CN102931077A - Annealing process of zinc oxide substrate transfer graphene and manufactured device - Google Patents
Annealing process of zinc oxide substrate transfer graphene and manufactured device Download PDFInfo
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- CN102931077A CN102931077A CN2012104081992A CN201210408199A CN102931077A CN 102931077 A CN102931077 A CN 102931077A CN 2012104081992 A CN2012104081992 A CN 2012104081992A CN 201210408199 A CN201210408199 A CN 201210408199A CN 102931077 A CN102931077 A CN 102931077A
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Abstract
The invention discloses an annealing process of zinc oxide substrate transfer graphene. By adopting a high-temperature annealing mode, graphene defect generated in a substrate transfer process is repaired, and impurities which can not be removed in a transfer process or are newly introduced are further removed. Meanwhile, the high-temperature annealing can ensure that the contact of the substrate and the graphene is improved, an expected substrate influence is established, and a forbidden band is introduced in the graphene. Finally, the surface of the transferred graphene is cleaner, the defects are less, and the flat graphene is in better contact with the SiC substrate. Because lower-temperature annealing is adopted in an Ar atmosphere, thus water molecules and other impurities absorbed on the surface of the graphene are effectively removed; and because a high-annealing temperature of higher than 1000 DEG C is adopted, effective contact of the graphene attached on the substrate and the SiC substrate is formed.
Description
Technical field
The invention belongs to technical field of semiconductors, relate to the method for annealing that Graphene is transferred to Semiconductor substrate, a kind of method for annealing based on the SiC substrate particularly can change by transferring to annealing behind the substrate character of grapheme material.
Background technology
The IC industry of being ruled by Moore's Law has obtained development at full speed in the past few decades, integrated circuit (IC) design manufacturing industry take Si as foundation stone has been created the per mythology that turned in 18 months of integration density, for social development provides positive contribution difficult to the appraisal.Continuous progress along with Si base technique, integrated circuit (IC) design manufacturing take CMOS as design cell has welcome bottleneck period, Moore's Law continue to be subject to the lot of challenges such as photoetching process, quantum effect, energy consumption, scientist wishes to find a kind of substitution material can replenish even replace Si as the integrated circuit basic material, Graphene is as a kind of emerging two-dimensional material, once occurring having caused that interest is paid close attention to widely.The mobility of Graphene at room temperature can reach 200000cm-2v-1s-1, has the great potential of making high speed device.Have simultaneously very high thermal conductivity, be higher than the thermal conductivity of copper far away, even be higher than diamond.
Although yet grapheme material has above-described many merits, this special material has lacked an important common trait---the forbidden band of ordinary semiconductor material.Grapheme material does not have the forbidden band, and having limited mixes regulates the ability of Graphene electrical properties.What is more, owing to there not being the forbidden band, the device that Graphene is made can not turn-off, and brings into play high speed characteristics for Graphene in digital circuit and is provided with obstacle.In order to make Graphene have the forbidden band, people have invented some methods, for example utilize the wave function confinement to make graphene nanobelt, make double-layer graphite alkene, apply uniaxial strain and introduce the ways such as forbidden band.Unfortunately, because the preparation means of nanobelt, double-layer graphite alkene is complicated, be difficult to realize large-scale application.A feasible method is by regulating substrate the forbidden band to be opened in the impact of upper layer graphene.
Yet, use conventional transfer method to transfer to Graphene defective on the general substrate and contact poorly more, be difficult to Graphene is formed effective influence, therefore be badly in need of a kind of suitable transfer post-processing approach of invention.
Summary of the invention
The object of the invention is to use suitable annealing process to set up the SiC substrate to the impact of Graphene, and then in Graphene, introduce the forbidden band, ready for making the Digital Logic turn-off device, a kind of transfer after annealing method of improving substrate contact is provided.
Realize that the object of the invention key problem in technology is: adopt the mode of high annealing, repair the Graphene defective that produces in the substrate-transfer process, further remove the impurity removing or newly introduce of failing in the transfer process.Simultaneously, high annealing can also make substrate contact with Graphene and improve, and sets up the substrate effect of expection, introduces the forbidden band in Graphene.
Performing step of the present invention comprises as follows: a kind of annealing process of SiC substrate-transfer Graphene, adopt the mode of high annealing, and repair the Graphene defective that produces in the substrate-transfer process, further remove the impurity removing or newly introduce of failing in the transfer process; High annealing is introduced the forbidden band in Graphene simultaneously.
Further, described annealing process performing step is as follows:
Copper Foil is placed in the reative cell, passes into H to reative cell
2, Copper Foil is processed;
Pass into Ar and CH to reative cell
4
At Fe (NOX)
3Soak 30-60min in the aqueous solution, use the GaN substrate to salvage, heat 60min in air, temperature remains on 150-200 ℃;
Put into acetone and soak 24 hours thoroughly residual PMMA of removal;
Use respectively absolute ethyl alcohol and rinsed with deionized water, high-purity N
2Dry up;
Reative cell vacuumizes, and passes into Ar gas again, air pressure 0.01-0.1Torr, and temperature rises to 100-200 ℃, keeps 30-40min;
Pass into again Ar and H
2Gaseous mixture, mixed proportion is 10: 1-1: 1, air pressure maintains 0.01-0.1Torr, annealing temperature is 1000-1100 ℃, annealing time 1-2h.
Further, Copper Foil is placed in the reative cell, passes into H to reative cell
2, Copper Foil is processed flow 1-20sccm, temperature 900-1000 ℃, time 20-60min, air pressure 1-50Torr;
Further, pass into Ar and CH to reative cell
4, keep Ar and CH
4Flow-rate ratio be 10: 1-2: 1, Ar flow 20-200sccm, CH
4Flow 1-20sccm, air pressure maintains 0.1-1Torr, and temperature 900-1100 ℃, intensification and retention time be 20-60min altogether;
Further, at 0.05g/m1-0.15g/m1 Fe (NO
4)
3Soak 30-60min in the aqueous solution, use the GaN substrate to salvage, heat 60min in air, temperature remains on 150-200 ℃.
Further, pass into again Ar and H
2Gaseous mixture, mixed proportion is 10: 1-1: 1, air pressure maintains 0.01-0.1Torr, annealing temperature is 1000-1100 ℃, annealing time 1-2h.
The device the present invention who another object of the present invention is to provide a kind of annealing process that utilizes above-mentioned SiC substrate-transfer Graphene to manufacture has following advantage:
1. owing to adopting lower temperature annealing in Ar gas atmosphere, effectively remove hydrone and other impurity molecules of Graphene adsorption.
2. owing to adopting and to be higher than 1000 ℃ high annealing temperature, formed and adhere to Graphene on the substrate and contact with the effective of SiC substrate.
Description of drawings
Fig. 1 is Graphene annealing flow chart on the SiC substrate of the present invention;
Fig. 2 is the annealing tube furnace of Graphene annealing on the SiC substrate of the present invention.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
With reference to Fig. 1,2, the present invention provides following embodiment:
Embodiment 1:
Performing step of the present invention is as follows:
Step 1, the high-temperature process Copper Foil.
Copper Foil is placed in the reative cell, passes into H to reative cell
2, Copper Foil is processed flow 5sccm, 900 ℃ of temperature, time 60min, air pressure 15Torr
Step 2, CVD growth Graphene.
Pass into Ar and CH to reative cell
4, keep Ar and CH
4Flow-rate ratio be 10: 1, Ar flow 200sccm, CH
4Flow 20sccm, air pressure maintains 1Torr, and 900 ℃ of temperature heat up and the retention time is total to 20min.
Step 3, corrosion Cu substrate.
At Fe (NO
4) the middle 30min that soaks of the X aqueous solution (0.15g/ml), use the SiC substrate to salvage, in air, heat 60min, temperature remains on 150 ℃.
Step 4 is removed surface organic matter.
Put into acetone and soak 24 hours thoroughly residual PMMA of removal.
Step 5 is used respectively absolute ethyl alcohol and rinsed with deionized water, high-purity N
2Dry up.
Step 6 is removed reative cell steam.
Reative cell vacuumizes, and passes into Ar gas again, air pressure 0.1Torr, and temperature rises to 160 ℃, keeps 40min.
Step 7, high annealing.
Pass into again Ar and H
2Gaseous mixture, mixed proportion is 10: 1, air pressure maintains 0.1Torr, annealing temperature is 700 ℃, annealing time 2h.
Embodiment 2:
Performing step of the present invention is as follows:
Steps A, the high-temperature process Copper Foil.
Copper Foil is placed in the reative cell, passes into H to reative cell
2, Copper Foil is processed flow 10sccm, 950 ℃ of temperature, time 40min, air pressure 25Torr
Step B, CVD growth Graphene.
Pass into Ar and CH to reative cell
4, keep Ar and CH
4Flow-rate ratio be 5: 1, Ar flow 100sccm, CH
4Flow 20sccm, air pressure maintains 1Torr, and 950 ℃ of temperature heat up and the retention time is total to 40min.
Step C, corrosion Cu substrate.
At Fe (NO
4)
3Soak 40min in the aqueous solution (0.1g/ml), use the SiC substrate to salvage, heat 60min in air, temperature remains on 200 ℃.
Step D removes surface organic matter.
Put into acetone and soak 24 hours thoroughly residual PMMA of removal.
Step e is used respectively absolute ethyl alcohol and rinsed with deionized water, high-purity N
2Dry up.
Step F is removed reative cell steam.
Reative cell vacuumizes, and passes into Ar gas again, air pressure 0.06Torr, and temperature rises to 170 ℃, keeps 30min.
Step G, high annealing.
Pass into again Ar and H
2Gaseous mixture, mixed proportion is 7: 1, air pressure maintains 0.07Torr, annealing temperature is 800 ℃, annealing time 1.5h.
Embodiment 3:
Performing step of the present invention is as follows:
Step 1, the high-temperature process Copper Foil.
Copper Foil is placed in the reative cell, passes into H to reative cell
2, Copper Foil is processed flow 20sccm, 1000 ℃ of temperature, time 20min, air pressure 50Torr
Step 2, CVD growth Graphene.
Pass into Ar and CH to reative cell
4, keep Ar and CH
4Flow-rate ratio be 3: 1, Ar flow 180sccm, CH
4Flow 60sccm, air pressure maintains 1Torr, and 1100 ℃ of temperature heat up and the retention time is total to 20min.
Step 3, corrosion Cu substrate.
At Fe (NO
4)
3Soak 30min in the aqueous solution (0.15g/ml), use the SiC substrate to salvage, heat 60min in air, temperature remains on 160 ℃.
Step 4 is removed surface organic matter.
Put into acetone and soak 24 hours thoroughly residual PMMA of removal.
Step 5 is used respectively absolute ethyl alcohol and rinsed with deionized water, high-purity N
2Dry up.
Step 6 is removed reative cell steam.
Reative cell vacuumizes, and passes into Ar gas again, air pressure 0.1Torr, and temperature rises to 200 ℃, keeps 30-40min.
Step 7, high annealing.
Pass into again Ar and H
2Gaseous mixture, mixed proportion is 3: 1, air pressure maintains 0.1Torr, annealing temperature is 900 ℃, annealing time 2h.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. the annealing process of a SiC substrate-transfer Graphene is characterized in that,
Adopt the mode of high annealing, repair the Graphene defective that produces in the substrate-transfer process, further remove the impurity removing or newly introduce of failing in the transfer process; High annealing is introduced the forbidden band in Graphene simultaneously.
2. annealing process as claimed in claim 1 is characterized in that, described annealing process performing step is as follows:
(1) Copper Foil is placed in the reative cell, passes into H to reative cell
2, Copper Foil is processed;
(2) pass into Ar and CH to reative cell
4
(3) at Fe (NO
4)
3Soak 30-60min in the aqueous solution, use the GaN substrate to salvage, heat 60min in air, temperature remains on 150-200 ℃;
(4) put into acetone and soak 24 hours thoroughly residual PMMA of removal;
(5) use respectively absolute ethyl alcohol and rinsed with deionized water, high-purity N
2Dry up;
(6) reative cell vacuumizes, and passes into Ar gas again, air pressure 0.01-0.1Torr, and temperature rises to 100-200 ℃, keeps 30-40min;
(7) pass into again Ar and H
2Gaseous mixture, annealing.
3. annealing process as claimed in claim 1 is characterized in that, Copper Foil is placed in the reative cell, passes into H to reative cell
2, Copper Foil is processed flow 1-20sccm, temperature 900-1000 ℃, time 20-60min, air pressure 1-50Torr.
4. annealing process as claimed in claim 1 is characterized in that, passes into Ar and CH to reative cell
4, keep Ar and CH
4Flow-rate ratio be 10: 1-2: 1, Ar flow 20-200sccm, CH
4Flow 1-20sccm, air pressure maintains 0.1-1Torr, and temperature 900-1100 ℃, intensification and retention time be 20-60min altogether;
5. annealing process as claimed in claim 1 is characterized in that, at 0.05g/ml-0.15g/mlFe (NO
4)
3Soak 30-60min in the aqueous solution, use the GaN substrate to salvage, heat 60min in air, temperature remains on 150-200 ℃.
6. annealing process as claimed in claim 1 is characterized in that, passes into Ar and H again
2Gaseous mixture, mixed proportion is 10: 1-1: 1, air pressure maintains 0.01-0.1Torr, annealing temperature is 1000-1100 ℃, annealing time 1-2h.
7. device that the annealing process that utilizes SiC substrate-transfer Graphene claimed in claim 1 is manufactured.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046247A (en) * | 2017-12-25 | 2018-05-18 | 中国电子科技集团公司第五十五研究所 | The method for improving carborundum pyrolytic graphite alkene thin layer number uniformity |
| CN113555497A (en) * | 2021-06-09 | 2021-10-26 | 浙江芯国半导体有限公司 | High-mobility SiC-based graphene device and preparation method thereof |
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| CN102134067A (en) * | 2011-04-18 | 2011-07-27 | 北京大学 | Method for preparing single-layer graphene |
| CN102351175A (en) * | 2011-11-03 | 2012-02-15 | 东南大学 | High-quality transfer method of graphene prepared by chemical vapor deposition method |
| CN102400109A (en) * | 2011-11-11 | 2012-04-04 | 南京航空航天大学 | Method for growing large area of layer-number-controllable graphene at low temperature through chemical vapor deposition (CVD) method by using polystyrene solid state carbon source |
| CN102433544A (en) * | 2012-01-11 | 2012-05-02 | 中国科学院上海微系统与信息技术研究所 | Method for growing large-area graphene by utilizing multi-benzene-ring carbon source low-temperature chemical vapor deposition |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134067A (en) * | 2011-04-18 | 2011-07-27 | 北京大学 | Method for preparing single-layer graphene |
| CN102351175A (en) * | 2011-11-03 | 2012-02-15 | 东南大学 | High-quality transfer method of graphene prepared by chemical vapor deposition method |
| CN102400109A (en) * | 2011-11-11 | 2012-04-04 | 南京航空航天大学 | Method for growing large area of layer-number-controllable graphene at low temperature through chemical vapor deposition (CVD) method by using polystyrene solid state carbon source |
| CN102433544A (en) * | 2012-01-11 | 2012-05-02 | 中国科学院上海微系统与信息技术研究所 | Method for growing large-area graphene by utilizing multi-benzene-ring carbon source low-temperature chemical vapor deposition |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046247A (en) * | 2017-12-25 | 2018-05-18 | 中国电子科技集团公司第五十五研究所 | The method for improving carborundum pyrolytic graphite alkene thin layer number uniformity |
| CN113555497A (en) * | 2021-06-09 | 2021-10-26 | 浙江芯国半导体有限公司 | High-mobility SiC-based graphene device and preparation method thereof |
| CN113555497B (en) * | 2021-06-09 | 2023-12-29 | 浙江芯科半导体有限公司 | SiC-based graphene device with high mobility and preparation method thereof |
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