CN114774846A - 一种n掺杂c膜的制备方法 - Google Patents
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- 239000007789 gas Substances 0.000 claims abstract description 12
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 4
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
本发明涉及一种N掺杂C膜的制备方法，其特征在于：（1）选择衬底材料，高纯石墨为溅射靶材，N2为离子束的N+源；（2）对衬底材料依次用丙酮、酒精、去离子水进行超声清洗，吹干；（3）把衬底材料放入溅射腔中，启动磁控溅射设备并抽真空，在真空度达到1.0~3.0*10－4Pa时，通入溅射Ar气，使C靶起辉，设定工艺参数，在Si片上制备C膜；关闭C靶，开启离子束沉积系统，通入N2作为氮源，通过离子束发射N+轰击C膜，与衬底C膜发生反应并实现掺杂；（4）取出样品，放入250‑400℃、N2气氛炉中1.5‑3h保温退火，制得N掺杂C薄膜。本发明优点：工艺简单，可控性强；以N2为离子源，不引入其他杂质元素，成膜几率高；保温退火，提高了掺杂均匀性及薄膜的结晶质量。
Description
技术领域
本发明属薄膜制备技术领域，涉及一种N掺杂C膜的制备方法。
背景技术
氮化碳的结构与氮硅共价化合物相类似，其具有较大的聚合能和力学稳定性，Teter等对CN结构进行推测，共计五种，即：α相、β 相、立方相、准立方相和类石墨相，大量研究表面，除类石墨相外，其他相氮化碳的体弹性模量理论值均可与金刚石相比拟，被认为是一种新型的超硬材料，具有许多优良性能。经过多年努力，理论与实验两方面都得到了较大的发展，并报道合成了a－C3N4、B－C3N4，石墨相或CNX等。
目前制备出的N掺杂C膜，大多数是以NH3为N掺杂源，或者以其他N化合物为掺杂源，这样会引入其他杂质源，不利于N掺杂C膜的纯度。
发明内容
本发明的目的是为了解决现有N掺杂C膜的纯度不高的问题，提供一种N掺杂C膜的制备方法；本发明以N2为离子源，直接利用离子束沉积技术，为C膜提供掺杂N离子。
为了实现上述目的，本发明采用的技术方案如下：
一种N掺杂C膜的制备方法，其特征在于包括如下步骤：
（1）选用单晶Si片或玻璃为衬底材料，高纯石墨为溅射靶材，N2为离子束的N+源；
（2）对衬底材料依次用丙酮、酒精、去离子水进行超声波清洗，以去除表面杂质和油污，吹干备用；
（3）把衬底材料放入溅射腔中，启动磁控溅射设备并抽真空，在真空度达到1.0~3.0*10－4Pa时，通入溅射气体Ar气，使C靶起辉，达到活化和去除表面杂质的目的，而后设定工艺参数，控制功率50-200w，Ar为10-30sccm，工作气压0.5-1.0Pa，时间10-60min；最终在Si片上制备一定性能的C膜，之后关闭C靶，开启离子束沉积系统，通入N2作为氮源，通过离子束发射N+轰击C膜，与衬底C膜发生反应并实现掺杂；
（4）然后取出样品，将其放入250-400℃、N2气氛炉中进行1.5-3h保温退火，最终制得N掺杂C薄膜。
进一步，所述工艺参数为：功率100w，Ar为20sccm，工作气压0.5Pa，时间30min。
进一步，所述工艺参数为：功率150w，Ar为25sccm，工作气压1Pa，时间45min。
首先利用磁控溅射法在Si或者玻璃衬底上制备一层C膜，而后配合离子束沉积技术，以N2为N+源，轰击C膜，进而与C膜发生反应并进行掺杂，最终生成一定性能的掺杂C薄膜。整个过程，引入变量较少，可控性、重复性强，可以根据需要制备各种掺杂量和各种性能的掺杂C薄膜，以利于电子元器件的使用要求。
本发明的有益效果：
1.磁控溅射只进行C薄膜的镀制，工艺简单，可控性强；
2.以N2为离子源，不引入其他杂质元素，减少其它工艺中N2的离化过程，是其他发明所无法比拟的，离子束沉积直接提高N+，成膜几率高；
3.进行保温退火，有利于薄膜中C、N离子进一步反应以及提高掺杂均匀性，提高薄膜的结晶质量。
具体实施方式
实施例1
（1）以纯度为99.99％的石墨作为溅射靶材，以单晶Si片为衬底材料，首先按照常规方法对衬底材料依次用丙酮、酒精、去离子水进行超声波清洗，以去除表面油脂和污物，而后用热风吹干备用；
（2）将吹干后的单晶Si片放入磁控溅射腔室中，在真空度达到2.0*10-4Pa时，通入溅射气体氩气，使C靶起辉，进行C薄膜的制备，其工艺参数为：功率100w，Ar为20sccm，工作气压0.6Pa，时间40min；
（3）C膜镀制结束，C靶熄灭，启动离子束沉积系统，以N2为气源，对准C膜，进行N+的发射，在此过程中N+与C膜进行反应并实现掺杂；
（4）然后取出样品，将其放入300℃、N2气氛炉中进行2.5小时保温退火，最终制得结晶质量较好的N掺杂C薄膜。
实施例2
（1）以纯度为99.99％的石墨作为溅射靶材，以单晶Si片为衬底材料，首先按照常规方法对衬底材料依次用丙酮、酒精、去离子水进行超声波清洗，以去除表面油脂和污物，而后用热风吹干备用；
（2）将吹干后的单晶Si片放入磁控溅射腔室中，在真空度达到1.0*10-4Pa时，通入溅射气体氩气，使C靶起辉，进行C薄膜的制备，其工艺参数为：功率50w，Ar为10sccm，工作气压0.5Pa，时间60min；
（3）C膜镀制结束，C靶熄灭，启动离子束沉积系统，以N2为气源，对准C膜，进行N+的发射，在此过程中N+与C膜进行反应并实现掺杂；
（4）然后取出样品，将其放入250℃、N2气氛炉中进行3小时保温退火，最终制得不同结晶质量的N掺杂C薄膜。
实施例3
（1）以纯度为99.99％的石墨作为溅射靶材，以单晶Si片为衬底材料，首先按照常规方法对衬底材料依次用丙酮、酒精、去离子水进行超声波清洗，以去除表面油脂和污物，而后用热风吹干备用；
（2）将吹干后的单晶Si片放入磁控溅射腔室中，在真空度达到3.0*10-4Pa时，通入溅射气体氩气，使C靶起辉，进行C薄膜的制备，其工艺参数为：功率200w，Ar为30sccm，工作气压1.0Pa，时间10min；
（3）C膜镀制结束，C靶熄灭，启动离子束沉积系统，以N2为气源，对准C膜，进行N+的发射，在此过程中N+与C膜进行反应并实现掺杂；
（4）然后取出样品，将其放入400℃、N2气氛炉中进行1.5小时保温退火，最终制得不同性能的N掺杂C薄膜。
以上所述，仅是本发明的较佳实施例而已，并非对本发明作任何形式上的限制；任何熟悉本领域的技术人员，在不脱离本发明技术方案范围情况下，都可利用上述揭示的方法和技术内容对本发明技术方案做出许多可能的变动和修饰，或修改为等同变化的等效实施例。因此，凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所做的任何简单修改、等同替换、等效变化及修饰，均仍属于本发明技术方案保护的范围内。
Claims (4)
1.一种N掺杂C膜的制备方法，其特征在于包括如下步骤：
（1）选用单晶Si片或玻璃为衬底材料，高纯石墨为溅射靶材，N2为离子束的N+源；
（2）对衬底材料依次用丙酮、酒精、去离子水进行超声波清洗，吹干备用；
（3）把衬底材料放入溅射腔中，启动磁控溅射设备并抽真空，在真空度达到1.0~3.0*10－4Pa时，通入溅射气体Ar气，使C靶起辉，而后设定工艺参数，在Si片上制备C膜；之后关闭C靶，开启离子束沉积系统，通入N2作为氮源，通过离子束发射N+轰击C膜，与衬底C膜发生反应并实现掺杂；
（4）然后取出样品，将其放入250-400℃、N2气氛炉中进行1.5-3h保温退火，最终制得N掺杂C薄膜。
2.根据权利要求1所述一种N掺杂C膜的制备方法，其特征在于：所述工艺参数为：功率50-200w，Ar为10-30sccm，工作气压0.5-1.0Pa，时间10-60min。
3.根据权利要求2所述一种N掺杂C膜的制备方法，其特征在于：所述工艺参数为：功率100w，Ar为20sccm，工作气压0.5Pa，时间30min。
4.根据权利要求2所述一种N掺杂C膜的制备方法，其特征在于：所述工艺参数为：功率150w，Ar为25sccm，工作气压1Pa，时间45min。
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| US5089104A (en) * | 1989-12-04 | 1992-02-18 | Hitachi, Ltd. | Method and apparatus for forming a multiple-element thin film based on ion beam sputtering |
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| CN112626470A (zh) * | 2020-12-09 | 2021-04-09 | 中建材蚌埠玻璃工业设计研究院有限公司 | 一种碳自掺杂且浓度呈梯度分布的cn薄膜的制备方法 |
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| CN112626470A (zh) * | 2020-12-09 | 2021-04-09 | 中建材蚌埠玻璃工业设计研究院有限公司 | 一种碳自掺杂且浓度呈梯度分布的cn薄膜的制备方法 |
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