quartzy furnace is evacuated to 10mTorr by sky pump, and argon gas is then passed through into quartzy furnace, 500 degrees Celsius of growth temperature, is grown
Time 10 minutes, the molybdenum disulfide was two-dimensional material, i.e., thickness direction only has single layer atom or a small number of several layers of atoms；
(2) the continuous polycrystalline molybdenum disulfide of the large area of generation is graphical by the method for dry etching, in substrate table
Face forms nucleus array, and the oxygen pressure that dry etching uses is 10Pa, flow velocity 50sccm, power 50W, etch period 2 minutes；
(3) surface is subjected to chemical vapor deposition with the substrate of nucleus array again, it will be in quartzy furnace with vacuum pump
Pressure is evacuated to 10mTorr, is then passed through argon gas into quartzy furnace, and 500 degrees Celsius of growth temperature, growth time 2 minutes, monocrystalline two
Molybdenum sulfide is only grown in the position of implantation nucleus, therefore the position of monocrystalline molybdenum disulfide growth is determined by the position of implantation nucleus,
Form monocrystalline molybdenum disulfide array；
(4) micro-nano technology technology machined metal electrodes are used, monocrystalline molybdenum disulfide device array is formed.
Embodiment three
A kind of preparation method of monocrystalline molybdenum disulfide device array, preparation step is successively are as follows:
(1) first by chemical vapour deposition technique in the continuous polycrystalline molybdenum disulfide of substrate surface growing large-area, with true
Pressure in quartzy furnace is evacuated to 10mTorr by sky pump, and argon gas is then passed through into quartzy furnace, 700 degrees Celsius of growth temperature, is grown
Time 30 minutes, the molybdenum disulfide was two-dimensional material, i.e., thickness direction only has single layer atom or a small number of several layers of atoms；
(2) the continuous polycrystalline molybdenum disulfide of the large area of generation is graphical by the method for dry etching, in substrate table
Face forms nucleus array, and the oxygen pressure that dry etching uses divides for 15Pa, flow velocity 100sccm, power 100W, etch period 5
Clock；
(3) surface is subjected to chemical vapor deposition with the substrate of nucleus array again, it will be in quartzy furnace with vacuum pump
Pressure is evacuated to 10mTorr, is then passed through argon gas into quartzy furnace, and 700 degrees Celsius of growth temperature, growth time 10 minutes, monocrystalline
Molybdenum disulfide is only grown in the position of implantation nucleus, therefore the position of monocrystalline molybdenum disulfide growth is true by the position of implantation nucleus
It is fixed, form monocrystalline molybdenum disulfide array；
(4) micro-nano technology technology machined metal electrodes are used, monocrystalline molybdenum disulfide device array is formed.
Claims (5)
1. a kind of preparation method of monocrystalline molybdenum disulfide device array, which is characterized in that its preparation step is successively are as follows:
(1) first by chemical vapour deposition technique in the continuous polycrystalline molybdenum disulfide of substrate surface growing large-area, vacuum pump is used
Pressure in quartzy furnace is evacuated to 10mTorr, argon gas is then passed through into quartzy furnace, 500-700 degrees Celsius of growth temperature, is grown
Time 10-30 minute, the molybdenum disulfide are two-dimensional material, i.e., thickness direction only has single layer atom or a small number of several layers of atoms；
(2) the continuous polycrystalline molybdenum disulfide of the large area of generation is graphical by the method for dry etching, in substrate surface shape
At nucleus array, when the oxygen pressure that dry etching uses is 10-15Pa, flow velocity 50-100sccm, power 50-100W, etching
Between 2-5 minutes；
(3) surface is subjected to chemical vapor deposition with the substrate of nucleus array again, with vacuum pump by the pressure in quartzy furnace
It is evacuated to 10mTorr, argon gas is then passed through into quartzy furnace, it is 500-700 degrees Celsius of growth temperature, growth time 2-10 minutes, single
Brilliant molybdenum disulfide is only grown in the position of implantation nucleus, therefore the position of monocrystalline molybdenum disulfide growth is true by the position of implantation nucleus
It is fixed, form monocrystalline molybdenum disulfide array；
(4) micro-nano technology technology machined metal electrodes are used, monocrystalline molybdenum disulfide device array is formed.
2. a kind of preparation method of monocrystalline molybdenum disulfide device array according to claim 1, which is characterized in that step
(1) the continuous polycrystalline molybdenum disulfide thickness direction of large area described in only has single layer atom or a small number of several layers of atoms, a small number of several layers of
Atom is not more than 10 layers.
3. a kind of preparation method of monocrystalline molybdenum disulfide device array according to claim 1, which is characterized in that step
(2) the nucleus diameter in nucleus array described in is 0.2-2 microns, and nucleus spacing is 10-100 microns.
4. a kind of preparation method of monocrystalline molybdenum disulfide device array according to claim 1, which is characterized in that step
(3) the monocrystalline molybdenum disulfide for carrying out chemical vapor deposition growth again described in is single layer or a small number of several layers of, a small number of several layers of atoms
To be not more than 10 layers.
5. a kind of preparation method of monocrystalline molybdenum disulfide device array according to claim 1, which is characterized in that step
(4) metal electrode described in is formed in upper surface of substrate, metal deposit using the step of electron beam lithography, metal deposit, removing
By sputtering or being deposited, wherein metal material selects any one in Au, Ag, Cu, Al, Pt.
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