CN102674317A - C injection-based Ni film assisted SiC substrate graphene nanoribbon preparation method - Google Patents
C injection-based Ni film assisted SiC substrate graphene nanoribbon preparation method Download PDFInfo
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- CN102674317A CN102674317A CN2012101764371A CN201210176437A CN102674317A CN 102674317 A CN102674317 A CN 102674317A CN 2012101764371 A CN2012101764371 A CN 2012101764371A CN 201210176437 A CN201210176437 A CN 201210176437A CN 102674317 A CN102674317 A CN 102674317A
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Abstract
The invention discloses a C injection-based Ni film assisted SiC substrate graphene nanoribbon preparation method. The preparation method comprises the following implementation steps of: performing standard cleaning on a SiC sample wafer; manufacturing a mask plate consisting of isolation ribbons and ion injection ribbons; injecting C ions into an ion injection region in the cleaned SiC sample wafer; holding the SiC sample wafer in an epitaxial furnace, introducing Ar gas, quickly heating to 1,200-1,300 DEG C, keeping the constant temperature for 30-90 minutes and pyrolyzing the SiC of the ion injection region to generate a carbon film; depositing a layer of Ni film on another Si wafer through an electron beam, holding the generated carbon film sample wafer on the Ni film, holding the Si wafer and the carbon film sample wafer in Ar gas together and annealing at the temperature of 900-1,200 DEG C to generate a graphene nanoribbon; and finally, removing the Ni film from the graphene nanoribbon sample wafer and obtaining a nanomaterial consisting of alternate isolation ribbons and graphene nanoribbons on the SiC substrate on the SiC substrate. The preparation method has the advantages of simple process, high safety and low SiC pyrolysis temperature, and the generated graphene nanoribbon has a smooth surface and high continuity and can be used for manufacturing a microelectronic device.
Description
Technical field
The invention belongs to microelectronics technology, relate to semiconductor film material and preparation method thereof, specifically be based on the auxiliary SiC substrate graphene nanobelt preparation method of Ni film that C injects, be used to make microelectronic device.
Technical background
Since the Andre Geim of Britain Manchester university in 2004 and his co-worker Kostya Novoselov use the mechanically peel method to prepare Graphene first; Graphene has promptly caused global sensation, thereby has caused the research boom in fields such as material, Condensed Matter Physics, microelectronics, chemistry.Graphene is by sp
2A kind of carbonaceous novel material of the tightly packed one-tenth bi-dimensional cellular of the monolayer carbon atom shape crystalline network of hydridization, this is to find the thinnest material at present.Because its unique two-dirnentional structure and excellent crystallography quality exist abundant and novel physical phenomenon and excellent physicals in the Graphene.Because these good character, Graphene are expected the acquisition widespread use in fields such as high-performance nano electron device, matrix material, solar cell, field emmision material, ultracapacitors.Therefore, Graphene becomes one of focus of Materials science and Condensed Matter Physics field Recent study rapidly.Scientific circles think that Graphene very likely replaces silicon and becomes following semiconductor material, has extremely wide application prospect.Graphene has caused extensive concern because its excellent electrology characteristic, and the novel method for preparing Graphene then emerges in an endless stream, but uses maximum two kinds of chemical Vapor deposition process and thermolysis SiC methods that mainly contain.
Chemical Vapor deposition process; It is the most widely used a kind of heavy industrialization method of preparation semiconductor film material; It is to utilize carbon compounds such as methane, ethene as carbon source; Through its pyrolytic decomposition growth Graphene, at last with obtaining independently graphene film after the chemical corrosion method removal metal base at matrix surface.The growth of the adjustable Graphenes of parameter such as flow of the type through selecting substrate, the temperature of growth, presoma, like growth velocity, thickness, area etc., the shortcoming of this method is a complicated process of preparation; Energy consumption is big; Cost is higher, accurately controls relatively poorly, and the Graphene lamella that obtains interacts by force with substrate; Lost the character of many single-layer graphenes, and the continuity of Graphene not fine.
Thermolysis SiC method is to make through heat the bond rupture of SiC substrate surface carbon silicon to make the lip-deep Si atom distillation of SiC that residue C atom forms Graphene in former substrate surface reconstruct.Yet temperature is higher during the SiC thermolysis, and the Graphene that grows out is island and distributes, and hole is many, and when making device because photoetching, dry etchings etc. can make the electronic mobility of Graphene reduce, thereby have influenced device performance.
Summary of the invention
The objective of the invention is to deficiency to above-mentioned prior art; A kind of auxiliary SiC substrate graphene nanobelt preparation method of Ni film who injects based on C is proposed; With the graphene nanobelt of growing selectively; Improve graphene nanobelt surface flatness and continuity, avoid simultaneously when postorder is made device, Graphene being carried out the technological process of etching, and the problem that causes electronic mobility to reduce.
For realizing above-mentioned purpose, preparation method of the present invention may further comprise the steps:
(1) the SiC print is cleaned, to remove surface contaminant;
(2) make the mask plate of being made up of isolation strip and ion implantation band, the isolation strip width is: 100-200nm, and ion implantation bandwidth is: 50-200nm;
(3) the ion implantation region injection energy in the SiC print after cleaning is 15-45keV, and dosage is 5 * 10
14~ 5 * 10
16Cm
-2The C ion;
The SiC print that (4) will inject behind the C ion is put into epitaxial furnace, regulates that pressure is 0.5 ~ 1 * 10 in the epitaxial furnace
-6Torr quickly heats up to 1200-1300 ℃, and feeding flow velocity then is the Ar gas of 500-800ml/min, and constant temperature keeps 30 ~ 90min, makes the SiC pyrolysis of ion implantation region generate carbon film;
(5) the Ni film that electron beam deposition 300-500nm is thick on the Si matrix;
(6) the carbon film print that generates is placed on the Ni film, again they together being placed flow velocity is the Ar gas of 30-150ml/min, is 900-1200 ℃ of annealing 10-20min down in temperature, makes carbon film reconstitute graphene nanobelt;
(7) take away the Ni film from the graphene nanobelt print, on the SiC substrate, obtain the nano material that isolation strip and graphene nanobelt are alternately formed each other.
The present invention compared with prior art has following advantage:
1. technology of the present invention is simple, and save energy is safe.
2. the present invention is owing to injected the C ion earlier in the ion implantation band of SiC sample; It is identical with the width that needs the making device to inject bandwidth; The width that is graphene nanobelt equates with the width that needs to make device, has avoided when postorder is made device owing to carrying out the problem that etching causes electronic mobility to reduce to Graphene.
3. the present invention anneals owing to being utilized on the Ni film, thereby the easier reconstruct formation of the carbon film that generates continuity is better, ganoid graphene nanobelt.
Description of drawings
Fig. 1 is the schema that the present invention prepares graphene nanobelt.
Embodiment
With reference to Fig. 1, making method of the present invention provides following three kinds of embodiment.
Embodiment 1
Step 1: clean the 6H-SiC print, to remove surface contaminant.
(1.1) the 6H-SiC substrate base is used NH
4OH+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove the sample surfaces organic residue;
(1.2) the 6H-SiC print that will remove behind the surperficial organic residue re-uses HCl+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove ionic contamination.
Step 2: the width of making device as required makes the mask plate of alternately being made up of each other isolation strip and ion implantation band, and it is 100nm that this instance is selected the isolation strip width for use, and ion implantation bandwidth is 200nm, and this ion implantation bandwidth is identical with the width of device.
Step 3: it is ion implantation that C is carried out in the ion implantation region of 6H-SiC print.
It is 15keV that energy is injected in ion implantation region in the 6H-SiC print after cleaning, and dosage is 5 * 10
14Cm
-2The C ion.
Step 4:6H-SiC pyrolysis generates carbon film.
SiC print behind the injection C ion is put into epitaxial furnace, and pressure is 0.5 * 10 in the adjusting epitaxial furnace
-6Torr quickly heats up to 1200 ℃, and feeding flow velocity then is the Ar gas of 500ml/min, and constant temperature keeps 90min, makes the SiC pyrolysis of ion implantation region generate carbon film.
Step 5: get another Si substrate print and put on the substrate slide glass of electron beam evaporation deposition machine, substrate is 50cm to the distance of target, and reaction chamber pressure is evacuated to 5 * 10
-4Pa, the adjusting line is 40mA, evaporation 10min, the thick Ni film of deposition one deck 300nm on Si substrate print.
Step 6: carbon film reconstitutes graphene nanobelt.
(6.1) the carbon film print that generates is taken out from epitaxial furnace, its carbon film is placed on the thick Ni film of 300nm;
(6.2) carbon film print and Ni film integral body being placed flow velocity is the Ar gas of 30ml/min, is 900 ℃ of annealing 20min down in temperature, and the katalysis through metal Ni makes carbon film reconstitute graphene nanobelt.
Step 7: take away the Ni film from the graphene nanobelt print, on the SiC substrate, obtain the nano material that isolation strip and graphene nanobelt are alternately formed each other.
Embodiment 2
Step 1: clean the 4H-SiC print, to remove surface contaminant.
The 4H-SiC substrate base is used NH earlier
4OH+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove the sample surfaces organic residue; Re-use HCl+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove ionic contamination.
Step 2: the width according to device is made the mask plate of alternately being made up of each other isolation strip and ion implantation band, and promptly ion implantation bandwidth is identical with the width of device, and it is 150nm that this instance is selected the isolation strip width for use, and ion implantation bandwidth is 100nm.
Step 3: it is ion implantation that C is carried out in the ion implantation region of 4H-SiC print.
It is 30keV that energy is injected in ion implantation region in the 4H-SiC print after cleaning, and dosage is 5 * 10
15Cm
-2The C ion;
Step 4: the 4H-SiC pyrolysis generates carbon film.
SiC print behind the injection C ion is put into epitaxial furnace, and pressure is 0.8 * 10 in the adjusting epitaxial furnace
-6Torr quickly heats up to 1250 ℃, and feeding flow velocity then is the Ar gas of 600ml/min, and constant temperature keeps 60min, makes the SiC pyrolysis of ion implantation region generate carbon film;
Step 5: get another Si substrate print and put on the substrate slide glass of electron beam evaporation deposition machine, substrate is 50cm to the distance of target, and reaction chamber pressure is evacuated to 5 * 10
-4Pa, the adjusting line is 40mA, evaporation 15min, the thick Ni film of deposition one deck 400nm on Si substrate print.
Step 6: carbon film reconstitutes graphene nanobelt.
The carbon film print that generates is taken out from epitaxial furnace and places on the thick Ni film of 400nm; Again they together being placed flow velocity is the Ar gas of 100ml/min; In temperature is 1000 ℃ of down annealing 15min, and the katalysis through metal Ni makes carbon film reconstitute graphene nanobelt.
Step 7: take away the Ni film from the graphene nanobelt print, on the SiC substrate, obtain the nano material that isolation strip and graphene nanobelt are alternately formed each other.
Embodiment 3
Steps A: the 6H-SiC substrate base is carried out cleaning surfaces handle, promptly use NH earlier
4OH+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove the sample surfaces organic residue; Re-use HCl+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove ionic contamination.
Step B: the width according to device is made the mask plate of alternately being made up of each other isolation strip and ion implantation band, and it is 200nm that this instance is selected the isolation strip width for use, and ion implantation bandwidth is 50nm, and this ion implantation bandwidth is identical with the width of device.
Step C: it is 45keV that energy is injected in the ion implantation region in the 6H-SiC print after cleaning, and dosage is 5 * 10
16Cm
-2The C ion.
Step D: the SiC print that will inject behind the C ion is put into epitaxial furnace, regulates that pressure is 1 * 10 in the epitaxial furnace
-6Torr quickly heats up to 1300 ℃, and feeding flow velocity then is the Ar gas of 800ml/min, and constant temperature keeps 30min, makes the SiC pyrolysis of ion implantation region generate carbon film.
Step e: get another Si substrate print and put on the substrate slide glass of electron beam evaporation deposition machine, substrate is 50cm to the distance of target, and reaction chamber pressure is evacuated to 5 * 10
-4Pa, the adjusting line is 40mA, evaporation 20min, the thick Ni film of deposition one deck 500nm on Si substrate print.
Step F: the carbon film print that generates is taken out from epitaxial furnace and places on the thick Ni film of 500nm; Again they together being placed flow velocity is the Ar gas of 150ml/min; In temperature is 1200 ℃ of down annealing 10min, and the katalysis through metal Ni makes carbon film reconstitute graphene nanobelt.
Step G: take away the Ni film from the graphene nanobelt print, on the SiC substrate, obtain the nano material that isolation strip and graphene nanobelt are alternately formed each other.
Claims (5)
1. a Ni film that injects based on C is assisted SiC substrate graphene nanobelt preparation method, may further comprise the steps:
(1) the SiC print is cleaned, to remove surface contaminant;
(2) make the mask plate of being made up of isolation strip and ion implantation band, the isolation strip width is: 100-200nm, and ion implantation bandwidth is: 50-200nm;
(3) the ion implantation region injection energy in the SiC print after cleaning is 15-45keV, and dosage is 5 * 10
14~ 5 * 10
16Cm
-2The C ion;
The SiC print that (4) will inject behind the C ion is put into epitaxial furnace, regulates that pressure is 0.5 ~ 1 * 10 in the epitaxial furnace
-6Torr quickly heats up to 1200-1300 ℃, and feeding flow velocity then is the Ar gas of 500-800ml/min, and constant temperature keeps 30 ~ 90min, makes the SiC pyrolysis of ion implantation region generate carbon film;
(5) the Ni film that electron beam deposition 300-500nm is thick on the Si matrix;
(6) the carbon film print that generates is placed on the Ni film, again they together being placed flow velocity is the Ar gas of 30-150ml/min, is 900-1200 ℃ of annealing 10-20min down in temperature, makes carbon film reconstitute graphene nanobelt;
(7) take away the Ni film from the graphene nanobelt print, on the SiC substrate, obtain the nano material that isolation strip and graphene nanobelt are alternately formed each other.
2. the auxiliary SiC substrate graphene nanobelt preparation method of Ni film who injects based on C according to claim 1 is characterized in that said step (1) cleans the SiC print, is to use NH earlier
4OH+H
2O
2Reagent soaked the SiC print 10 minutes, took out the back oven dry, to remove print surface organic residue; Re-use HCl+H
2O
2Reagent soaked print 10 minutes, took out the back oven dry, to remove ionic contamination.
3. the auxiliary SiC substrate graphene nanobelt preparation method of Ni film who injects based on C according to claim 1; It is characterized in that the injection bandwidth in the said step (2); The width of making device with needs is identical, and promptly the width of graphene nanobelt equates with the width that needs to make device.
4. the Ni film auxiliary annealing graphene nanobelt preparation method who injects based on C according to claim 1 is characterized in that electron beam deposition in the said step (5), its processing condition:
Substrate is 50cm to the distance of target,
Reaction chamber pressure is 5 * 10
-4Pa,
Line is 40mA,
Evaporation time is 10-20min.
5. the auxiliary SiC substrate graphene nanobelt preparation method of Ni film who injects based on C according to claim 1 is characterized in that the crystal formation of said SiC print adopts 4H-SiC or 6H-SiC.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963883A (en) * | 2012-10-22 | 2013-03-13 | 武汉大学 | Method for preparing graphene |
| CN105097452A (en) * | 2015-07-07 | 2015-11-25 | 中山大学 | Method for preparing silicon carbide film with micron, submicron and nanometer multilevel structure |
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| CN101602503A (en) * | 2009-07-20 | 2009-12-16 | 西安电子科技大学 | The method of 4H-SiC silicon face extending and growing graphene |
| US20110309336A1 (en) * | 2010-06-18 | 2011-12-22 | Samsung Electronics Co., Ltd. | Semiconducting graphene composition, and electrical device including the same |
| CN102433586A (en) * | 2011-10-02 | 2012-05-02 | 西安电子科技大学 | Method for epitaxial growth of wafer-level graphene on 4H/6H-SiC (0001) surface |
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Patent Citations (3)
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| CN101602503A (en) * | 2009-07-20 | 2009-12-16 | 西安电子科技大学 | The method of 4H-SiC silicon face extending and growing graphene |
| US20110309336A1 (en) * | 2010-06-18 | 2011-12-22 | Samsung Electronics Co., Ltd. | Semiconducting graphene composition, and electrical device including the same |
| CN102433586A (en) * | 2011-10-02 | 2012-05-02 | 西安电子科技大学 | Method for epitaxial growth of wafer-level graphene on 4H/6H-SiC (0001) surface |
Non-Patent Citations (1)
| Title |
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| 廖志宇等: "石墨烯纳米间隙电极对的制备研究进展", 《电子元件与材料》, vol. 30, no. 8, 31 August 2011 (2011-08-31), pages 72 - 75 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963883A (en) * | 2012-10-22 | 2013-03-13 | 武汉大学 | Method for preparing graphene |
| CN105097452A (en) * | 2015-07-07 | 2015-11-25 | 中山大学 | Method for preparing silicon carbide film with micron, submicron and nanometer multilevel structure |
| CN105097452B (en) * | 2015-07-07 | 2017-10-13 | 中山大学 | A kind of preparation method of the carborundum films with micron, sub-micron and nanometer hierarchical structure |
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