WO2021114068A1 - Preparation method for tin coating on titanium alloy part of aircraft engine - Google Patents

Preparation method for tin coating on titanium alloy part of aircraft engine Download PDF

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Publication number
WO2021114068A1
WO2021114068A1 PCT/CN2019/124208 CN2019124208W WO2021114068A1 WO 2021114068 A1 WO2021114068 A1 WO 2021114068A1 CN 2019124208 W CN2019124208 W CN 2019124208W WO 2021114068 A1 WO2021114068 A1 WO 2021114068A1
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titanium alloy
arc
tin coating
parts
aeroengine
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PCT/CN2019/124208
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French (fr)
Chinese (zh)
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王悦欣
敖斌
李昌
郭向民
杨斌
桂培培
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中国航发贵州黎阳航空动力有限公司
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Priority to PCT/CN2019/124208 priority Critical patent/WO2021114068A1/en
Publication of WO2021114068A1 publication Critical patent/WO2021114068A1/en

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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
    • C23C14/02—Pretreatment of the material to be coated
    • 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
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • 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
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/04—Treatment of selected surface areas, e.g. using masks
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding

Definitions

  • the invention belongs to the technical field of heat treatment and surface engineering, and relates to a process method for physical vapor deposition of TiN wear-resistant coatings on titanium alloy parts of aeroengines.
  • the purpose of the present invention is to overcome the deficiencies in the prior art and provide a method for preparing TiN coatings on titanium alloy parts of aeroengines, which can control the deformation of the parts, reduce the process cycle and increase the wear resistance of the parts.
  • the basic idea of the invention is: after the surface of the part to be sprayed is processed to the final size, blow sand, clean the part, put the part into the fixture, the internal dimension of the fixture is the same as the external dimension of the part, tighten the screws, and put the parts with the fixture into the furnace ; First deposit a high Ti transition layer from Ti to TiN on the surface of the substrate to improve the bonding strength between the multilayer film and the substrate; perform etching according to the parameters; then deposit the TiN coating.
  • the utility model relates to a titanium alloy part of an aircraft engine, and the surface of the titanium alloy part is partially covered with a TiN coating.
  • the TiN coating is obtained by ion nitridation combined with physical vapor deposition.
  • a preparation method of TiN coating on titanium alloy parts of aeroengine including:
  • Step 1 spray surface pretreatment and non-spray surface protection treatment
  • Step two pretreatment of the surface of the part, ion nitriding is used to form a layer of TiN, Ti 2 N-rich underlayer on the surface of the titanium alloy substrate.
  • Step three etching, including glow discharge gas ion bombardment and cathodic arc Ti ion bombardment;
  • Step four deposit TiN layer.
  • the spray surface pretreatment includes sandblasting, water washing, surface degreasing and drying in sequence.
  • the sandblasting is wet sandblasting, using Al 2 O 3 particles of 500 meshes, and the sandblasting wind pressure is 2-5 bar; the surface degreasing adopts ultrasonic cleaning; the drying temperature of the drying is 150 °C ⁇ 180°C, drying time is 1h ⁇ 2h.
  • the non-sprayed surface protection treatment adopts a clamp to shield the non-sprayed surface.
  • the clamp includes a hook, a first arc-shaped part and a second arc-shaped part, and the first arc-shaped part and the second arc-shaped part form a complete ring.
  • the shape of the inner ring surface matches the shape of the non-sprayed surface of the titanium alloy part, one end of the first arc-shaped part and the second arc-shaped part are hinged to each other, and the other end is detachably connected by screws.
  • the nitriding furnace starts to be vacuumed.
  • the vacuum pump is turned off and the leakage rate of the nitriding furnace is checked to ensure Air leakage rate ⁇ 0.13Pa/min.
  • the vacuum chamber is flushed with NH 3 several times. Under the right amount of NH 3 flow rate, heat the parts to 600°C and keep the temperature for 30min ⁇ 60min. During the heat preservation process, the NH 3 flow rate is 1.0L/min ⁇ 2.0L/min.
  • the bombardment time is 40min-50min
  • the pressure in the vacuum chamber is 2.0Pa-3.0Pa
  • the cathode arc Ti ion bombards the Ti target current is 60A-80A
  • the bombardment time It is 15min-20min
  • the pressure in the vacuum chamber during bombardment is 0.5-0.6MPa.
  • the Ti target current is 70A-90A
  • the N 2 flow rate is 700 sccm
  • the deposition time is 180 min-250 min
  • the pressure in the vacuum chamber is 1.0-1.2 Pa.
  • the core of the present invention is to first prepare a TiN and Ti 2 N-rich bottom layer on the surface of a titanium alloy part by using an ion nitriding method, and then deposit a TiN layer by a physical vapor deposition method.
  • the TiN coating preparation method of the present invention is applicable to all titanium alloy materials without limitation; the ion nitriding preparation transition layer in the present invention is mainly used for bottoming, which relieves the hardness and deformation mutation between the titanium alloy substrate and TiN, and increases Bonding force, the thickness of the transition layer is small (about 5 ⁇ m); etching is mainly used to clean the surface of the part, remove the slight oxide film and oil stain on the surface of the part, and prevent insufficient bonding force in the later stage.
  • the TiN and Ti 2 N transition layer prepared by the ion nitriding method is diffused from the substrate by chemical heat treatment, and the bonding force is far better than the transition layer prepared by physical vapor deposition methods such as multi-arc ion plating. ;
  • the depth of the TiN and Ti 2 N transition layer prepared by ion nitriding is much lower than that of the titanium alloy ion nitriding layer, and the deformation is controllable;
  • the method of titanium alloy ion nitriding + PVD composite treatment can meet the performance of anti-friction and wear and fretting friction required during the use of titanium alloy parts.
  • the present invention not only guarantees the wear resistance requirements of the parts, but also reduces the deformation of the parts.
  • the preparation time of the TiN coating on the surface of the titanium alloy is reduced from the original 40 hours to 8 hours, which greatly reduces the process. Cycle (using the method of the present invention, the current processing cycle is 8 hours), which saves production costs and improves production efficiency. After wear resistance test and trial run assessment, the coating has good binding force and the wear resistance meets the long-term use requirements of parts.
  • Figure 1 is a schematic diagram of the deposition position of the parts
  • Figure 2 is a schematic diagram of the assembly of the shielding fixture and parts
  • Figure 3 is a front view of the fixture
  • Figure 4 is a left side view of Figure 3;
  • titanium alloy bearing seats and bearing bushing parts in aero engines are partially covered with TiN coating on the surface of the parts through ion nitriding and physical vapor deposition.
  • the deposition position of the ring part is indicated by the letters E and F in the figure.
  • a method for preparing TiN coating on titanium alloy parts of aeroengine, and its steps are as follows:
  • Spraying surface pretreatment Wet sandblasting is used to pretreat the sprayed surface to increase the bonding strength between the film and the substrate.
  • the sandblasting uses 500 mesh Al 2 O 3 particles, and the sandblasting wind pressure is (2 ⁇ 5)bar;
  • Ultrasonic cleaning is used to remove residues and recontaminants such as oil stains, grease, rust, residual cleaning agents and water stains on the surface of the parts;
  • Parts drying parts are dried in a drying box, the drying temperature is 150°C ⁇ 180°C, and the drying time is 1h ⁇ 2h;
  • the fixture 2 includes a hook, a first arc-shaped part and a second arc-shaped part.
  • the first arc-shaped part and the second arc-shaped part form a complete ring ,
  • the hook is connected to the outside of the first arc-shaped part, the inner ring surface shape of the first arc-shaped part and the second arc-shaped part matches the shape of the non-sprayed surface of the titanium alloy part, one end of the first arc-shaped part and the second arc-shaped part Hinge each other, the other end can be detachably connected with the screw 3, put the part 1 into the fixture 2, tighten the screw 3, and shield the non-painted surface;
  • Glow discharge gas ion bombardment The bombardment time is 40min-50min, and the pressure in the vacuum chamber is 2.0Pa ⁇ 3.0Pa;
  • Cathodic arc Ti ion bombardment Ti target current is 60A ⁇ 80A, bombardment time is 15min ⁇ 20min, and the pressure in the vacuum chamber during bombardment is 0.5 ⁇ 0.6MPa;
  • the Ti target current is 70A ⁇ 90A
  • the N 2 flow rate is 700sccm
  • the deposition time is 180min ⁇ 250min
  • the pressure in the vacuum chamber is 1.0 ⁇ 1.2Pa;
  • Coating quality inspection including appearance, thickness, hardness, adhesion, etc.
  • the invention adopts a special and simple physical vapor deposition TiN wear-resistant coating method suitable for engine titanium alloy parts according to the structural characteristics of parts of titanium alloy bearing seats, bearing bushes, mounting rings and other types of parts, which not only ensures the later stage of the parts
  • the requirements for wear resistance ensure the size of the parts, save time and reduce production costs.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

Disclosed in the present invention is a preparation method for a TiN coating on a titanium alloy part of an aircraft engine, comprising: after a surface of a part to be sprayed is machined to a final size, performing sand blasting; cleaning the part; putting the part into a clamp, wherein the inner size of the clamp is the same as the outer size of the part; screwing a screw; putting the part on which the clamp is mounted into an ion nitriding furnace; first generating a bottom layer rich in TiN and Ti2N on the surface of a substrate according to parameters, so as to improve the bonding strength between a multilayer film and the substrate; then putting the part on which the clamp is mounted into a deposition device; performing etching according to the parameters; and then depositing the TiN coating. The coating preparation method of the present invention controls the deformation of the titanium alloy part, reduces the coating process period, and increases the wear resistance of the part.

Description

一种航空发动机钛合金零件TiN涂层制备方法Preparation method of TiN coating on titanium alloy parts of aeroengine 技术领域Technical field
本发明属于热处理和表面工程技术领域，涉及航空发动机钛合金零件物理气相沉积TiN耐磨涂层的工艺方法。The invention belongs to the technical field of heat treatment and surface engineering, and relates to a process method for physical vapor deposition of TiN wear-resistant coatings on titanium alloy parts of aeroengines.
背景技术Background technique
在航空发动机中，由于轻量化、抗腐蚀等需要，会使用到大量钛合金轴承座、轴承衬套、安装环等类型零件，对耐磨性及零件加工精度要求很高。但是传统的气相渗氮及离子氮化方法在保证钛合金渗层组织的情况下无法保证零件精密加工、后期变形很大，采用预留研磨余量的方法控制零件变形易造成氮化层不均匀减薄，影响产品质量，同时传统的气相渗氮及离子氮化方法加工周期长、约40余小时，影响产品加工交付进度。In aero engines, due to the needs of light weight and corrosion resistance, a large number of titanium alloy bearing seats, bearing bushes, mounting rings and other types of parts are used, which require high wear resistance and parts processing accuracy. However, the traditional gas phase nitriding and ion nitriding methods cannot guarantee the precision machining of the parts while ensuring the structure of the titanium alloy layer. The later deformation is very large. The method of using reserved grinding allowance to control the deformation of the parts can easily cause the uneven nitride layer. Thinning affects product quality. At the same time, the traditional gas-phase nitriding and ion nitriding methods have a long processing cycle of about 40 hours, which affects the progress of product processing and delivery.
发明内容Summary of the invention
本发明的目的是，克服现有技术中的不足，提供一种航空发动机钛合金零件TiN涂层制备方法，控制零件变形、减少工艺周期、增加零件耐磨性。The purpose of the present invention is to overcome the deficiencies in the prior art and provide a method for preparing TiN coatings on titanium alloy parts of aeroengines, which can control the deformation of the parts, reduce the process cycle and increase the wear resistance of the parts.
为了实现上述目的，本发明采用以下技术方案：In order to achieve the above objectives, the present invention adopts the following technical solutions:
本发明的基本思路是：零件待喷涂表面加工到最终尺寸后，吹砂、清洗零件，将零件放入夹具，夹具内部尺寸与零件外部尺寸相同，拧紧螺钉，将装好夹具的零件入炉中；先在基体表面沉积一层Ti过渡到TiN的高Ti过渡层，以提高多层膜与基体之间的结合强度；按参数进行刻蚀；然后沉积TiN涂层。The basic idea of the invention is: after the surface of the part to be sprayed is processed to the final size, blow sand, clean the part, put the part into the fixture, the internal dimension of the fixture is the same as the external dimension of the part, tighten the screws, and put the parts with the fixture into the furnace ; First deposit a high Ti transition layer from Ti to TiN on the surface of the substrate to improve the bonding strength between the multilayer film and the substrate; perform etching according to the parameters; then deposit the TiN coating.
一种航空发动机钛合金零件，所述钛合金零件表面表面局部覆盖TiN涂层。The utility model relates to a titanium alloy part of an aircraft engine, and the surface of the titanium alloy part is partially covered with a TiN coating.
进一步，所述TiN涂层通过离子氮化配合物理气相沉积获得。Further, the TiN coating is obtained by ion nitridation combined with physical vapor deposition.
一种航空发动机钛合金零件TiN涂层制备方法，包括：A preparation method of TiN coating on titanium alloy parts of aeroengine, including:
步骤一，喷涂表面预处理和非喷涂表面防护处理； Step 1, spray surface pretreatment and non-spray surface protection treatment;
步骤二，零件表面预处理，采用离子氮化的方法在钛合金基体表面生成一层富含TiN、Ti 2N的底层。 Step two, pretreatment of the surface of the part, ion nitriding is used to form a layer of TiN, Ti 2 N-rich underlayer on the surface of the titanium alloy substrate.
步骤三，刻蚀，包括辉光放电气体离子轰击和阴极电弧Ti离子轰击；Step three, etching, including glow discharge gas ion bombardment and cathodic arc Ti ion bombardment;
步骤四，沉积TiN层。Step four, deposit TiN layer.
优选的，所述步骤一中，喷涂表面预处理包括依次进行的喷砂、水洗、表面 除油和烘干。Preferably, in the first step, the spray surface pretreatment includes sandblasting, water washing, surface degreasing and drying in sequence.
优选的，所述喷砂为湿喷砂，采用砂粒为500目的Al 2O 3颗粒，喷砂风压为2～5bar；所述表面除油采用超声波清洗；所述烘干的烘干温度150℃～180℃，烘干时间1h～2h。 Preferably, the sandblasting is wet sandblasting, using Al 2 O 3 particles of 500 meshes, and the sandblasting wind pressure is 2-5 bar; the surface degreasing adopts ultrasonic cleaning; the drying temperature of the drying is 150 ℃～180℃, drying time is 1h～2h.
进一步，所述步骤一中，非喷涂表面防护处理采用夹具屏蔽非喷涂表面。Further, in the first step, the non-sprayed surface protection treatment adopts a clamp to shield the non-sprayed surface.
进一步，所述夹具包括挂钩、第一弧形部件和第二弧形部件，且第一弧形部件和第二弧形部件组成完整的圆环，第一弧形部件和第二弧形部件的内环面形状与钛合金零件非喷涂表面形状匹配，第一弧形部件和第二弧形部件的一端相互铰接，另一端通过螺钉可拆卸连接。Further, the clamp includes a hook, a first arc-shaped part and a second arc-shaped part, and the first arc-shaped part and the second arc-shaped part form a complete ring. The shape of the inner ring surface matches the shape of the non-sprayed surface of the titanium alloy part, one end of the first arc-shaped part and the second arc-shaped part are hinged to each other, and the other end is detachably connected by screws.
进一步，所述步骤二中，零件表面预处理时，零件室温装入真空离子氮化炉后，氮化炉开始抽真空，抽至<1Pa后，关闭真空泵，检验氮化炉漏气率，保证空气漏气率<0.13Pa/min。当漏气率满足要求后，充NH 3数次冲洗真空室。在适量的NH 3流量下，加热零件至600℃，保温30min～60min，保温过程中NH 3流量为1.0L/min～2.0L/min。保温结束后，用纯N 2替换炉内气体，并缓慢降温至550℃，以防止零件在降温过程中大量吸氢，造成氢脆。在适量的N 2气氛下，由550℃缓慢降至100℃以下出炉。 Further, in the second step, during the surface pretreatment of the parts, after the parts are put into the vacuum ion nitriding furnace at room temperature, the nitriding furnace starts to be vacuumed. After pumping to <1Pa, the vacuum pump is turned off and the leakage rate of the nitriding furnace is checked to ensure Air leakage rate <0.13Pa/min. When the air leakage rate meets the requirements, the vacuum chamber is flushed with NH 3 several times. Under the right amount of NH 3 flow rate, heat the parts to 600°C and keep the temperature for 30min～60min. During the heat preservation process, the NH 3 flow rate is 1.0L/min～2.0L/min. After the heat preservation is over, replace the furnace gas with pure N 2 and slowly lower the temperature to 550°C to prevent the parts from absorbing a large amount of hydrogen during the cooling process, causing hydrogen embrittlement. In an appropriate amount of N 2 atmosphere, slowly drop from 550°C to below 100°C and release.
进一步，所述步骤三中，辉光放电气体离子轰击时，轰击时间为40min～50min，真空室内的压强为2.0Pa～3.0Pa；阴极电弧Ti离子轰击时，Ti靶电流60A～80A，轰击时间为15min～20min，轰击时真空室内的压强为0.5～0.6MPa。Further, in the step three, when the glow discharge gas ion bombards, the bombardment time is 40min-50min, the pressure in the vacuum chamber is 2.0Pa-3.0Pa; when the cathode arc Ti ion bombards, the Ti target current is 60A-80A, the bombardment time It is 15min-20min, and the pressure in the vacuum chamber during bombardment is 0.5-0.6MPa.
进一步，所述步骤四中，沉积TiN层时，Ti靶电流70A～90A，N 2流量为700sccm，沉积时间为180min～250min，真空室内压强1.0～1.2Pa。 Further, in the fourth step, when depositing the TiN layer, the Ti target current is 70A-90A, the N 2 flow rate is 700 sccm, the deposition time is 180 min-250 min, and the pressure in the vacuum chamber is 1.0-1.2 Pa.
本发明的核心在于先采用离子氮化的方法在钛合金制件表面制备富含TiN、Ti 2N的底层，再采用物理气相沉积的方法沉积TiN层。 The core of the present invention is to first prepare a TiN and Ti 2 N-rich bottom layer on the surface of a titanium alloy part by using an ion nitriding method, and then deposit a TiN layer by a physical vapor deposition method.
本发明的TiN涂层制备方法适用于所有钛合金材料，无限制范围；本发明中离子氮化制备过渡层主要是打底用，缓解钛合金基材到TiN之间的硬度以及形变突变，增加结合力，过渡层厚度较小(5μm左右即可)；刻蚀主要是用来对零件表面进行清洁，去除制件表面轻微的氧化膜以及油污，防止后期结合力不足。The TiN coating preparation method of the present invention is applicable to all titanium alloy materials without limitation; the ion nitriding preparation transition layer in the present invention is mainly used for bottoming, which relieves the hardness and deformation mutation between the titanium alloy substrate and TiN, and increases Bonding force, the thickness of the transition layer is small (about 5μm); etching is mainly used to clean the surface of the part, remove the slight oxide film and oil stain on the surface of the part, and prevent insufficient bonding force in the later stage.
与单一的钛合金离子氮化或表面物理气相沉积TiN及TiN复合涂层方法相比，本发明主要优势如下：Compared with a single titanium alloy ion nitridation or surface physical vapor deposition TiN and TiN composite coating method, the main advantages of the present invention are as follows:
1.采用离子氮化的方法制备的TiN及Ti 2N过渡层与基体之间是通过化学热处理的方法扩散而成，结合力远远优于多弧离子镀等物理气相沉积方法制备的过渡层； 1. The TiN and Ti 2 N transition layer prepared by the ion nitriding method is diffused from the substrate by chemical heat treatment, and the bonding force is far better than the transition layer prepared by physical vapor deposition methods such as multi-arc ion plating. ；
2.采用离子氮化的方式制备的TiN及Ti 2N过渡层深度远远低于钛合金离子氮化渗层深度，变形可控； 2. The depth of the TiN and Ti 2 N transition layer prepared by ion nitriding is much lower than that of the titanium alloy ion nitriding layer, and the deformation is controllable;
3.采用钛合金离子氮化+PVD复合处理的方法所需要的工艺时间远远低于直接离子氮化，而且不存在离子氮化时渗层较深所易导致的表面脆性等问题；3. The process time required by the method of titanium alloy ion nitriding + PVD composite treatment is much lower than that of direct ion nitriding, and there are no problems such as surface brittleness caused by the deep infiltration layer during ion nitriding;
4.采用钛合金离子氮化+PVD复合处理的方法能够满足钛合金制件使用过程中所需要的抗摩擦磨损以及微动摩擦等性能。4. The method of titanium alloy ion nitriding + PVD composite treatment can meet the performance of anti-friction and wear and fretting friction required during the use of titanium alloy parts.
与传统的离子氮化工艺相比，本发明既保证了零件耐磨性要求，又降低了零件变形，将钛合金表面TiN涂层制备时间由原来的40余小时缩减至8h，大大缩减了工艺周期(采用本发明的方法目前加工周期为8小时)、节约了生产成本、提高了生产效率，经耐磨性试验及试车考核，涂层结合力良好，耐磨性满足零件长期使用要求。Compared with the traditional ion nitriding process, the present invention not only guarantees the wear resistance requirements of the parts, but also reduces the deformation of the parts. The preparation time of the TiN coating on the surface of the titanium alloy is reduced from the original 40 hours to 8 hours, which greatly reduces the process. Cycle (using the method of the present invention, the current processing cycle is 8 hours), which saves production costs and improves production efficiency. After wear resistance test and trial run assessment, the coating has good binding force and the wear resistance meets the long-term use requirements of parts.
附图说明Description of the drawings
图1为零件沉积位置示意图；Figure 1 is a schematic diagram of the deposition position of the parts;
图2为遮蔽夹具与零件的装配示意图；Figure 2 is a schematic diagram of the assembly of the shielding fixture and parts;
图3为夹具的主视图；Figure 3 is a front view of the fixture;
图4为图3的左视图；Figure 4 is a left side view of Figure 3;
图中，1零件；2夹具；3螺钉。In the figure, 1 part; 2 fixtures; 3 screws.
具体实施方式Detailed ways
下面结合说明书附图和实施例对本发明的构思做进一步详细说明。The concept of the present invention will be further described in detail below in conjunction with the drawings and embodiments of the specification.
本实施例中针对航空发动机中钛合金轴承座、轴承衬套类零件通过离子氮化和物理气相沉积在零件表面部分覆盖TiN涂层。如图1所示，该环形零件的沉积位置为图中字母E和F指示处。In this embodiment, titanium alloy bearing seats and bearing bushing parts in aero engines are partially covered with TiN coating on the surface of the parts through ion nitriding and physical vapor deposition. As shown in Figure 1, the deposition position of the ring part is indicated by the letters E and F in the figure.
一种航空发动机钛合金零件TiN涂层制备方法，其步骤：A method for preparing TiN coating on titanium alloy parts of aeroengine, and its steps are as follows:
(1)喷涂表面预处理：采用湿喷砂的方法对待喷涂表面进行预处理，增加膜层与基体结合强度，喷砂采用砂粒为500目的Al 2O 3颗粒，喷砂风压为(2～5)bar； (1) Spraying surface pretreatment: Wet sandblasting is used to pretreat the sprayed surface to increase the bonding strength between the film and the substrate. The sandblasting uses 500 mesh Al 2 O 3 particles, and the sandblasting wind pressure is (2～ 5)bar;
(2)水洗：对喷砂零件进行水洗，去除零件表面砂粒；(2) Washing: Wash the sandblasted parts with water to remove sand particles on the surface of the parts;
(3)零件表面除油：采用超声波清洗去除零件表面油污、油脂、水锈、残留清洗剂和水渍等残留物以及再污染物；(3) Degreasing on the surface of parts: Ultrasonic cleaning is used to remove residues and recontaminants such as oil stains, grease, rust, residual cleaning agents and water stains on the surface of the parts;
(4)零件烘干：采用烘干箱进行零件烘干，烘干温度150℃～180℃，烘干时间1h～2h；(4) Parts drying: parts are dried in a drying box, the drying temperature is 150℃～180℃, and the drying time is 1h～2h;
(5)非喷涂表面防护：如图2～图4所示，夹具2包括挂钩、第一弧形部件和第二弧形部件，第一弧形部件和第二弧形部件组成完整的圆环，挂钩连接在第一弧形部件外侧，第一弧形部件和第二弧形部件的内环面形状与钛合金零件非喷涂表面形状匹配，第一弧形部件和第二弧形部件的一端相互铰接，另一端通过螺钉3可拆卸连接，将零件1放入夹具2中，拧紧螺钉3，对非喷涂表面进行屏蔽处理；(5) Non-sprayed surface protection: As shown in Figures 2 to 4, the fixture 2 includes a hook, a first arc-shaped part and a second arc-shaped part. The first arc-shaped part and the second arc-shaped part form a complete ring , The hook is connected to the outside of the first arc-shaped part, the inner ring surface shape of the first arc-shaped part and the second arc-shaped part matches the shape of the non-sprayed surface of the titanium alloy part, one end of the first arc-shaped part and the second arc-shaped part Hinge each other, the other end can be detachably connected with the screw 3, put the part 1 into the fixture 2, tighten the screw 3, and shield the non-painted surface;
(6)零件表面预处理：零件室温装入真空离子氮化炉后，氮化炉开始抽真空，抽至<1Pa后，关闭真空泵，检验氮化炉漏气率，保证空气漏气率<0.13Pa/min。当漏气率满足要求后，充NH 3数次冲洗真空室。在适量的NH 3流量下，加热零件至600℃，保温30min～60min，保温过程中NH 3流量为1.0L/min～2.0L/min。保温结束后，用纯N 2替换炉内气体，并缓慢降温至550℃，以防止零件在降温过程中大量吸氢，造成氢脆。在适量的N 2气氛下，由550℃缓慢降至100℃以下出炉； (6) Surface pretreatment of parts: After the parts are put into the vacuum ion nitriding furnace at room temperature, the nitriding furnace starts to vacuum, after pumping to <1Pa, turn off the vacuum pump, check the air leakage rate of the nitriding furnace, and ensure that the air leakage rate is <0.13 Pa/min. When the air leakage rate meets the requirements, the vacuum chamber is flushed with NH 3 several times. Under the right amount of NH 3 flow rate, heat the parts to 600°C and keep the temperature for 30min～60min. During the heat preservation process, the NH 3 flow rate is 1.0L/min～2.0L/min. After the heat preservation is over, replace the furnace gas with pure N 2 and slowly lower the temperature to 550°C to prevent the parts from absorbing a large amount of hydrogen during the cooling process, causing hydrogen embrittlement. Under an appropriate amount of N 2 atmosphere, slowly drop from 550°C to below 100°C and release from the furnace;
(6)入炉：将装好夹具2的零件1及试样入沉积炉装吊时，需戴洁净纯棉手套进行操作，严禁裸手触摸或用不干净的夹具夹持；(6) Entering the furnace: When placing parts 1 and samples with fixture 2 into the deposition furnace, wear clean cotton gloves for operation, and it is strictly forbidden to touch with bare hands or clamp with dirty fixtures;
(7)刻蚀工艺为：(7) The etching process is:
辉光放电气体离子轰击：轰击时间为40min～50min，真空室内的压强为2.0Pa～3.0Pa；Glow discharge gas ion bombardment: The bombardment time is 40min-50min, and the pressure in the vacuum chamber is 2.0Pa～3.0Pa;
阴极电弧Ti离子轰击：Ti靶电流60A～80A，轰击时间为15min～20min，轰击时真空室内的压强为0.5～0.6MPa；Cathodic arc Ti ion bombardment: Ti target current is 60A～80A, bombardment time is 15min～20min, and the pressure in the vacuum chamber during bombardment is 0.5～0.6MPa;
(8)沉积TiN涂层,沉积工艺为：(8) TiN coating is deposited, the deposition process is:
Ti靶电流70A～90A，N 2流量为700sccm，沉积时间为180min～250min，真空室内压强1.0～1.2Pa； The Ti target current is 70A～90A, the N 2 flow rate is 700sccm, the deposition time is 180min～250min, and the pressure in the vacuum chamber is 1.0～1.2Pa;
(10)出炉；(10) Released;
(11)涂层质量检查：包括外观、厚度、硬度、结合力等。(11) Coating quality inspection: including appearance, thickness, hardness, adhesion, etc.
本发明针对钛合金轴承座、轴承衬套、安装环等类型零件的零件结构特点，采取了特殊而简易的、适合发动机钛合金零件的物理气相沉积TiN耐磨涂层方式，既保证了零件后期对耐磨性的要求，又保证了零件尺寸，节约了时间、降低了生产成本。The invention adopts a special and simple physical vapor deposition TiN wear-resistant coating method suitable for engine titanium alloy parts according to the structural characteristics of parts of titanium alloy bearing seats, bearing bushes, mounting rings and other types of parts, which not only ensures the later stage of the parts The requirements for wear resistance ensure the size of the parts, save time and reduce production costs.

Claims (10)

  1. 一种航空发动机钛合金零件，其特征在于：所述钛合金零件表面局部覆盖TiN涂层。An aeroengine titanium alloy part, which is characterized in that the surface of the titanium alloy part is partially covered with a TiN coating.
  2. 根据权利要求1所述的一种航空发动机钛合金零件，其特征在于：所述TiN涂层通过离子氮化配合物理气相沉积获得。The aeroengine titanium alloy part according to claim 1, wherein the TiN coating is obtained by ion nitriding combined with physical vapor deposition.
  3. 一种航空发动机钛合金零件TiN涂层制备方法，其特征在于，包括：A preparation method of TiN coating on titanium alloy parts of aeroengine, which is characterized in that it comprises:
    步骤一，喷涂表面预处理和非喷涂表面防护处理；Step 1, spray surface pretreatment and non-spray surface protection treatment;
    步骤二，零件表面预处理，采用离子氮化的方法在钛合金基体表面生成一层富含TiN、Ti 2N的底层； Step two, pretreatment of the surface of the part, using ion nitriding to form a layer of TiN, Ti 2 N-rich underlayer on the surface of the titanium alloy substrate;
    步骤三，刻蚀，包括辉光放电气体离子轰击和阴极电弧Ti离子轰击；Step three, etching, including glow discharge gas ion bombardment and cathodic arc Ti ion bombardment;
    步骤四，沉积TiN层。Step four, deposit TiN layer.
  4. 根据权利要求3所述的一种航空发动机钛合金零件TiN涂层制备方法，其特征在于：所述步骤一中，喷涂表面预处理包括依次进行的喷砂、水洗、表面除油和烘干。The method for preparing TiN coating on titanium alloy parts of aeroengine according to claim 3, characterized in that: in the first step, the sprayed surface pretreatment includes sandblasting, water washing, surface degreasing and drying in sequence.
  5. 根据权利要求4所述的一种航空发动机钛合金零件TiN涂层制备方法，其特征在于：The method for preparing TiN coating on titanium alloy parts of aeroengine according to claim 4, characterized in that:
    所述喷砂为湿喷砂，采用砂粒为500目的Al 2O 3颗粒，喷砂风压为2～5bar； The sandblasting is wet sandblasting, using Al 2 O 3 particles of 500 meshes, and the sandblasting wind pressure is 2 to 5 bar;
    所述表面除油采用超声波清洗；Ultrasonic cleaning is used for the degreasing of the surface;
    所述烘干的烘干温度150℃～180℃，烘干时间1h～2h。The drying temperature of the drying is 150°C-180°C, and the drying time is 1h-2h.
  6. 根据权利要求3所述的一种航空发动机钛合金零件TiN涂层制备方法，其特征在于：所述步骤一中，非喷涂表面防护处理采用夹具屏蔽非喷涂表面。The method for preparing TiN coating on titanium alloy parts of aeroengine according to claim 3, characterized in that: in the step 1, the non-sprayed surface protection treatment adopts a clamp to shield the non-sprayed surface.
  7. 根据权利要求6所述的一种航空发动机钛合金零件TiN涂层制备方法，其特征在于：所述夹具包括挂钩、第一弧形部件和第二弧形部件，且第一弧形部件和第二弧形部件组成完整的圆环，第一弧形部件和第二弧形部件的内环面形状与钛合金零件非喷涂表面形状匹配，第一弧形部件和第二弧形部件的一端相互铰接，另一端通过螺钉可拆卸连接。The method for preparing TiN coating on titanium alloy parts of aeroengine according to claim 6, wherein the clamp includes a hook, a first arc-shaped part and a second arc-shaped part, and the first arc-shaped part and the second arc-shaped part The two arc-shaped parts form a complete ring. The inner ring shape of the first arc-shaped part and the second arc-shaped part matches the shape of the non-sprayed surface of the titanium alloy part. One end of the first arc-shaped part and the second arc-shaped part are mutually Hinge, the other end can be detachably connected by screws.
  8. 根据权利要求3所述的一种航空发动机钛合金零件TiN涂层制备方法，其特征在于：所述步骤二中，零件表面预处理时，加热温度为600℃，保温时间30min～60min，保温过程中NH 3流量为1.0L/min～2.0L/min。 The method for preparing TiN coating on titanium alloy parts of aeroengine according to claim 3, characterized in that: in the second step, when the surface of the part is pretreated, the heating temperature is 600°C, the heat preservation time is 30min-60min, and the heat preservation process The medium NH 3 flow rate is 1.0L/min～2.0L/min.
  9. 根据权利要求3所述的一种航空发动机钛合金零件TiN涂层制备方法，其特征 在于：所述步骤三中，辉光放电气体离子轰击时，轰击时间为40min～50min，真空室内的压强为2.0Pa～3.0Pa；阴极电弧Ti离子轰击时，Ti靶电流60A～80A，轰击时间为15min～20min，轰击时真空室内的压强为0.5～0.6MPa。The method for preparing TiN coating on titanium alloy parts of aeroengine according to claim 3, characterized in that: in the step three, when the glow discharge gas ion bombards, the bombardment time is 40min-50min, and the pressure in the vacuum chamber is 2.0Pa～3.0Pa; when the cathodic arc Ti ion bombards, the Ti target current is 60A～80A, the bombardment time is 15min～20min, and the pressure in the vacuum chamber is 0.5～0.6MPa during the bombardment.
  10. 根据权利要求3所述的一种航空发动机钛合金零件TiN涂层制备方法，其特征在于：所述步骤四中，沉积TiN层时，Ti靶电流70A～90A，N 2流量为700sccm，沉积时间为180min～250min，真空室内压强1.0～1.2Pa。 The method for preparing TiN coating on titanium alloy parts of aeroengine according to claim 3, characterized in that: in the step four, when depositing the TiN layer, the Ti target current is 70A～90A, the N 2 flow rate is 700 sccm, and the deposition time It is 180min～250min, and the pressure in the vacuum chamber is 1.0～1.2Pa.
PCT/CN2019/124208 2019-12-10 2019-12-10 Preparation method for tin coating on titanium alloy part of aircraft engine WO2021114068A1 (en)

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