CN106119796A - A kind of preparation method of amorphous diamond coatings - Google Patents
A kind of preparation method of amorphous diamond coatings Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 43
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 30
- 239000010432 diamond Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 37
- 238000000151 deposition Methods 0.000 claims abstract description 30
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 30
- 230000008021 deposition Effects 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 229910052754 neon Inorganic materials 0.000 claims abstract description 24
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000012298 atmosphere Substances 0.000 claims abstract description 14
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 17
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 235000012431 wafers Nutrition 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000005137 deposition process Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004549 pulsed laser deposition Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001234 light alloy Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000001420 photoelectron spectroscopy Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C14/0605—Carbon
- C23C14/0611—Diamond
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
本发明公开一种非晶金刚石涂层的制备方法，在氖气气氛或含氖气的混合气氛中对基材进行磁控溅射沉积，功率为0.3‑5kW，衬底偏压为‑50～‑500V，沉积时间为1～3小时，得到非晶金刚石涂层，所述磁控溅射沉积采用的磁控源为纯度大于99.9％的单质石墨靶。该方法具有成本低、制备速度快、可大面积均匀沉积、适应复杂沉积表面的优点，具有很好的应用前景。The invention discloses a method for preparing an amorphous diamond coating. The base material is deposited by magnetron sputtering in a neon gas atmosphere or a mixed atmosphere containing neon gas. The power is 0.3-5kW, and the substrate bias voltage is -50～ -500V, the deposition time is 1 to 3 hours to obtain an amorphous diamond coating, and the magnetron source used in the magnetron sputtering deposition is a simple graphite target with a purity greater than 99.9%. The method has the advantages of low cost, fast preparation speed, large-area uniform deposition, and adaptability to complex deposition surfaces, and has a good application prospect.
Description
技术领域technical field
本发明属于磨具技术领域，涉及一种非晶金刚石涂层的制备方法。The invention belongs to the technical field of grinding tools, and relates to a preparation method of an amorphous diamond coating.
技术背景technical background
碳基涂层(如金刚石、类金刚石DLC、非晶金刚石ta-C等)具有极高的硬度和耐磨性、低摩擦系数和热膨胀系数、高弹性模量、良好的化学稳定性以及与非铁族亲和弱等优异性能，被广泛应用于刀具、模具、精密零部件、微电子等领域。其中，非晶金刚石ta-C是一种四面体无定形非晶碳，其金刚石sp3键含量高达80％以上，结构和性能非常接近金刚石(100％sp3)，具有极高的硬度和耐磨性、低摩擦自润滑性、高热导系数、等特性低热膨胀系数、良好的化学稳定性以及与非铁族亲和弱等优异性能。相比传统的DLC涂层(a-C或a-C:H)，ta-C涂层sp3键含量高，且不含有氢，具有更高的硬度(高达80GPa)、密度和热稳定性(>500℃)。此外，与金刚石涂层相比，ta-C涂层具有(1)无晶界的光滑表面；(2)低温生长(<150C)(金刚石涂层沉积通常>700C)；(3)工艺参数可调，使涂层结构和性能可在大范围内剪裁等优点。因此，ta-C涂层有望取代昂贵的CVD沉积微晶金刚石涂层应用在钻头，刀片，立铣刀等刀具上，进一步应用于轻合金(铝合金)、金属基复合材料、工程陶瓷、纤维增强复合塑料等难加工材料的切削加工。同时，ta-C作为理想的耐磨材料，还应用于内表面要求耐磨和低粗糙度的场合，如内燃机活塞环、拉丝模、紧压模、各种模具等。Carbon-based coatings (such as diamond, diamond-like DLC, amorphous diamond ta-C, etc.) have extremely high hardness and wear resistance, low coefficient of friction and thermal expansion, high elastic modulus, good chemical stability and compatibility with non- It has excellent properties such as weak iron family affinity, and is widely used in the fields of cutting tools, molds, precision parts, and microelectronics. Among them, amorphous diamond ta-C is a kind of tetrahedral amorphous amorphous carbon, its diamond sp3 bond content is as high as 80%, its structure and performance are very close to diamond (100% sp3), and it has extremely high hardness and wear resistance , low friction and self-lubricating properties, high thermal conductivity, low thermal expansion coefficient, good chemical stability, and weak affinity with non-iron groups. Compared with traditional DLC coatings (a-C or a-C:H), ta-C coatings have high sp3 bond content and no hydrogen, and have higher hardness (up to 80GPa), density and thermal stability (>500℃) . In addition, compared with diamond coating, ta-C coating has (1) smooth surface without grain boundaries; (2) low temperature growth (<150C) (diamond coating deposition is usually >700C); (3) process parameters can be Adjustment, so that the structure and performance of the coating can be tailored in a wide range. Therefore, ta-C coating is expected to replace expensive CVD-deposited microcrystalline diamond coatings on drills, blades, end mills and other tools, and is further applied to light alloys (aluminum alloys), metal matrix composites, engineering ceramics, fiber Machining of difficult-to-machine materials such as reinforced composite plastics. At the same time, as an ideal wear-resistant material, ta-C is also used in occasions where the inner surface requires wear resistance and low roughness, such as internal combustion engine piston rings, wire drawing dies, compression dies, and various molds.
非晶金刚石ta-C的制备关键是sp3键的形成，需要高离化率的碳离子束流。目前ta-C的制备技术主要有电弧蒸发沉积(Cathodic arc evaporation,CVA)、激光蒸发沉积(Pulsed laser deposition,PLD)、磁控溅射等技术。CVA和PLD虽然能获得较高离化率的碳粒子束，但石墨靶材的蒸发易产生大颗粒，而且涂层横向沉积速率不均匀，不能大面积镀膜。现在较为主流的制备技术是FCVA，采用电磁过滤系统将宏观大颗粒过滤，获得离化率接近100％的碳离子束流，但过滤导致沉积速率大幅下降，涂层成本提升。此外，受磁场约束的碳离子流横截面小，很难应用于大尺寸工件镀膜。而磁控溅射不会产生大颗粒，能实现大面积均匀沉积，但是传统磁控溅射难以获得高离化率的碳粒子束合成sp3键。因此，寻求一种能、大面积、快速、低成本、适应复杂工件表面均匀沉积、高质量的非晶金刚石制备方法是目前实现非晶金刚石涂层推广应用所急需解决的问题。The key to the preparation of amorphous diamond ta-C is the formation of sp3 bonds, which requires a carbon ion beam with a high ionization rate. At present, the preparation technologies of ta-C mainly include arc evaporation deposition (Cathodic arc evaporation, CVA), laser evaporation deposition (Pulsed laser deposition, PLD), magnetron sputtering and other technologies. Although CVA and PLD can obtain carbon particle beams with higher ionization rates, the evaporation of graphite targets tends to produce large particles, and the lateral deposition rate of the coating is not uniform, so it cannot be coated on a large area. The current mainstream preparation technology is FCVA, which uses an electromagnetic filtration system to filter macroscopic large particles to obtain a carbon ion beam with an ionization rate close to 100%. However, the deposition rate is greatly reduced by filtration and the coating cost is increased. In addition, the cross-section of the carbon ion flow confined by the magnetic field is small, so it is difficult to apply to the coating of large-sized workpieces. Magnetron sputtering does not produce large particles and can achieve large-area uniform deposition, but it is difficult for traditional magnetron sputtering to obtain high ionization rate carbon particle beams to synthesize sp3 bonds. Therefore, seeking a high-energy, large-area, fast, low-cost, uniform deposition method for complex workpiece surfaces, and high-quality amorphous diamond preparation methods is an urgent problem to be solved for the promotion and application of amorphous diamond coatings.
发明内容Contents of the invention
针对上述现有技术的不足，本发明提供提供一种非晶金刚石涂层的制备方法，该方法中的磁控溅射碳离化率高，制备的非晶金刚石涂层具有高密度、高sp3键含量优点，具有成本低、制备速度快、可大面积均匀沉积、适应复杂沉积表面的优点，具有很好的应用前景。For above-mentioned deficiencies in the prior art, the present invention provides a kind of preparation method of amorphous diamond coating, the magnetron sputtering carbon ionization rate in this method is high, the prepared amorphous diamond coating has high density, high sp3 It has the advantages of low bond content, low cost, fast preparation speed, large-area uniform deposition, and adaptability to complex deposition surfaces, and has a good application prospect.
本发明的目的通过以下技术方案实现：The object of the present invention is achieved through the following technical solutions:
一种非晶金刚石涂层的制备方法，在氖气气氛或含氖气的混合气氛中对基材进行磁控溅射沉积，功率为0.3-5kW，衬底偏压为-50～-500V，沉积时间为1～3小时，得到非晶金刚石涂层，所述磁控溅射沉积采用的磁控源为纯度大于99.9％的单质石墨靶。A method for preparing an amorphous diamond coating, in which a base material is deposited by magnetron sputtering in a neon atmosphere or a mixed atmosphere containing neon, with a power of 0.3-5kW and a substrate bias of -50--500V, The deposition time is 1-3 hours to obtain an amorphous diamond coating, and the magnetron source used in the magnetron sputtering deposition is a simple graphite target with a purity greater than 99.9%.
本发明所用的基材包括硅片和合金基材，具体没有特殊限制。The substrates used in the present invention include silicon wafers and alloy substrates, and are not specifically limited.
优选的，对上述基材的待沉积表面进行辉光预处理，具体是在氩气气氛中对基材进行轰击刻蚀，以除去表面的氧化层，提高涂层与基材的结合力。Preferably, glow pretreatment is performed on the surface of the substrate to be deposited, specifically performing bombardment etching on the substrate in an argon atmosphere, so as to remove the oxide layer on the surface and improve the bonding force between the coating and the substrate.
优选的，所述预处理过程中，所述氩气气氛的压力为0.5～1Pa。Preferably, during the pretreatment process, the pressure of the argon atmosphere is 0.5-1 Pa.
优选的，所述预处理过程中，衬底偏压设置为-100～-1000V，时间为30-180min。Preferably, in the pretreatment process, the substrate bias voltage is set to -100--1000V, and the time is 30-180min.
优选的，所述氖气或含氖气的混合气氛的压强为0.3～3Pa。Preferably, the pressure of the neon gas or the mixed atmosphere containing neon gas is 0.3-3Pa.
优选的，所述含氖气的混合气氛为氖气和氩气的混合气氛，所述混合气氛中氖气的分压百分比为10％～90％。Preferably, the mixed atmosphere containing neon is a mixed atmosphere of neon and argon, and the partial pressure percentage of neon in the mixed atmosphere is 10%-90%.
本发明具有以下有益效果：本发明采用电离能高的氖气或含氖气的混合气体作为溅射气体，能提高电子温度，进而提高碳粒子离化率，获得高sp3键含量的非晶金刚石ta-C涂层，同时本发明的方法能够实现低成本、大面积、快速沉积得到涂层，且能适应复杂表面实现均匀沉积，所制备的非晶金刚石ta-C涂层sp3含量高、结构致密，性能优异。The present invention has the following beneficial effects: the present invention uses neon gas with high ionization energy or a mixed gas containing neon gas as the sputtering gas, which can increase the electron temperature, thereby increasing the ionization rate of carbon particles, and obtaining amorphous diamond with high sp3 bond content ta-C coating, while the method of the present invention can achieve low cost, large area, rapid deposition to obtain the coating, and can adapt to complex surfaces to achieve uniform deposition, the prepared amorphous diamond ta-C coating has high sp3 content and structure Dense, excellent performance.
具体实施方式detailed description
本发明可通过如下的实施例进一步的说明，但实施例不是对本发明保护范围的限制。The present invention can be further illustrated by the following examples, but the examples are not intended to limit the protection scope of the present invention.
实施例1Example 1
非晶金刚石ta-C涂层的制备具体如下：The preparation of amorphous diamond ta-C coating is as follows:
用酒精超声波清洗硅片基体，然后用去离子水漂洗，用干燥压缩空气吹干，在高功率脉冲等离子体增强型复合磁控溅射设备GDUT-HAS500型镀膜机(磁控溅射源为纯度为99.9％的石墨靶)的真空室中将基体置于工件支架上，将真空室抽真空至5.0×10-3Pa以下，向真空室通入100sccm氩气，使真空室压力为1Pa，开启衬底偏压进行预处理，预处理过程设置衬底偏压-500V，预处理时间为30分钟；然后开启磁控溅射源进行磁控溅射沉积，沉积过程中向真空室通入10sccm氖和90sccm氩(氖气占10％)，控制气压0.5Pa，设置功率为2kW，偏压为-100V，沉积时间为2小时，沉积完成后待真空室温度降至室温，即在基体表面制备得到非晶金刚石ta-C涂层。Ultrasonic cleaning of the silicon wafer substrate with alcohol, then rinsing with deionized water, drying with dry compressed air, in the high-power pulse plasma enhanced composite magnetron sputtering equipment GDUT-HAS500 coating machine (magnetron sputtering source is purity 99.9% graphite target) in the vacuum chamber, place the substrate on the workpiece support, evacuate the vacuum chamber to below 5.0×10 -3 Pa, feed 100 sccm argon gas into the vacuum chamber, make the vacuum chamber pressure 1Pa, open The substrate bias is used for pretreatment, and the substrate bias is set to -500V during the pretreatment process, and the pretreatment time is 30 minutes; then the magnetron sputtering source is turned on for magnetron sputtering deposition, and 10 sccm neon is introduced into the vacuum chamber during the deposition process and 90sccm argon (neon accounts for 10%), the control pressure is 0.5Pa, the set power is 2kW, the bias voltage is -100V, and the deposition time is 2 hours. Amorphous diamond ta-C coating.
对硅片上制备的ta-C涂层样品进行测试，具体采用D8 Discover型XRR测试涂层密度达2.8g/cm3，采用AXIS ULTRADLD型X光电子谱测得sp3键含量62％、用NANO G200纳米压痕测试测得涂层的硬度达到30GPa。The ta-C coating sample prepared on the silicon wafer was tested. Specifically, the D8 Discover XRR was used to test the coating density to 2.8g/cm 3 , and the sp 3 bond content was measured by AXIS ULTRADLD X photoelectron spectroscopy to be 62%. The G200 nano-indentation test shows that the hardness of the coating reaches 30GPa.
实施例2Example 2
用酒精超声波清洗硅片基体，然后用去离子水漂洗，用干燥压缩空气吹干，在高功率脉冲等离子体增强型复合磁控溅射设备GDUT-HAS500型镀膜机(磁控溅射源为纯度为99.9％的石墨靶)的真空室中将基体置于工件支架上，将真空室抽真空至5.0×10-3Pa以下，向真空室通入100sccm氩气，使真空室压力为1Pa，开启衬底偏压进行预处理，预处理过程设置衬底偏压-500V，预处理时间为30分钟；然后开启磁控溅射源进行磁控溅射沉积，沉积过程中向真空室通入90sccm氖气和10sccm氩气(氖气占90％)，控制气压0.5Pa，设置磁控溅射功率2kW，同时偏压设置为-100V，沉积时间为2小时，沉积完成后待真空室温度降至室温，即在基体表面制备得到非晶金刚石ta-C涂层。Ultrasonic cleaning of the silicon wafer substrate with alcohol, then rinsing with deionized water, drying with dry compressed air, in the high-power pulse plasma enhanced composite magnetron sputtering equipment GDUT-HAS500 coating machine (magnetron sputtering source is purity 99.9% graphite target) in the vacuum chamber, place the substrate on the workpiece support, evacuate the vacuum chamber to below 5.0×10 -3 Pa, feed 100 sccm argon gas into the vacuum chamber, make the vacuum chamber pressure 1Pa, open The substrate bias is used for pretreatment, and the substrate bias is set to -500V during the pretreatment process, and the pretreatment time is 30 minutes; then the magnetron sputtering source is turned on for magnetron sputtering deposition, and 90sccm neon is introduced into the vacuum chamber during the deposition process Argon gas and 10 sccm argon (neon accounted for 90%), the control pressure is 0.5Pa, the magnetron sputtering power is set to 2kW, and the bias voltage is set to -100V at the same time, the deposition time is 2 hours, and the temperature of the vacuum chamber is lowered to room temperature after the deposition is completed. , that is, an amorphous diamond ta-C coating is prepared on the surface of the substrate.
参照实施例1的测试方法，测得所制备的非晶金刚石ta-C涂层的密度达3.3g/cm3，sp3键含量在75％以上，硬度达到38GPa。Referring to the test method of Example 1, it is measured that the prepared amorphous diamond ta-C coating has a density of 3.3 g/cm 3 , a sp 3 bond content of over 75%, and a hardness of 38 GPa.
实施例3Example 3
用酒精超声波清洗硅片基体，然后用去离子水漂洗，用干燥压缩空气吹干，在高功率脉冲等离子体增强型复合磁控溅射设备GDUT-HAS500型镀膜机(磁控溅射源为纯度为99.9％的石墨靶)的真空室中将基体置于工件支架上，将真空室抽真空至5.0×10-3Pa以下，向真空室通入100sccm氩气，使真空室压力为1Pa，开启衬底偏压进行预处理，预处理过程设置偏压-500V，预处理时间为30分钟；然后开启磁控溅射源进行磁控溅射沉积，沉积过程中向真空室通入50sccm氖气和50sccm氩气(氖气占50％)，控制气压0.5Pa，设置磁控溅射功率2kW，同时偏压设置为-100V，沉积时间为2小时，沉积完成后待真空室温度降至室温，即在基体表面制备得到非晶金刚石ta-C涂层。Ultrasonic cleaning of the silicon wafer substrate with alcohol, then rinsing with deionized water, drying with dry compressed air, in the high-power pulse plasma enhanced composite magnetron sputtering equipment GDUT-HAS500 coating machine (magnetron sputtering source is purity 99.9% graphite target) in the vacuum chamber, place the substrate on the workpiece support, evacuate the vacuum chamber to below 5.0×10 -3 Pa, feed 100 sccm argon gas into the vacuum chamber, make the vacuum chamber pressure 1Pa, open The substrate bias is pretreated, the pretreatment process is set to bias -500V, and the pretreatment time is 30 minutes; then the magnetron sputtering source is turned on for magnetron sputtering deposition, and 50 sccm neon gas and 50 sccm argon gas (neon gas accounts for 50%), control the air pressure 0.5Pa, set the magnetron sputtering power to 2kW, and set the bias voltage to -100V at the same time, and the deposition time is 2 hours. After the deposition is completed, the temperature of the vacuum chamber drops to room temperature, that is An amorphous diamond ta-C coating was prepared on the surface of the substrate.
参照实施例1的制备方法，经过密度、X光电子谱、纳米压痕测试，所制备的非晶金刚石ta-C涂层的密度达3g/cm3，sp3键含量为65％，硬度达到34GPa。Referring to the preparation method of Example 1, through density, X-ray photoelectron spectroscopy, and nanoindentation tests, the prepared amorphous diamond ta-C coating has a density of 3 g/cm 3 , an sp3 bond content of 65%, and a hardness of 34 GPa.
对比实施例comparative example
用酒精超声波清洗硅片基体，然后用去离子水漂洗，用干燥压缩空气吹干，在高功率脉冲等离子体增强型复合磁控溅射设备GDUT-HAS500型镀膜机(磁控溅射源为纯度为99.9％的石墨靶)的真空室中将基体置于工件支架上，将真空室抽真空至5.0×10-3Pa以下，向真空室通入100sccm氩气，使真空室压力为1Pa，开启衬底偏压行预处理，预处理过程设置偏压-500V，预处理时间为30分钟；然后开启磁控溅射源进行磁控溅射沉积，沉积过程中向真空室通入100scmm氩气，控制气压0.5Pa，设置磁控溅射功率2kW，同时偏压设置为-100V，沉积时间为2小时，，沉积完成后待真空室温度降至室温，即在基体表面制备得到非晶金刚石ta-C涂层。Ultrasonic cleaning of the silicon wafer substrate with alcohol, then rinsing with deionized water, drying with dry compressed air, in the high-power pulse plasma enhanced composite magnetron sputtering equipment GDUT-HAS500 coating machine (magnetron sputtering source is purity 99.9% graphite target) in the vacuum chamber, place the substrate on the workpiece support, evacuate the vacuum chamber to below 5.0×10 -3 Pa, feed 100 sccm argon gas into the vacuum chamber, make the vacuum chamber pressure 1Pa, open The substrate bias is pretreated, the pretreatment process is set to a bias of -500V, and the pretreatment time is 30 minutes; then the magnetron sputtering source is turned on for magnetron sputtering deposition, and 100 scmm argon gas is introduced into the vacuum chamber during the deposition process. Control the air pressure to 0.5Pa, set the magnetron sputtering power to 2kW, and set the bias voltage to -100V at the same time, and the deposition time is 2 hours. C coating.
参照实施例1的测试方法，测得所制备的对比非晶金刚石ta-C涂层的密度为2g/cm3，sp3键含量为40％，硬度为18GPa。Referring to the test method of Example 1, it was measured that the prepared comparative amorphous diamond ta-C coating had a density of 2 g/cm 3 , a sp3 bond content of 40%, and a hardness of 18 GPa.
最后应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制。本领域的技术人员应当理解，可以对本发明的技术方案进行若干推演或者等同替换，而不脱离本发明技术方案的实质和范围。Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than limit the protection scope of the present invention. Those skilled in the art should understand that several inferences or equivalent replacements can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
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