CN115537750A - 一种N和Ta离子注入钛合金改性涂层及其制备方法与应用 - Google Patents
一种N和Ta离子注入钛合金改性涂层及其制备方法与应用 Download PDFInfo
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- 238000005468 ion implantation Methods 0.000 title claims abstract description 40
- 238000000576 coating method Methods 0.000 title claims abstract description 37
- 239000011248 coating agent Substances 0.000 title claims abstract description 36
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 9
- 239000007924 injection Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000013077 target material Substances 0.000 claims description 4
- 229910000883 Ti6Al4V Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000002513 implantation Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 7
- 239000000758 substrate Substances 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
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- 238000012986 modification Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000004372 laser cladding Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000006467 substitution reaction 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
- C23C14/48—Ion implantation
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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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
- C23C14/06—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
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic 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
- 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
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Abstract
本发明属于生物植入材料技术领域，特别涉及一种N和Ta离子注入钛合金改性涂层及其制备方法与应用。本发明在钛合金表面进行N离子注入和Ta离子注入，然后在完成离子注入后的钛合金表面进行磁控溅射Ta，最终得到钛合金改性涂层。所得涂层具有良好的机械性能，并且与基体具有优异的结合力。
Description
技术领域
本发明属于生物植入材料技术领域，特别涉及一种N和Ta离子注入钛合金改性涂层及其制备方法与应用。
背景技术
目前，在钛合金表面制备减摩耐磨涂层是解决钛合金耐磨性差的最有效方法之一。减摩耐磨涂层一般是指摩擦系数低、磨损量小的摩擦涂层。通过改变其微观结构或在表面生成金属化合物和陶瓷来增强摩擦副耐磨性的能够减少或控制摩擦和磨损，如离子注入、激光熔覆、激光喷丸、表面氮化、微弧氧化等。但传统的单一结构涂层在体内环境存在局限性。因此不同表面复合改性技术制备的多相、多层次、多尺度混合增强涂层，可以充分发挥涂层中不同相之间的协同、耦合和多功能响应机制。
离子注入技术中加速的离子被引导到目标材料的表面，但离子注入在材料表面的穿透深度一般只有100～500nm。涂层太薄改性层会完全损坏。另外在磨损过程中摩擦副与基体直接接触，磨损的改性层产生的硬质颗粒会加剧基体的磨损，从而导致涂层失效。并且基材与涂层的结合力也会影响涂层的保护性能。
发明内容
为了克服上述现有技术的缺点与不足，本发明的首要目的在于提供一种N和Ta离子注入钛合金改性涂层的制备方法。
本发明另一目的在于提供上述方法制得的N和Ta离子注入钛合金改性涂层。
本发明再一目的在于提供所述N和Ta离子注入钛合金改性涂层在制备减摩耐磨材料中的应用。
本发明的目的通过下述方案实现：
一种N和Ta离子注入钛合金改性涂层的制备方法，包括以下步骤：
在钛合金表面进行N离子注入和Ta离子注入，然后在完成离子注入后的钛合金表面进行磁控溅射Ta，最终得到钛合金改性涂层。
所述钛合金为Ti6Al4V、Ti、Ti-2Al-2.5Zr或Ti-5Al-2.5Sn。
注入前对钛合金进行表面去油处理。
所述N离子注入时的真空压力为2×10-4～5×10-4Pa，电压为50～80Kv，注入计量为2×1017～8×1017ion/cm2。优选地，真空压力为5×10-4Pa，电压为60Kv，注入计量为5×1017ion/cm2。
所述Ta离子注入时的真空压力为2×10-4～5×10-4Pa，电压为40～70Kv，注入计量为2×1017～8×1017ion/cm2。优选地，真空压力为5×10-4Pa，电压为50Kv，注入计量为5×1017ion/cm2。
磁控溅射Ta的具体操作为用纯Ta靶材，将真空腔体抽至5×10-4Pa，并加热腔室温度至200-400℃，电源功率为1800-2000W，磁控溅射的同时通入氩气。磁控溅射时间2-6h。
一种N和Ta离子注入钛合金改性涂层，通过上述方法制备得到。
所述N和Ta离子注入钛合金改性涂层在制备减摩耐磨材料中的应用。
本发明相对于现有技术，具有如下的优点及有益效果：
通过离子注入在钛合金表面先形成了TaN层，N和Ta同时注入可以形成TaN0.1的相，TaN0.1有利于提高与基材的结合能力。
在离子注入后的涂层上进行磁控溅射，所制备涂层中包含2种Ta的相结构。一般磁控溅射初期，温度较低时会生成β-Ta，导致涂层硬而脆。β-Ta晶格常数与基材的匹配度是较差的，容易造成界面结合较弱，涂层剥落。但β-Ta属于亚稳相，离子注入时形成TaN0.1不稳定相，在磁控溅射高温过程中，使离子注入涂层中少量的N渗出，N渗出量比较少，不至于氮化磁控溅射的涂层，但可以确保β-Ta相减少，生成的α-Ta相增多，提高涂层韧性，提高Ta涂层的硬度。
同时，N可以使Ta原子的溅射逸出功增大，从而进一步导致运动到基体表面的吸附Ta原子活动能力降低，形核率提高，促使晶粒细化，进一步增加涂层强度。
具体实施方式
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例中所用试剂如无特殊说明均可从市场常规购得。
实施例1
一种N和Ta离子注入钛合金表面耐磨涂层的制备方法，包括以下步骤：
(1)对Ti6Al4V合金表面打磨抛光，随后在乙醇中超声清洗，烘干备用。
(2)先进行N离子注入，真空压力为4×10-4Pa，电压为60Kv，注入剂量为5×1017ion/cm2。随后离子注入Ta元素，真空压力为4×10-4Pa，电压为50Kv，注入剂量为5×1017ion/cm2。离子注入Ta时，将氩气(Ar)以6sccm(标准立方厘米每分钟)的流速引入阴极电弧源。
(3)磁控溅射Ta
磁控溅射Ta的具体操作为用纯Ta靶材，将真空腔体抽至5×10-4Pa，并加热腔室温度至400℃，电源功率为2000W，磁控溅射的同时通入氩气，磁控溅射时间4h。
对比例1
本对比例与实施例1的区别在于，仅进行N离子注入。
对比例2
本对比例与实施例1的区别在于，仅进行N离子注入和Ta离子注入。
对比例3
本对比例与实施例1的区别在于，仅进行磁控溅射Ta。
对比例4
本对比例与实施例1的区别在于，仅进行N离子注入和磁控溅射Ta。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (10)
1.一种N和Ta离子注入钛合金改性涂层的制备方法，其特征在于包括以下步骤：
在钛合金表面进行N离子注入和Ta离子注入，然后在完成离子注入后的钛合金表面进行磁控溅射Ta，最终得到钛合金改性涂层。
2.根据权利要求1所述的制备方法，其特征在于：所述N离子注入时的真空压力为2×10-4～5×10-4Pa，电压为50～80Kv，注入计量为2×1017～8×1017ion/cm2。
3.根据权利要求1所述的制备方法，其特征在于：所述N离子注入时的真空压力为5×10-4Pa，电压为60Kv，注入计量为5×1017ion/cm2。
4.根据权利要求1所述的制备方法，其特征在于：所述Ta离子注入时的真空压力为2×10-4～5×10-4Pa，电压为40～70Kv，注入计量为2×1017～8×1017ion/cm2。
5.根据权利要求1所述的制备方法，其特征在于：所述Ta离子注入时的真空压力为5×10-4Pa，电压为50Kv，注入计量为5×1017ion/cm2。
6.根据权利要求1所述的制备方法，其特征在于：磁控溅射Ta的具体操作为用纯Ta靶材，将真空腔体抽至5×10-4Pa，并加热腔室温度至200-400℃，电源功率为1800-2000W，磁控溅射的同时通入氩气。
7.根据权利要求1所述的制备方法，其特征在于：所述磁控溅射时间2-6h。
8.根据权利要求1所述的制备方法，其特征在于：所述钛合金为Ti6Al4V、Ti、Ti-2Al-2.5Zr或Ti-5Al-2.5Sn。
9.一种N和Ta离子注入钛合金改性涂层，通过权利要求1～8任一项所述方法制备得到。
10.根据权利要求9所述的N和Ta离子注入钛合金改性涂层在制备减摩耐磨材料中的应用。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020053997A (ko) * | 2000-12-26 | 2002-07-06 | 신현준 | 스퍼터링에 의한 탄탈륨 피막의 형성방법 |
| RU2008135603A (ru) * | 2008-09-02 | 2010-03-10 | Общество с ограниченной ответственностью Научно-производственное предприятие "Уралавиаспецтехнология" (RU) | Способ получения ионно-плазменного нанослойного покрытия на лопатках турбомашин из титановых сплавов |
| CN102181842A (zh) * | 2011-04-14 | 2011-09-14 | 中国科学院上海硅酸盐研究所 | 一种对钛金属表面进行改性的方法 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020053997A (ko) * | 2000-12-26 | 2002-07-06 | 신현준 | 스퍼터링에 의한 탄탈륨 피막의 형성방법 |
| RU2008135603A (ru) * | 2008-09-02 | 2010-03-10 | Общество с ограниченной ответственностью Научно-производственное предприятие "Уралавиаспецтехнология" (RU) | Способ получения ионно-плазменного нанослойного покрытия на лопатках турбомашин из титановых сплавов |
| CN102181842A (zh) * | 2011-04-14 | 2011-09-14 | 中国科学院上海硅酸盐研究所 | 一种对钛金属表面进行改性的方法 |
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| Title |
|---|
| 李建萍 等: "钽的氮离子注入法研究", 《表面技术》, vol. 24, no. 6, 31 December 1995 (1995-12-31), pages 16 - 22 * |
| 赵青 等: "升温Ta+N双注入对硬质合金性能的影响", 《核聚变与等离子体物理》, vol. 22, no. 1, 31 March 2002 (2002-03-31), pages 61 - 64 * |
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