CN110306153A - A kind of preparation method of DLC coating doped with Cr - Google Patents
A kind of preparation method of DLC coating doped with Cr Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims abstract description 53
- 238000000576 coating method Methods 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 230000007704 transition Effects 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000004544 sputter deposition Methods 0.000 claims description 25
- 239000000758 substrate Substances 0.000 claims description 16
- 230000004907 flux Effects 0.000 claims description 12
- 239000012495 reaction gas Substances 0.000 claims description 10
- 238000000168 high power impulse magnetron sputter deposition Methods 0.000 claims description 9
- JPNWDVUTVSTKMV-UHFFFAOYSA-N cobalt tungsten Chemical compound [Co].[W] JPNWDVUTVSTKMV-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 229910000531 Co alloy Inorganic materials 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000005554 pickling Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- -1 pickling Substances 0.000 claims 1
- 230000006872 improvement Effects 0.000 abstract description 6
- 238000000151 deposition Methods 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract description 2
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000012938 design process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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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
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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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- 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
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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
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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- 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
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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
- C23C14/0641—Nitrides
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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
- C23C14/14—Metallic material, boron or silicon
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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
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Abstract
本发明公开了一种掺杂Cr的DLC涂层的制备方法，充分利用了高功率脉冲磁控溅射膜层光洁度、均匀度、致密度高的优点，为改善DLC涂层结合力和膜层韧性差的缺点，采用了底层和过渡层设计方法。这一独特的膜系设计和参杂工艺既保证了涂层结合力的提高，又保证了涂层沉积速率、涂层致密性和耐磨减摩性能的提高。采用本发明的方法制备的掺Cr的DLC涂层外观呈灰黑色，表面光滑致密，涂层的硬度32GPa，膜基结合力达到72N，涂层厚度为1.45μm。涂层的干摩擦系数为0.2。表明掺Cr的DLC涂层具有良好的耐磨和减摩性能。
The invention discloses a preparation method of a Cr-doped DLC coating, which fully utilizes the advantages of high-power pulse magnetron sputtering film layer smoothness, uniformity, and high density, in order to improve the bonding force of the DLC coating and the film layer Due to the disadvantage of poor toughness, the design method of the bottom layer and transition layer is adopted. This unique film system design and doping process not only ensure the improvement of coating adhesion, but also ensure the improvement of coating deposition rate, coating compactness and wear resistance and friction reduction performance. The appearance of the Cr-doped DLC coating prepared by the method of the present invention is gray-black, the surface is smooth and compact, the hardness of the coating is 32GPa, the bonding force of the film base reaches 72N, and the coating thickness is 1.45 μm. The dry friction coefficient of the coating is 0.2. It shows that the Cr-doped DLC coating has good wear resistance and antifriction properties.
Description
技术领域technical field
本发明属于涂层材料技术领域，具体涉及一种掺杂Cr的DLC涂层的制备方法。The invention belongs to the technical field of coating materials, and in particular relates to a preparation method of a Cr-doped DLC coating.
背景技术Background technique
物理气相沉积技术表示在真空条件下，采用物理方法，将材料源——固体或液体表面气化成气态原子、分子或部分电离成离子，并通过低压气体(或等离子体)过程，在基体表面沉积具有某种特殊功能的薄膜的技术。申请号为“201210423173.5”，专利名称为“一种掺Ti的类金刚石涂层的制备方法”中公开了一种制备掺Ti的DLC涂层的方法，将预处理好的基体放入电弧与磁控溅射复合镀膜设备的转架杆上，以柱弧Ti靶作为Ti源，以平面C靶作为C的来源，平面C靶共三对，以均布的方式安置在炉体内壁上，采用高纯Ar作为主要离化气体，保证有效的辉光放电过程；采用高纯N2作为反应气体，使其离化并与Ti、C元素结合，在基体表面沉积形成掺Ti的DLC涂层。制备的该掺Ti的DLC涂层外观呈黑色，表面光滑致密，涂层的硬度28GPa，膜基结合力达到60N，涂层厚度为2.5μm，当摩擦副为Al2O3球时，涂层的干摩擦系数为0.2。表明掺Ti的DLC涂层具有良好的耐磨和减摩性能。Physical vapor deposition technology refers to the use of physical methods under vacuum conditions to vaporize material sources—solid or liquid surfaces into gaseous atoms, molecules or parts of them into ions, and deposit them on the surface of the substrate through a low-pressure gas (or plasma) process. The technology of thin films with certain special functions. The application number is "201210423173.5", and the patent name is "A method for preparing a Ti-doped diamond-like coating", which discloses a method for preparing a Ti-doped DLC coating. The pretreated substrate is placed in an arc and magnetic On the turret rod of the controlled sputtering composite coating equipment, the column arc Ti target is used as the Ti source, and the plane C target is used as the C source. There are three pairs of plane C targets, which are placed on the inner wall of the furnace in a uniform manner. High-purity Ar is used as the main ionization gas to ensure an effective glow discharge process; high-purity N2 is used as the reaction gas to ionize it and combine with Ti and C elements to form a Ti-doped DLC coating on the surface of the substrate. The appearance of the prepared Ti-doped DLC coating is black, the surface is smooth and compact, the hardness of the coating is 28GPa, the film-base bonding force reaches 60N, and the coating thickness is 2.5μm. When the friction pair is Al2O3 ball, the dry friction of the coating The coefficient is 0.2. It shows that the Ti-doped DLC coating has good wear resistance and antifriction properties.
上述专利在制备工艺、膜系设计均取有一定的新颖性，性能上取得了一定的突破。然并不适用于钨钴硬质合金系列的膜层设计与制备工艺。针对硬质合金工具最常用的材料钨钴合金的DLC膜系设计和制备方法，鲜有报道。The above-mentioned patents have certain novelties in the preparation process and film system design, and have achieved certain breakthroughs in performance. However, it is not suitable for the film layer design and preparation process of tungsten-cobalt cemented carbide series. There are few reports on the design and preparation of DLC film system for tungsten-cobalt alloy, the most commonly used material for cemented carbide tools.
发明内容Contents of the invention
本发明为解决上述技术问题采用如下技术方案，一种掺杂Cr的DLC涂层的制备方法，具体步骤为：The present invention adopts following technical scheme for solving the above-mentioned technical problem, a kind of preparation method of the DLC coating of doping Cr, concrete steps are:
步骤S1:将表面处理好的钨钴合金基体放入溅射设备腔体的转架杆上，该转架整体转动的同时，转架杆自转，以保证涂层的均匀性；Step S1: Put the surface-treated tungsten-cobalt alloy substrate on the turret rod of the sputtering equipment cavity, and when the turret rotates as a whole, the turret rod rotates to ensure the uniformity of the coating;
步骤S2:以长柱型Cr靶作为参杂源，以长住型石墨靶作为碳元素的来源，平面Cr靶为参杂Cr元素来源，均匀分布并安装在炉体内壁上，采用高纯Ar作为主要离化气体，保证有效的辉光放电过程；分别采用Cr层作为打底层、CrN、CrN2、Cr+C作为梯度过渡层，高纯N2作为过渡层反应气体，C2H2作为DLC层反应气体，形成Cr、CrN、CrN2、Cr+C、α-C：H的多层膜系涂层；Step S2: Use the long-column Cr target as the doping source, the long-lived graphite target as the source of the carbon element, and the flat Cr target as the source of the doping Cr element, which is evenly distributed and installed on the inner wall of the furnace, using high-purity Ar As the main ionized gas to ensure an effective glow discharge process; respectively use Cr layer as the bottom layer, CrN, CrN 2 , Cr+C as the gradient transition layer, high-purity N 2 as the transition layer reaction gas, and C 2 H 2 as the transition layer. The DLC layer reacts with gas to form a multi-layer film system coating of Cr, CrN, CrN 2 , Cr+C, α-C:H;
步骤S3:制备工艺条件：Step S3: preparation process conditions:
A)等离子体洗靶：A) Plasma washing target:
靶体装入真空室后，抽真空并加热到真空室温度为400℃。通入200sccm的Ar到真空室，开偏压至1000V，炉体内气压为2Pa，对真空室的靶体表面进行轰击清洗，持续800s；After the target body is loaded into the vacuum chamber, it is evacuated and heated to a temperature of 400°C in the vacuum chamber. Introduce 200 sccm of Ar into the vacuum chamber, turn on the bias voltage to 1000V, and the air pressure in the furnace is 2Pa, and bombard and clean the surface of the target body in the vacuum chamber for 800s;
B)等离子体清洗基体：B) Plasma cleaning of the substrate:
基体装入真空室后，抽真空并加热到真空室温度为400℃。通入200sccm的Ar到真空室，开偏压至1000V，炉体内气压为2Pa，对真空室的靶体表面进行轰击清洗，持续1940s；After the substrate was loaded into the vacuum chamber, it was evacuated and heated to a vacuum chamber temperature of 400°C. Introduce 200sccm Ar into the vacuum chamber, turn on the bias voltage to 1000V, and the air pressure in the furnace is 2Pa, and bombard and clean the surface of the target body in the vacuum chamber for 1940s;
C)Cr底层制备：C) Preparation of Cr bottom layer:
腔体温度设定400度，调节Ar通量到200sccm、腔体气压设定为2Pa，然后开启柱弧Cr靶，调整偏压到60V，HIPIMS电压为2000V，电流500A，溅射功率10Kw，打底层阶段时间设定为600秒；The chamber temperature is set to 400 degrees, the Ar flux is adjusted to 200sccm, the chamber pressure is set to 2Pa, then the column arc Cr target is turned on, the bias voltage is adjusted to 60V, the HIPIMS voltage is 2000V, the current is 500A, and the sputtering power is 10Kw. The bottom stage time is set to 600 seconds;
D)CrN过渡层制备：D) Preparation of CrN transition layer:
Cr底层制备完成后，腔体气压设定为0.5Pa，通入反应气体N2，N2通量设定为20sccm，Ar通量保持不变，腔体气压设定为2Pa，调整偏压到60V，HIPIMS电压为2000V，电流500A，溅射功率10Kw，在Cr底层上制备CrN过渡层，持续900s；After the preparation of the Cr bottom layer is completed, the chamber pressure is set to 0.5Pa, the reaction gas N2 is introduced, the N2 flux is set to 20sccm, the Ar flux remains unchanged, the chamber pressure is set to 2Pa, and the bias voltage is adjusted to 60V, HIPIMS voltage is 2000V, current is 500A, sputtering power is 10Kw, and a CrN transition layer is prepared on the Cr bottom layer for 900s;
E)CrN2过渡层制备：E) Preparation of CrN2 transition layer:
将N2通量设定为20sccm，溅射时间为840s，其余参数与CrN过渡层制备参数一致； The N flux is set to 20sccm, the sputtering time is 840s, and the rest of the parameters are consistent with the preparation parameters of the CrN transition layer;
F)Cr+C过渡层制备：F) Preparation of Cr+C transition layer:
关闭N2通道，启动双极脉冲电源，将功率设定为10KW，持续溅射900s，其余参数与CrN过渡层制备参数一致；Close the N2 channel, start the bipolar pulse power supply, set the power to 10KW, and continue sputtering for 900s, and the rest of the parameters are consistent with those for the preparation of the CrN transition layer;
G)掺Cr的DLC涂层的制备：G) Preparation of Cr-doped DLC coating:
在CrN过渡层制备完成后，关闭N2通道，通入C2N2作为反应气体，C2H2流量控制为60sccm；该溅射阶段膜系设计为三层，每层溅射时间为900s，溅射功率分别为10Kw、7Kw、4Kw，腔体气压设定为2Pa，调整偏压到60V，HIPIMS电压为2000V，电流500A；After the preparation of the CrN transition layer is completed, the N2 channel is closed, C2N2 is introduced as the reaction gas, and the flow rate of C2H2 is controlled to 60 sccm ; the film system of this sputtering stage is designed as three layers, and the sputtering time of each layer is 900s , the sputtering power is 10Kw, 7Kw, 4Kw respectively, the chamber pressure is set to 2Pa, the bias voltage is adjusted to 60V, the HIPIMS voltage is 2000V, and the current is 500A;
进一步的，所述钨钴合金基体通过超声波清洗、超声碱洗、酸洗，去离子水清洗后用吹风机吹干。Further, the tungsten-cobalt alloy substrate is cleaned by ultrasonic cleaning, ultrasonic alkali cleaning, pickling, and deionized water, and then dried with a hair dryer.
进一步的，所述掺杂Cr的DLC涂层的厚度为1.45μm。Further, the thickness of the Cr-doped DLC coating is 1.45 μm.
本发明充分利用了高功率脉冲磁控溅射膜层光洁度、均匀度、致密度高的优点，为改善DLC涂层结合力和膜层韧性差的缺点，采用了底层和过渡层设计方法。这一独特的膜系设计和参杂工艺既保证了涂层结合力的提高，又保证了涂层沉积速率、涂层致密性和耐磨减摩性能的提高。采用本发明的方法制备的掺Cr的DLC涂层外观呈灰黑色，表面光滑致密，涂层的硬度32GPa，膜基结合力达到72N，涂层厚度为1.45μm。涂层的干摩擦系数为0.2。表明掺Cr的DLC涂层具有良好的耐磨和减摩性能。The present invention makes full use of the advantages of high-power pulse magnetron sputtering film smoothness, uniformity and high density, and adopts the bottom layer and transition layer design method in order to improve the shortcomings of DLC coating bonding force and poor film toughness. This unique film system design and doping process not only ensure the improvement of coating adhesion, but also ensure the improvement of coating deposition rate, coating compactness and wear resistance and friction reduction performance. The appearance of the Cr-doped DLC coating prepared by the method of the present invention is gray-black, the surface is smooth and compact, the hardness of the coating is 32GPa, the bonding force of the film base reaches 72N, and the coating thickness is 1.45 μm. The dry friction coefficient of the coating is 0.2. It shows that the Cr-doped DLC coating has good wear resistance and antifriction properties.
附图说明Description of drawings
图1为纳米氧化锆粉体的微观形貌图；Fig. 1 is the microscopic topography figure of nanometer zirconia powder;
图2为2000倍涂层断面SEM图；Figure 2 is a SEM image of the coating section at 2000 times;
图3为40000倍涂层表面微观结构图；Figure 3 is a microstructure diagram of the coating surface at 40,000 times;
图4为Ballcrater测试下多层膜系结构设计截面图；Figure 4 is a cross-sectional view of the multilayer film structure design under the Ballcrater test;
图5为本发明在刀具上的实施；Fig. 5 is the implementation of the present invention on the cutter;
图6为本发明在钻头上的实施。Figure 6 shows the implementation of the invention on a drill bit.
具体实施方式Detailed ways
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。The above-mentioned contents of the present invention are described in further detail below through the embodiments, but this should not be interpreted as the scope of the above-mentioned themes of the present invention being limited to the following embodiments, and all technologies realized based on the above-mentioned contents of the present invention all belong to the scope of the present invention.
实施例1Example 1
本实施例的掺杂Cr的DLC涂层的制备方法，包括下列步骤：The preparation method of the Cr-doped DLC coating of the present embodiment comprises the following steps:
步骤S1:将表面处理好的钨钴合金基体放入溅射设备腔体的转架杆上，该转架整体转动的同时，转架杆自转，以保证涂层的均匀性；Step S1: Put the surface-treated tungsten-cobalt alloy substrate on the turret rod of the sputtering equipment cavity, and when the turret rotates as a whole, the turret rod rotates to ensure the uniformity of the coating;
步骤S2:以长柱型Cr靶作为参杂源，以长住型石墨靶作为碳元素的来源，平面Cr靶为参杂Cr元素来源，均匀分布并安装在炉体内壁上，采用高纯Ar作为主要离化气体，保证有效的辉光放电过程；分别采用Cr层作为打底层、CrN、CrN2、Cr+C作为梯度过渡层，高纯N2作为过渡层反应气体，C2H2作为DLC层反应气体，形成Cr、CrN、CrN2、Cr+C、α-C：H的多层膜系涂层；Step S2: Use the long-column Cr target as the doping source, the long-lived graphite target as the source of the carbon element, and the flat Cr target as the source of the doping Cr element, which is evenly distributed and installed on the inner wall of the furnace, using high-purity Ar As the main ionized gas to ensure an effective glow discharge process; respectively use Cr layer as the bottom layer, CrN, CrN 2 , Cr+C as the gradient transition layer, high-purity N 2 as the transition layer reaction gas, and C 2 H 2 as the transition layer. The DLC layer reacts with gas to form a multi-layer film system coating of Cr, CrN, CrN 2 , Cr+C, α-C:H;
步骤S3:制备工艺条件：Step S3: preparation process conditions:
A)等离子体洗靶：A) Plasma washing target:
靶体装入真空室后，抽真空并加热到真空室温度为400℃。通入200sccm的Ar到真空室，开偏压至1000V，炉体内气压为2Pa，对真空室的靶体表面进行轰击清洗，持续800s；After the target body is loaded into the vacuum chamber, it is evacuated and heated to a temperature of 400°C in the vacuum chamber. Introduce 200 sccm of Ar into the vacuum chamber, turn on the bias voltage to 1000V, and the air pressure in the furnace is 2Pa, and bombard and clean the surface of the target body in the vacuum chamber for 800s;
B)等离子体清洗基体：B) Plasma cleaning of the substrate:
基体装入真空室后，抽真空并加热到真空室温度为400℃。通入200sccm的Ar到真空室，开偏压至1000V，炉体内气压为2Pa，对真空室的靶体表面进行轰击清洗，持续1940s；After the substrate was loaded into the vacuum chamber, it was evacuated and heated to a vacuum chamber temperature of 400°C. Introduce 200sccm Ar into the vacuum chamber, turn on the bias voltage to 1000V, and the air pressure in the furnace is 2Pa, and bombard and clean the surface of the target body in the vacuum chamber for 1940s;
C)Cr底层制备：C) Preparation of Cr bottom layer:
腔体温度设定400度，调节Ar通量到200sccm、腔体气压设定为2Pa，然后开启柱弧Cr靶，调整偏压到60V，HIPIMS电压为2000V，电流500A，溅射功率10Kw，打底层阶段时间设定为600秒；The chamber temperature is set to 400 degrees, the Ar flux is adjusted to 200sccm, the chamber pressure is set to 2Pa, then the column arc Cr target is turned on, the bias voltage is adjusted to 60V, the HIPIMS voltage is 2000V, the current is 500A, and the sputtering power is 10Kw. The bottom stage time is set to 600 seconds;
D)CrN过渡层制备：D) Preparation of CrN transition layer:
Cr底层制备完成后，腔体气压设定为0.5Pa，通入反应气体N2，N2通量设定为20sccm，Ar通量保持不变，腔体气压设定为2Pa，调整偏压到60V，HIPIMS电压为2000V，电流500A，溅射功率10Kw，在Cr底层上制备CrN过渡层，持续900s；After the preparation of the Cr bottom layer is completed, the chamber pressure is set to 0.5Pa, the reaction gas N2 is introduced, the N2 flux is set to 20sccm, the Ar flux remains unchanged, the chamber pressure is set to 2Pa, and the bias voltage is adjusted to 60V, HIPIMS voltage is 2000V, current is 500A, sputtering power is 10Kw, and a CrN transition layer is prepared on the Cr bottom layer for 900s;
E)CrN2过渡层制备：E) Preparation of CrN2 transition layer:
将N2通量设定为20sccm，溅射时间为840s，其余参数与CrN过渡层制备参数一致； The N flux is set to 20sccm, the sputtering time is 840s, and the rest of the parameters are consistent with the preparation parameters of the CrN transition layer;
F)Cr+C过渡层制备：F) Preparation of Cr+C transition layer:
关闭N2通道，启动双极脉冲电源，将功率设定为10KW，持续溅射900s，其余参数与CrN过渡层制备参数一致；Close the N2 channel, start the bipolar pulse power supply, set the power to 10KW, and continue sputtering for 900s, and the rest of the parameters are consistent with those for the preparation of the CrN transition layer;
G)掺Cr的DLC涂层的制备：G) Preparation of Cr-doped DLC coating:
在CrN过渡层制备完成后，关闭N2通道，通入C2N2作为反应气体，C2H2流量控制为60sccm；该溅射阶段膜系设计为三层，每层溅射时间为900s，溅射功率分别为10Kw、7Kw、4Kw，腔体气压设定为2Pa，调整偏压到60V，HIPIMS电压为2000V，电流500A；After the preparation of the CrN transition layer is completed, the N2 channel is closed, C2N2 is introduced as the reaction gas, and the flow rate of C2H2 is controlled to 60 sccm ; the film system of this sputtering stage is designed as three layers, and the sputtering time of each layer is 900s , the sputtering power is 10Kw, 7Kw, 4Kw respectively, the chamber pressure is set to 2Pa, the bias voltage is adjusted to 60V, the HIPIMS voltage is 2000V, and the current is 500A;
进一步的，所述钨钴合金基体通过超声波清洗、超声碱洗、酸洗，去离子水清洗后用吹风机吹干。Further, the tungsten-cobalt alloy substrate is cleaned by ultrasonic cleaning, ultrasonic alkali cleaning, pickling, and deionized water, and then dried with a hair dryer.
进一步的，所述掺杂Cr的DLC涂层的厚度为1.45μm。Further, the thickness of the Cr-doped DLC coating is 1.45 μm.
涂层结合界面如图2所示，厚度为1.45μm，组织致密，与基体结合紧密。图3为放大40000倍后涂层表面的微观结构，涂层颗粒结合紧密，致密度高。Ballcrater测试下多层膜系结构设计截面图如图4所示，图中可看到多层膜系结构具有层次性，层间界面清晰。The bonding interface of the coating is shown in Figure 2, with a thickness of 1.45 μm, a dense structure, and a tight bond with the substrate. Figure 3 shows the microstructure of the coating surface after magnification of 40,000 times. The coating particles are tightly combined and dense. The cross-sectional view of the multilayer film structure design under the Ballcrater test is shown in Figure 4. In the figure, it can be seen that the multilayer film structure is hierarchical and the interface between layers is clear.
以上实施例描述了本发明的主要特征及优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。The above embodiments have described the main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. What are described in the above embodiments and description are only to illustrate the principle of the present invention, without departing from the present invention. Under the scope of the principles of the invention, the present invention will also have various changes and improvements, and these changes and improvements all fall within the protection scope of the present invention.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114686829A (en) * | 2020-12-29 | 2022-07-01 | 苏州吉恒纳米科技有限公司 | Wear-resistant, fatigue-resistant and repeated impact-resistant coating and production process thereof |
| CN117568764A (en) * | 2023-11-16 | 2024-02-20 | 东北大学 | A method to improve the deposition rate of ta-C coating prepared by high-power pulse magnetron sputtering technology |
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