CN102891074A - SiC substrate-based graphene CVD (Chemical Vapor Deposition) direct epitaxial growth method and manufactured device - Google Patents
SiC substrate-based graphene CVD (Chemical Vapor Deposition) direct epitaxial growth method and manufactured device Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 58
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000005229 chemical vapour deposition Methods 0.000 title claims description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000004065 semiconductor Substances 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 38
- 239000007789 gas Substances 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 2
- 238000007599 discharging Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 14
- 238000012546 transfer Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 239000010703 silicon Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000003749 cleanliness Effects 0.000 abstract 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 24
- 229910010271 silicon carbide Inorganic materials 0.000 description 23
- 238000011160 research Methods 0.000 description 3
- 238000000407 epitaxy Methods 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
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Abstract
本发明公开了一种基于SiC衬底的石墨烯CVD直接外延生长方法，采用半导体SiC作为衬底，通过对SiC衬底进行合理的预处理，调节生长压力，流量以及温度，在SiC上面直接生长石墨烯，无需金属作为催化剂，生长的石墨烯无需转移过程，便可以直接用于制造各种器件，提高了器件的电学特性，可靠性，降低了器件制造的复杂性。可以生长出具有半导体洁净度的大面积石墨烯材料，可用于无需转移的大面积石墨烯材料的生长制备，并为碳化硅-石墨烯器件的制造提供材料。
The invention discloses a direct epitaxial growth method of graphene CVD based on a SiC substrate. The semiconductor SiC is used as the substrate, and the SiC substrate is properly pretreated to adjust the growth pressure, flow rate and temperature to directly grow on the SiC. Graphene does not require metal as a catalyst, and the grown graphene can be directly used to manufacture various devices without a transfer process, which improves the electrical characteristics and reliability of the device and reduces the complexity of device manufacturing. Large-area graphene materials with semiconductor cleanliness can be grown, which can be used for the growth and preparation of large-area graphene materials without transfer, and provide materials for the manufacture of silicon carbide-graphene devices.
Description
技术领域technical field
本发明属于半导体材料与器件制造技术领域，涉及半导体材料的生长方法，特别是一种半导体碳化硅衬底的石墨烯CVD外延生长方法，可用于无需转移的大面积石墨烯材料的生长制备，并为碳化硅-石墨烯器件的制造提供材料。The invention belongs to the technical field of semiconductor materials and device manufacturing, and relates to a growth method of semiconductor materials, in particular to a graphene CVD epitaxial growth method of a semiconductor silicon carbide substrate, which can be used for the growth and preparation of large-area graphene materials without transfer, and Provide materials for the fabrication of silicon carbide-graphene devices.
背景技术Background technique
石墨烯是一种由碳原子组成的二维晶体，是目前已知最轻最薄的材料，具有非常奇特的物理化学性质，具有突出的产业优势，有望替代Si成为下一代基础半导体材料的新材料。Graphene is a two-dimensional crystal composed of carbon atoms. It is the lightest and thinnest material known so far. It has very peculiar physical and chemical properties and has outstanding industrial advantages. Material.
过渡族金属催化化学气象沉积(CVD)外延是国际上广泛采用的大面积石墨烯制备的方法，它不受衬底尺寸的限制，设备简单，可以大批量生产。但是，CVD外延制备的原生石墨烯下方的金属衬底导电性使得其无法直接应用，必须依赖衬底转移技术，将金属衬底去除然后转移至合适的衬底上，而在转移过程中不可避免地会对石墨烯薄膜产生污染和损坏，影响石墨烯材料和器件的性能。Transition metal-catalyzed chemical vapor deposition (CVD) epitaxy is a method widely used in the world to prepare large-area graphene. It is not limited by the size of the substrate, the equipment is simple, and it can be mass-produced. However, the conductivity of the metal substrate under the native graphene prepared by CVD epitaxy makes it impossible to be directly applied, and the substrate transfer technology must be relied on to remove the metal substrate and then transfer it to a suitable substrate, and it is inevitable in the transfer process The ground will pollute and damage the graphene film, affecting the performance of graphene materials and devices.
碳化硅(SiC)作为一种宽禁带材料，具有良好的电学和热学性能，成为电子研究领域的热门研究课题。可用于制备功率器件、频率器件等。特别是石墨烯发现之后，碳化硅—石墨烯器件结构已经成为研究热点。因此，在碳化硅衬底上直接利用CVD方法外延生长石墨烯，能够减小晶格失配，避免转移过程中残胶引起的性能退化，提高石墨烯和碳化硅衬底接触质量，具有重要的意义。Silicon carbide (SiC), as a wide bandgap material, has good electrical and thermal properties, and has become a hot research topic in the field of electronics research. It can be used to prepare power devices, frequency devices, etc. Especially after the discovery of graphene, the silicon carbide-graphene device structure has become a research hotspot. Therefore, epitaxial growth of graphene directly on SiC substrates by CVD can reduce lattice mismatch, avoid performance degradation caused by residual glue in the transfer process, and improve the contact quality between graphene and SiC substrates, which is of great importance. significance.
发明内容Contents of the invention
本发明的目的在于克服现有大面积石墨烯生长技术中的不足，提出一种基于SiC衬底的无需转移的大面积高质量石墨烯生长方法，以改善石墨烯及器件的电学特性。The purpose of the present invention is to overcome the deficiencies in the existing large-area graphene growth technology, and propose a large-area high-quality graphene growth method based on SiC substrates without transfer, so as to improve the electrical properties of graphene and devices.
实现本发明的技术关键是：采用半导体SiC作为衬底，通过对SiC衬底进行合理的预处理，调节生长压力，流量以及温度，在SiC上面直接生长石墨烯薄膜，无需金属作为催化剂，生长的石墨烯无需转移过程，为碳化硅—石墨烯结构器件提供了材料，可直接用于制造各种器件，提高了器件的电学特性，可靠性，降低了器件制造的复杂性。其生长方法实现步骤包括如下：The technical key to realize the present invention is: use semiconductor SiC as the substrate, and through reasonable pretreatment of the SiC substrate, adjust the growth pressure, flow rate and temperature, and directly grow the graphene film on the SiC without metal as a catalyst. Graphene does not require a transfer process, providing a material for silicon carbide-graphene structural devices, which can be directly used to manufacture various devices, improving the electrical characteristics and reliability of devices, and reducing the complexity of device manufacturing. Its growth method realization steps include as follows:
(1)将SiC衬底先后放入丙酮，乙醇和去离子水中进行清洗，每次时间5～10min，从去离子水中取出衬底，用高纯氮气(99.9999％)吹干。(1) Put the SiC substrate into acetone, ethanol and deionized water successively for cleaning, each time for 5-10 minutes, take out the substrate from the deionized water, and dry it with high-purity nitrogen (99.9999%).
(2)将SiC衬底放入化学气相淀积CVD反应室中，抽取真空至10-5～10-6Torr，以去除反应室内的残留气体；(2) Put the SiC substrate into the chemical vapor deposition CVD reaction chamber, and pump the vacuum to 10 -5 ~ 10 -6 Torr to remove the residual gas in the reaction chamber;
(3)向反应室内通入高纯Ar，温度150～250℃，保持10～30min，然后抽真空至10-5～10-6Torr，排出衬底表面吸附气体。(3) Feed high-purity Ar into the reaction chamber at a temperature of 150-250° C., keep it for 10-30 minutes, and then evacuate to 10 -5 -10 -6 Torr to discharge the adsorbed gas on the substrate surface.
(4)向反应室内通入H2进行衬底表面预处理，气体流量1～20sccm，反应室真空度0.1～1Torr，衬底温度900～1000℃，处理时间1～10min；(4) Introduce H2 into the reaction chamber to pretreat the substrate surface, the gas flow rate is 1-20sccm, the vacuum degree of the reaction chamber is 0.1-1Torr, the substrate temperature is 900-1000°C, and the treatment time is 1-10min;
(5)向反应室中通入H2和CH4，保持H2和CH4的流量比为10∶1～2∶1，H2流量20～200sccm，CH4流量1～20sccm，气压维持在0.1～1atm，温度1000～1300℃，升温时间20～60min，保持时间30～60min；(5) Feed H2 and CH4 into the reaction chamber, keep the flow ratio of H2 and CH4 at 10:1～2:1, H2 flow rate of 20～200sccm, CH4 flow rate of 1～20sccm, and maintain the air pressure at 0.1～1atm, temperature 1000～1300℃, heating time 20～60min, holding time 30～60min;
(6)自然降温，保持工序(5)中的H2和CH4流量不变，气压0.1～1atm，完成石墨烯的生长。(6) Cool down naturally, keep the flow of H2 and CH4 in the process (5) constant, and the air pressure is 0.1-1 atm to complete the growth of graphene.
(7)温度降至100℃以下，关闭CH4、H2，通入Ar，打开反应室，取出样品。(7) When the temperature drops below 100°C, close CH 4 and H 2 , feed Ar, open the reaction chamber, and take out the sample.
本发明具有如下优点：The present invention has the following advantages:
1.由于采用基于碳化硅衬底的常压无催化金属的石墨烯CVD外延生长方法，无需在后续步骤中对石墨烯进行转移，避免了对石墨烯材料的破坏。1. Due to the adoption of the CVD epitaxial growth method of graphene without catalytic metal at atmospheric pressure based on the silicon carbide substrate, there is no need to transfer the graphene in the subsequent steps, and the damage to the graphene material is avoided.
2.由于采用于碳化硅衬底的石墨烯CVD外延生长方法，可以直接在碳化硅衬底上制造石墨烯器件，为碳化硅-石墨烯器件提供材料基础。2. Due to the graphene CVD epitaxial growth method used on silicon carbide substrates, graphene devices can be directly fabricated on silicon carbide substrates, providing a material basis for silicon carbide-graphene devices.
附图说明Description of drawings
图1是本发明的基于SiC衬底的石墨烯生长流程图；Fig. 1 is the graphene growth flowchart based on SiC substrate of the present invention;
图2是本发明的基于SiC衬底的石墨烯生长过程结构示意图。Fig. 2 is a schematic structural diagram of the graphene growth process based on the SiC substrate of the present invention.
具体实施方式Detailed ways
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步的详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定发明。In order to make the object, technical solution and advantages of the present invention more clear, the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the invention.
实施例1在碳化硅衬底上制备石墨烯薄膜。Example 1 A graphene film is prepared on a silicon carbide substrate.
(1)将SiC衬底先后放入丙酮，乙醇和去离子水中进行清洗，每次时间10min，从去离子水中取出衬底，用高纯氮气(99.9999％)吹干。(1) Put the SiC substrate into acetone, ethanol and deionized water successively for cleaning, each time for 10 minutes, take out the substrate from the deionized water, and dry it with high-purity nitrogen (99.9999%).
(2)将SiC衬底放入化学气相淀积CVD反应室中，抽取真空至10-5Torr，以去除反应室内的残留气体；(2) Put the SiC substrate into the chemical vapor deposition CVD reaction chamber, and pump the vacuum to 10 -5 Torr to remove the residual gas in the reaction chamber;
(3)向反应室内通入高纯Ar，温度150℃，保持10min，然后抽真空至10-5Torr，排出衬底表面吸附气体。(3) Feed high-purity Ar into the reaction chamber, keep the temperature at 150°C for 10 minutes, and then evacuate to 10 -5 Torr to discharge the adsorbed gas on the substrate surface.
(4)向反应室内通入H2进行衬底表面预处理，气体流量1sccm，反应室真空度0.1Torr，衬底温度1000℃，处理时间1min；(4) Introduce H2 into the reaction chamber to pretreat the substrate surface, the gas flow rate is 1 sccm, the vacuum degree of the reaction chamber is 0.1 Torr, the substrate temperature is 1000 ° C, and the processing time is 1 min;
(5)向反应室中通入H2和CH4，保持H2和CH4的流量比为10∶1，H2流量20sccm，CH4流量2sccm，气压维持在0.1atm，温度1200℃，升温时间20min，保持时间50min；(5) Feed H 2 and CH 4 into the reaction chamber, keep the flow ratio of H 2 and CH 4 at 10:1, H 2 flow rate 20 sccm, CH 4 flow rate 2 sccm, the air pressure is maintained at 0.1 atm, the temperature is 1200 ° C, and the temperature rises Time 20min, hold time 50min;
(6)自然降温，保持工序(5)中的H2和CH4流量不变，气压0.1atm，完成石墨烯的生长。(6) Cool down naturally, keep the H in the process (5) and CH The flow rate is constant, the air pressure is 0.1 atm, and the growth of graphene is completed.
(7)温度降至100℃以下，关闭CH4、H2，通入Ar，打开反应室，取出样品。(7) When the temperature drops below 100°C, close CH 4 and H 2 , feed Ar, open the reaction chamber, and take out the sample.
实施例2在碳化硅衬底上制备石墨烯薄膜。Example 2 A graphene film is prepared on a silicon carbide substrate.
(1)将SiC衬底先后放入丙酮，乙醇和去离子水中进行清洗，每次时间8min，从去离子水中取出衬底，用高纯氮气(99.9999％)吹干。(1) Put the SiC substrate into acetone, ethanol and deionized water successively for 8 minutes each time, take out the substrate from the deionized water, and dry it with high-purity nitrogen (99.9999%).
(2)将SiC衬底放入化学气相淀积CVD反应室中，抽取真空至10-6Torr，以去除反应室内的残留气体；(2) Put the SiC substrate into the chemical vapor deposition CVD reaction chamber, and pump the vacuum to 10 -6 Torr to remove the residual gas in the reaction chamber;
(3)向反应室内通入高纯Ar，温度250℃，保持30min，然后抽真空至10-6Torr，排出衬底表面吸附气体。(3) Feed high-purity Ar into the reaction chamber, keep the temperature at 250°C for 30 minutes, and then evacuate to 10 -6 Torr to discharge the adsorbed gas on the substrate surface.
(4)向反应室内通入H2进行衬底表面预处理，气体流量20sccm，反应室真空度1Torr，衬底温度1100℃，处理时间10min；(4) Introduce H2 into the reaction chamber to pretreat the substrate surface, the gas flow rate is 20 sccm, the reaction chamber vacuum is 1 Torr, the substrate temperature is 1100 ° C, and the treatment time is 10 min;
(5)向反应室中通入H2和CH4，保持H2和CH4的流量比为2∶1，H2流量200sccm，CH4流量100sccm，气压维持在1atm，温度1200℃，升温时间40min，保持时间40min；(5) Feed H2 and CH4 into the reaction chamber, keep the flow ratio of H2 and CH4 at 2:1, H2 flow rate 200 sccm, CH4 flow rate 100 sccm, air pressure maintained at 1 atm, temperature 1200 ° C, heating time 40min, hold time 40min;
(6)自然降温，保持工序(5)中的H2和CH4流量不变，气压1atm，完成石墨烯的生长。(6) Cool down naturally, keep the H in the operation (5) and CH The flow rate is constant , the air pressure is 1 atm, and the growth of graphene is completed.
(7)温度降至100℃以下，关闭CH4、H2，通入Ar，打开反应室，取出样品。(7) When the temperature drops below 100°C, close CH 4 and H 2 , feed Ar, open the reaction chamber, and take out the sample.
实施例3在碳化硅衬底上制备石墨烯薄膜。Example 3 A graphene film is prepared on a silicon carbide substrate.
(1)将SiC衬底先后放入丙酮，乙醇和去离子水中进行清洗，每次时间5min，从去离子水中取出衬底，用高纯氮气(99.9999％)吹干。(1) Put the SiC substrate into acetone, ethanol and deionized water successively for cleaning, each time for 5 minutes, take out the substrate from the deionized water, and dry it with high-purity nitrogen (99.9999%).
(2)将SiC衬底放入化学气相淀积CVD反应室中，抽取真空至10-6Torr，以去除反应室内的残留气体；(2) Put the SiC substrate into the chemical vapor deposition CVD reaction chamber, and pump the vacuum to 10 -6 Torr to remove the residual gas in the reaction chamber;
(3)向反应室内通入高纯Ar，温度100℃，保持20min，然后抽真空至10-6Torr，排出衬底表面吸附气体。(3) Pass high-purity Ar into the reaction chamber, keep the temperature at 100°C for 20 minutes, and then evacuate to 10 -6 Torr to discharge the adsorbed gas on the substrate surface.
(4)向反应室内通入H2进行衬底表面预处理，气体流量10sccm，反应室真空度0.5Torr，衬底温度1200℃，处理时间50min；(4) Introduce H2 into the reaction chamber to pretreat the substrate surface, the gas flow rate is 10sccm, the vacuum degree of the reaction chamber is 0.5Torr, the substrate temperature is 1200°C, and the treatment time is 50min;
(5)向反应室中通入H2和CH4，保持H2和CH4的流量比为5∶1，H2流量100sccm，CH4流量20sccm，气压维持在0.5atm，温度1300℃，升温时间40min，保持时间50min；(5) Feed H 2 and CH 4 into the reaction chamber, keep the flow ratio of H 2 and CH 4 at 5:1, H 2 flow rate 100 sccm, CH 4 flow rate 20 sccm, air pressure maintained at 0.5 atm, temperature 1300 ° C, heat up Time 40min, hold time 50min;
(6)自然降温，保持工序(5)中的H2和CH4流量不变，气压0.5atm，完成石墨烯的生长。(6) Cool down naturally, keep the H in the operation (5) and CH The flow rate is constant, the air pressure is 0.5atm, and the growth of graphene is completed.
(7)温度降至100℃以下，关闭CH4、H2，通入Ar，打开反应室，取出样品。(7) When the temperature drops below 100°C, close CH 4 and H 2 , feed Ar, open the reaction chamber, and take out the sample.
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention should be included in the protection of the present invention. within range.
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Cited By (7)
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|---|---|---|---|---|
| CN103556217A (en) * | 2013-09-27 | 2014-02-05 | 西安电子科技大学 | Preparation method for 1-5 layer single crystal graphene |
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| CN104409594A (en) * | 2014-11-20 | 2015-03-11 | 北京中科天顺信息技术有限公司 | SiC substrate-based nitride LED (Light Emitting Diode) film flip chip and preparation method thereof |
| CN105990091A (en) * | 2015-01-29 | 2016-10-05 | 中国科学院微电子研究所 | Graphene growth method, graphene layer and semiconductor device |
| WO2016149934A1 (en) * | 2015-03-26 | 2016-09-29 | 中国科学院上海微系统与信息技术研究所 | Growing method for graphene |
| CN107611189A (en) * | 2017-09-08 | 2018-01-19 | 南通强生光电科技有限公司 | Thin film solar cell sheet and preparation method thereof |
| CN109399620A (en) * | 2018-12-05 | 2019-03-01 | 中国电子科技集团公司第十三研究所 | A method of preparing the silicon carbide-based grapheme material of high mobility |
| CN115548115A (en) * | 2022-09-27 | 2022-12-30 | 西安电子科技大学芜湖研究院 | Nitride heterojunction on silicon carbide based on nitrogen-doped graphitization and its preparation method |
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