CN113564517A - Device and method for in-situ deposition of PVD (physical vapor deposition) coating after low-temperature rapid toughness nitriding - Google Patents
Device and method for in-situ deposition of PVD (physical vapor deposition) coating after low-temperature rapid toughness nitriding Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
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Abstract
The invention discloses a device and a method for in-situ deposition of a PVD (physical vapor deposition) coating after low-temperature rapid toughness nitriding, and relates to a device and a method for in-situ deposition of a PVD coating after low-temperature rapid toughness nitriding. The invention aims to solve the existing problems, firstly, the arc enhanced glow discharge technology is utilized to carry out grinding, polishing and cleaning on the surface of a high-speed steel substrateAr+、H+Etching and cleaning the plasma; then high-purity nitrogen, high-purity hydrogen or high-purity nitrogen, high-purity hydrogen and inert gas argon are continuously introduced into the vacuum chamber to carry out plasma nitriding treatment; and finally, depositing the PVD coating in situ by using an electric field enhanced cathode arc technology at a similar temperature. According to the invention, the auxiliary anode is added on the traditional equipment, and the L-shaped baffle is added in front of the cathode arc source on one side, so that the in-situ deposition of the PVD coating after low-temperature rapid and tough nitriding is realized. The method is applied to the field of in-situ deposition of PVD coatings.
Description
Technical Field
The invention relates to a device and a method for in-situ deposition of a PVD coating after low-temperature rapid toughness nitriding.
Background
In industrial practice, nitriding and coating processes are often used to improve the surface properties of the cutting tools, thereby prolonging the service life of the cutting tools. The ion nitriding process is simple, the nitriding time is short, a penetrated layer is deep, but the surface microhardness is low; the coating process can improve the surface hardness to a rather high level, but the coating thickness is relatively thin and cannot completely meet the requirements of industrial production. For a high-speed cutting tool, although high-speed steel has good toughness and formability during cutting processing, the cutting speed of the high-speed steel can only reach 20-25 m/min, and when the cutting speed reaches 70-100 m/min, the coating tool generates plastic deformation and softening of a matrix due to heat effect, so that the coating cracks, and the cutting efficiency is not high enough.
As early as 1983, Finnish scientist Korhonen et al proposed a new technology (PN/PVD for short) of Plasma Nitriding (PN)/Physical Vapor Deposition (PVD) composite treatment, which combines the advantages of Plasma Nitriding and Vapor Deposition, and simultaneously weakens the problems of the difference of hardness and plastic deformation between a coating and a substrate, the mismatch of thermal expansion coefficient and elastic modulus, and the like. Due to the easy realizability and excellent performance of the composite coating process, a large number of scholars at home and abroad are attracted to research the composite coating process, and the composite coating process is expected to be applied to the industry and gradually realize commercialization. The plasma nitriding-physical vapor deposition (PN-PVD) composite treatment technology is applied to the material industry, and the research on how to improve the composite coating film/base bonding force has important theoretical and practical application values. However, factors that limit the performance and application of composite coatings are also manifold. The coating equipment has the problems of coating equipment, the surface interface of the coating, the selection of the coating material, the design and preparation of a composite structure and the like.
The composite treatment can significantly improve the bond strength of the coating to the substrate because most studies have added transition treatments such as grinding, polishing, etc. that eliminate most of the compound layer on the nitrided substrate. Among the parameters controlling the nitrogen diffusion, the temperature is undoubtedly the most important parameter. The temperature is too high in the nitriding process, so that a steel matrix is softened; and low temperatures reduce the nitridation efficiency. Therefore, how to rapidly nitridize at low temperature is a main problem to be solved. On the other hand, the surface of the steel matrix can generate certain brittleness after nitriding, so that the realization of the toughness nitriding of the surface of the steel matrix is also a problem to be solved in the nitriding process.
Disclosure of Invention
The invention aims to provide a device and a deposition method for in-situ deposition of a PVD coating after low-temperature rapid toughness nitriding, aiming at the problems of low nitriding efficiency at low temperature or increased brittleness of the surface of a steel matrix after nitriding treatment in the in-situ deposition PVD coating technology after nitriding. The nitriding layer which does not contain a compound layer and has high toughness is quickly prepared under the low-temperature condition, and the thickness of the nitriding layer can reach more than 50 mu m.
The invention relates to a device for in-situ deposition of a PVD (physical vapor deposition) coating after low-temperature rapid tough nitriding, which comprises a vacuum chamber, a rotating frame, a workpiece tray, a matrix bias power supply, a first metal cathode arc group, a second metal cathode arc group, an L-shaped baffle, a first auxiliary anode, a second auxiliary anode, a first metal cathode arc direct-current power supply, a second metal cathode arc direct-current power supply, a first auxiliary anode direct-current power supply and a second auxiliary anode direct-current power supply, wherein the vacuum chamber is used for accommodating a workpiece; the rotating frame is positioned at the center of the bottom of the vacuum chamber, the rotating frame is rotationally connected with the vacuum chamber, a first metal cathode arc group, a second metal cathode arc group, a first auxiliary anode and a second auxiliary anode are arranged in the vacuum chamber along the circumferential direction, the first metal cathode arc group and the second auxiliary anode are oppositely arranged, and the second metal cathode arc group and the first auxiliary anode are oppositely arranged; an L-shaped baffle is arranged between the second metal cathode arc group and the rotating frame, the anode of the first auxiliary anode direct-current power supply is connected with the first auxiliary anode, the cathode of the first auxiliary anode direct-current power supply is grounded, and the anode of the second auxiliary anode direct-current power supply is connected with the second auxiliary anode, and the cathode of the second auxiliary anode direct-current power supply is grounded; a first metal cathode arc direct-current power supply is connected between the first metal cathode arc group and the vacuum chamber, and a second metal cathode arc direct-current power supply is connected between the second metal cathode arc group and the vacuum chamber; a bias power supply is connected between the rotating frame and the vacuum chamber.
The method for carrying out in-situ deposition of the PVD coating after low-temperature rapid toughness nitriding by using the device comprises the following steps:
firstly, pretreatment of a substrate surface: grinding and polishing the surface of a substrate, then placing the substrate in absolute ethyl alcohol for ultrasonic cleaning, clamping the substrate on a workpiece tray in a vacuum chamber after drying, vacuumizing the vacuum chamber, and preheating;
secondly, plasma etching and cleaning the surface of the substrate: introducing argon and hydrogen into the vacuum chamber, and starting a second metal cathode arc direct-current power supply, a first auxiliary anode direct-current power supply and a second auxiliary anode direct-current power supply; controlling the pulse bias voltage of the substrate bias power supply to be-500V, the duty ratio to be 50% and the frequency to be 40KHz, cleaning for 10min, adjusting the pulse bias voltage of the substrate bias power supply to be-200V, the duty ratio to be 80% and the frequency to be 40KHz, and cleaning for 20 min; the current of the direct current end of the second metal cathode arc direct current power supply is kept to be 85A in the substrate surface plasma etching cleaning process, and the current of the direct current ends of the first auxiliary anode direct current power supply and the second auxiliary anode direct current power supply is kept to be 100A;
thirdly, arc plasma assisted nitriding: introducing gas into a vacuum chamber, and performing 120min ion enhanced nitriding treatment under the conditions of the temperature of 450 ℃, the air pressure of 0.45Pa, the current of the direct current end of the second metal cathode arc direct current power supply of 85A, the current of the direct current end of the first auxiliary anode direct current power supply of 100A, the current of the direct current end of the second auxiliary anode direct current power supply of 100A and the bias voltage of matrix bias electric pulse of-200V, the duty ratio of 80% and the frequency of 40KHz in the vacuum chamber;
fourthly, in-situ deposition of the PVD coating: regulating the nitrogen flow to 800sccm, controlling the vacuum chamber gas pressure to 1Pa, regulating the matrix bias power supply pulse bias voltage to-125V, regulating the duty ratio to 80 percent and regulating the frequency to 40 KHz; the current 100A of the direct current end of the second auxiliary anode direct current power supply keeps constant; starting a first metal cathode arc direct current power supply, wherein the current is 85A; closing the second metal cathode arc direct-current power supply and the first auxiliary anode direct-current power supply; and depositing the TiN coating for 120min at the temperature of 450 +/-5 ℃, thus finishing.
The invention has the following beneficial effects:
(1) according to the invention, the auxiliary anode is arranged in the vacuum chamber, the L-shaped suspension baffle is arranged in front of the metal cathode arc, the discharge passage is constructed between the cathode arc and the auxiliary anode, electrons emitted by the cathode arc are pulled out from one side of the opening of the L-shaped suspension baffle by the auxiliary anode, the movement path of the electrons is prolonged, the collision ionization with gas is increased, the plasma density in the vacuum chamber is improved, the nitriding rate is improved by high-density plasma in the ion nitriding process, and the toughness nitriding is realized by adjusting the nitriding gas proportion.
(2) The invention adopts the arc enhanced glow discharge technology for nitriding, and the high-density plasma can obtain lower nitriding temperature and effectively improve the nitriding rate in the nitriding process. Activating the surface by argon ion bombardment, on one hand, increasing the lattice defects on the surface layer of the workpiece, and increasing nitrogen atom diffusion channels; on the other hand, the formation of a compound layer is avoided, the diffusion barrier of nitrogen atoms is reduced, the diffusion of the nitrogen atoms is facilitated, and the rapid permeation effect is achieved.
(3) In the nitriding process, N2The content is an important parameter influencing nitriding, and because the nitrogen dissolving rate of high-speed steel is very low, the nitrogen content and the gas proportion need to be strictly controlled in the nitriding process. H+Has high reducibility, and can reduce an oxide layer on the surface of a sample. Ar (Ar)+Bombard and activate the surface of the workpiece, can increase the nitrogen atom diffusion channel and accelerate the nitriding process. The invention is in N2、H2Flow ratio of 1:9 (N)2The proportion is 10%), the surface toughness nitridation of the high-speed steel can be realized; by adding inert gas Ar, the nitrogen content can be increased2The proportion is 26 percent) to realize the surface toughness nitridation of the high-speed steel.
(4) The PVD coating is deposited in situ after plasma nitriding in the same vacuum chamber, so that the surface treatment efficiency of the workpiece can be greatly improved.
Drawings
FIG. 1 is a schematic view of an apparatus of the present invention;
FIG. 2 is a cross-sectional metallographic photograph of a nitrided layer/TiN composite coating prepared in example 1;
FIG. 3 shows example 1N2:H2The shape of the Rockwell indentation on the surface of the nitrided layer after nitriding treatment when the flow ratio is 30: 270;
FIG. 4 is a graph showing the results of Rockwell indentation of the nitrided layer/TiN composite coating prepared in example 1;
FIG. 5 shows example 2N2:H2The shape of the Rockwell indentation on the surface of the nitrided layer after nitriding treatment when the flow ratio is 50: 250;
FIG. 6 is a graph showing the results of Rockwell indentation of the nitrided layer/TiN composite coating prepared in example 2;
FIG. 7 is a cross-sectional metallographic photograph of a nitrided layer/TiN composite coating prepared in example 3;
FIG. 8 shows example 3N2:Ar:H2The shape of the Rockwell indentation on the surface of the nitriding layer after nitriding treatment is 80:20: 200;
fig. 9 is a graph showing rockwell indentation results of the nitrided layer/TiN composite coating prepared in example 3.
Detailed Description
The first embodiment is as follows: the device for in-situ deposition of the PVD coating after low-temperature rapid tough nitriding comprises a vacuum chamber 5, a rotating frame 4, a workpiece tray 6, a substrate bias power supply 7, a first metal cathode arc group 2-1, a second metal cathode arc group 2-2, an L-shaped baffle 1, a first auxiliary anode 3-1, a second auxiliary anode 3-2, a first metal cathode arc direct current power supply 8-1, a second metal cathode arc direct current power supply 8-2, a first auxiliary anode direct current power supply 9-1 and a second auxiliary anode direct current power supply 9-2; the rotating frame 4 is positioned at the center of the bottom of the vacuum chamber 5, the rotating frame 4 is rotatably connected with the vacuum chamber 5, a first metal cathode arc group 2-1, a second metal cathode arc group 2-2, a first auxiliary anode 3-1 and a second auxiliary anode 3-2 are arranged in the vacuum chamber 5 along the circumferential direction, the first metal cathode arc group 2-1 and the second auxiliary anode 3-2 are oppositely arranged, and the second metal cathode arc group 2-2 and the first auxiliary anode 3-1 are oppositely arranged; an L-shaped baffle plate 1 is arranged between the second metal cathode arc group 2-2 and the rotating frame 4, the anode of a first auxiliary anode direct current power supply 9-1 is connected with a first auxiliary anode 3-1, the cathode is grounded, the anode of a second auxiliary anode direct current power supply 9-2 is connected with a second auxiliary anode 3-2, and the cathode is grounded; a first metal cathode arc direct current power supply 8-1 is connected between the first metal cathode arc group 2-1 and the vacuum chamber 5, and a second metal cathode arc direct current power supply 8-2 is connected between the second metal cathode arc group 2-2 and the vacuum chamber 5; a bias power supply 7 is connected between the rotary frame 4 and the vacuum chamber 5.
The second embodiment is as follows: the difference between the present embodiment and the first embodiment is that the rotating frame 4, the first metal cathode arc group 2-1, the second metal cathode arc group 2-2, the first auxiliary anode 3-1, the second auxiliary anode 3-2, and the L-shaped baffle 1 are all insulated from the vacuum chamber 5. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the first metal cathode arc group 2-1, the second metal cathode arc group 2-2, the first auxiliary anode 3-1 and the second auxiliary anode 3-2 are fixedly connected with the vacuum chamber 5 through flanges. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the first metal cathode arc group 2-1 and the second metal cathode arc group 2-2 are respectively composed of three metal cathode arcs which are vertically arranged. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the electric connection end of the first metal cathode arc group 2-1 is electrically connected with the negative electrode of the first metal cathode arc direct current power supply 8-1, the electric connection end of the second metal cathode arc group 2-2 is electrically connected with the negative electrode of the second metal cathode arc direct current power supply 8-2, and the negative electrode of the bias power supply 7 is electrically connected with the electric connection end of the rotating frame 4; the electric connection end of the vacuum chamber 5 is respectively and electrically connected with the anode of the first metal cathode arc direct current power supply 8-1, the anode of the second metal cathode arc direct current power supply 8-2 and the anode of the bias power supply 7, and the vacuum chamber 5 is grounded. The rest is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the method for in-situ deposition of the PVD coating after low-temperature rapid toughness nitriding comprises the following steps:
firstly, pretreatment of a substrate surface: grinding and polishing the surface of the substrate, then placing the substrate in absolute ethyl alcohol for ultrasonic cleaning, drying the substrate by blowing, clamping the substrate on a workpiece tray 6 of a rotating frame 4 in a vacuum chamber 5, vacuumizing the vacuum chamber 5, and preheating the substrate;
secondly, plasma etching and cleaning the surface of the substrate: introducing argon and hydrogen into the vacuum chamber 5, and starting a second metal cathode arc direct current power supply 8-2, a first auxiliary anode direct current power supply 9-1 and a second auxiliary anode direct current power supply 9-2; controlling the pulse bias voltage of the substrate bias power supply 7 to be-500V, the duty ratio is 50%, the frequency is 40KHz, after cleaning for 10min, adjusting the pulse bias voltage of the substrate bias power supply 7 to be-200V, the duty ratio is 80%, the frequency is 40KHz, and cleaning for 20 min; the current of the direct current end of the second metal cathode arc direct current power supply 8-2 is kept to be 85A in the substrate surface plasma etching cleaning process, and the current of the direct current ends of the first auxiliary anode direct current power supply 9-1 and the second auxiliary anode direct current power supply 9-2 is kept to be 100A;
thirdly, arc plasma assisted nitriding: introducing gas into a vacuum chamber 5, and performing 120min ion enhanced nitriding treatment under the conditions that the temperature in the vacuum chamber 5 is 450 ℃, the air pressure is 0.45Pa, the current of a direct current end 8-2 of a second metal cathode arc direct current power supply is 85A, the current of a direct current end 9-1 of a first auxiliary anode direct current power supply is 100A, the current of a direct current end 9-2 of a second auxiliary anode direct current power supply is 100A, the pulse bias voltage of a matrix bias voltage power supply is 7-200V, the duty ratio is 80%, and the frequency is 40 KHz;
fourthly, in-situ deposition of the PVD coating: regulating the nitrogen flow to 800sccm, controlling the vacuum chamber gas pressure to 1Pa, regulating the substrate bias power supply 7 to-125V under the pulse bias, regulating the duty ratio to 80 percent and regulating the frequency to 40 KHz; the current 100A of the direct current end of the second auxiliary anode direct current power supply 9-2 keeps constant; starting a first metal cathode arc direct current power supply 8-1, wherein the current is 85A; closing a second metal cathode arc direct current power supply 8-2 and a first auxiliary anode direct current power supply 9-1; and depositing the TiN coating for 120min at the temperature of 450 +/-5 ℃, thus finishing.
The seventh embodiment: the sixth embodiment is different from the sixth embodiment in that: in the first step, the vacuum is pumped to 3 multiplied by 10-3Pa, the vacuum chamber 5 is preheated to 450 ℃. The rest is the same as the sixth embodiment.
The specific implementation mode is eight: the sixth or seventh embodiment is different from the sixth or seventh embodiment in that: and in the second step, the flow ratio of the argon to the hydrogen is 200: 20. The rest is the same as the sixth or seventh embodiment.
The specific implementation method nine: this embodiment differs from one of the sixth to eighth embodiments in that: the first metal cathode arc group 2-1 and the second metal cathode arc group 2-2 are Ti targets, and the purity reaches 99.5%. The rest is the same as in one of the sixth to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the sixth to ninth embodiments in that: the gas in the third step is high-purity N with the flow ratio of 30:2702And high purity H2Or 80:20:200 of high-purity N2Inert gas Ar and high-purity H2The mixed gas of (1). The others are the same as in one of the sixth to ninth embodiments.
The following experiments were performed to verify the beneficial effects of the present invention:
example 1
The device for in-situ deposition of PVD coating after low-temperature rapid tough nitriding in the embodiment is shown in figure 1 and comprises a vacuum chamber 5, a rotating frame 4, a workpiece tray 6, a substrate bias power supply 7, a first metal cathode arc group 2-1, a second metal cathode arc group 2-2, an L-shaped baffle 1, a first auxiliary anode 3-1, a second auxiliary anode 3-2, a first metal cathode arc direct current power supply 8-1, a second metal cathode arc direct current power supply 8-2, a first auxiliary anode direct current power supply 9-1 and a second auxiliary anode direct current power supply 9-2; the rotating frame 4 is positioned at the center of the bottom of the vacuum chamber 5, the rotating frame 4 is rotatably connected with the vacuum chamber 5, a first metal cathode arc group 2-1, a second metal cathode arc group 2-2, a first auxiliary anode 3-1 and a second auxiliary anode 3-2 are arranged in the vacuum chamber 5 along the circumferential direction, the first metal cathode arc group 2-1 and the second auxiliary anode 3-2 are oppositely arranged, and the second metal cathode arc group 2-2 and the first auxiliary anode 3-1 are oppositely arranged; an L-shaped baffle plate 1 is arranged between the second metal cathode arc group 2-2 and the rotating frame 4, the anode of a first auxiliary anode direct current power supply 9-1 is connected with a first auxiliary anode 3-1, the cathode is grounded, the anode of a second auxiliary anode direct current power supply 9-2 is connected with a second auxiliary anode 3-2, and the cathode is grounded; a first metal cathode arc direct current power supply 8-1 is connected between the first metal cathode arc group 2-1 and the vacuum chamber 5, and a second metal cathode arc direct current power supply 8-2 is connected between the second metal cathode arc group 2-2 and the vacuum chamber 5; a bias power supply 7 is connected between the rotary frame 4 and the vacuum chamber 5. The rotating frame 4, the first metal cathode arc group 2-1, the second metal cathode arc group 2-2, the L-shaped baffle 1, the first auxiliary anode 3-1 and the second auxiliary anode 3-2 are all insulated from the vacuum chamber 5 through polytetrafluoroethylene.
The method for carrying out in-situ deposition of the PVD coating after low-temperature rapid toughness nitriding by using the device comprises the following steps:
(1) preparing a matrix: prepare the specification as
M2 high-speed steel basal body, and grinding with 180#, 320#, 600#, 800#, 1000#, 1200# metallographic abrasive paper in sequence; then polishing the glass to a mirror surface by utilizing a diamond spray polishing agent; after polishing, placing the sample in absolute ethyl alcohol for ultrasonic cleaning, and drying by hot air; then placing the workpiece tray 6 on a rotating frame 4 in a vacuum chamber 5, vacuumizing the vacuum chamber 5, and preheating;
(2) and (3) etching and cleaning the surface of the substrate by plasma: performing plasma (Ar) on the surface of the substrate by adopting an arc enhanced glow discharge technology+、H+) And (5) etching and cleaning. Introducing 200sccm argon gas and 20sccm hydrogen gas into the cavity of the vacuum chamber; starting a second metal cathode arc direct current power supply 8-2, a first auxiliary anode direct current power supply 9-1 and a second auxiliary anode direct current power supply 9-2; the metal cathode arc Ti target is used as an electron source, and the current of the direct current end is 85A; the current of the auxiliary anode direct current power supply is 100A; the temperature of the heating pipe is set to 450 ℃; controlling the pulse bias voltage of a substrate bias power supply to be-500V, the duty ratio to be 50 percent and the frequency to be 40KHz, cleaning for 10min, adjusting the pulse bias voltage of a substrate bias power supply 7 to be-200V, the duty ratio to be 80 percent and the frequency to be 40KHz, and cleaning for 20 min;
(3) nitriding the surface of the matrix: after the plasma etching cleaning of the substrate surface, high-purity N with the flow ratio of 30:270 is introduced into the vacuum chamber 52High purity H2Keeping the temperature and the air pressure in the vacuum chamber constant, the current 85A at the direct current end of the second metal cathode arc direct current power supply 8-2 and the current at the direct current end of the first auxiliary anode direct current power supply 9-1100A, keeping constant current 100A at the direct current end of a second auxiliary anode direct current power supply 9-2 and pulse bias voltage-200V, duty ratio 80% and frequency 40KHz of a matrix bias power supply, and performing ion enhanced nitriding treatment for 120 min;
(4) deposition of TiN coating: and after the surface of the matrix is subjected to plasma nitriding, depositing a TiN coating in situ. Regulating the nitrogen flow to 800sccm, controlling the gas pressure to be 1Pa, regulating the pulse bias voltage of the substrate bias power supply to-125V, regulating the duty ratio to be 80 percent and regulating the frequency to be 40 KHz; the current 100A of the direct current end of the second auxiliary anode direct current power supply 9-2 keeps constant; starting a first metal cathode arc direct current power supply 8-1, wherein the current is 85A; closing a second metal cathode arc direct current power supply 8-2 and a first auxiliary anode direct current power supply 9-1; depositing TiN coating for 120min at the temperature similar to the ion nitriding process.
(5) And (3) cooling: and cooling the cavity by using a furnace body cooling water circulation system, and cooling the workpiece to be below 100 ℃ along with the cavity in a vacuum state.
And (3) after the matrix is taken out, carrying out analysis characterization and performance test:
(1) microstructure observation is carried out on the section of the infiltrated layer/TiN coating by adopting an optical metallographic microscope (OLYMPUS manufactured by model SZX 12), and figure 2 shows the section structure morphology of the deposited TiN coating after nitriding of the M2 high-speed steel matrix. TiN coating thickness about 1.2 μm under metallographic microscope (700X); the thickness of the nitriding layer reaches 40 mu m, and the nitriding layer does not have a compound layer and a network grain boundary structure.
(2) And testing the crack condition of the nitriding layer by adopting a Rockwell (HRC) indentation method, and evaluating the toughness of the nitriding layer according to the crack condition, wherein the load is 1470N. FIG. 3 is N2:H2And when the flow ratio is 30:270, the appearance of the Rockwell indentations on the surface of the nitriding layer after nitriding treatment is realized. No obvious cracks are formed around the indentation, and the indentation test shows that the surface of the nitriding layer has excellent toughness.
(3) The film-based bond strength was evaluated by rockwell indentation according to the coating bond standard (VDI standard 3198) using a standard conical diamond indenter with a load of 1470N and a dwell time of 10 s. Fig. 4 is an indentation morphology of a percolated layer/TiN coating prepared on an M2 high speed steel substrate, and it can be seen that the film-substrate bonding strength is good, the coating does not peel off, only a few bending cracks exist around the indentation, and the indentation grade is HF 1.
Example 2
The device for in-situ deposition of the PVD coating after low-temperature rapid tough nitriding comprises a vacuum chamber 5, a rotating frame 4, a workpiece tray 6, a matrix bias power supply 7, a first metal cathode arc group 2-1, a second metal cathode arc group 2-2, an L-shaped baffle 1, a first auxiliary anode 3-1, a second auxiliary anode 3-2, a first metal cathode arc direct current power supply 8-1, a second metal cathode arc direct current power supply 8-2, a first auxiliary anode direct current power supply 9-1 and a second auxiliary anode direct current power supply 9-2; the rotating frame 4 is positioned at the center of the bottom of the vacuum chamber 5, the rotating frame 4 is rotatably connected with the vacuum chamber 5, a first metal cathode arc group 2-1, a second metal cathode arc group 2-2, a first auxiliary anode 3-1 and a second auxiliary anode 3-2 are arranged in the vacuum chamber 5 along the circumferential direction, the first metal cathode arc group 2-1 and the second auxiliary anode 3-2 are oppositely arranged, and the second metal cathode arc group 2-2 and the first auxiliary anode 3-1 are oppositely arranged; an L-shaped baffle plate 1 is arranged between the second metal cathode arc group 2-2 and the rotating frame 4, the anode of a first auxiliary anode direct current power supply 9-1 is connected with a first auxiliary anode 3-1, the cathode is grounded, the anode of a second auxiliary anode direct current power supply 9-2 is connected with a second auxiliary anode 3-2, and the cathode is grounded; a first metal cathode arc direct current power supply 8-1 is connected between the first metal cathode arc group 2-1 and the vacuum chamber 5, and a second metal cathode arc direct current power supply 8-2 is connected between the second metal cathode arc group 2-2 and the vacuum chamber 5; a bias power supply 7 is connected between the rotary frame 4 and the vacuum chamber 5. The rotating frame 4, the first metal cathode arc group 2-1, the second metal cathode arc group 2-2, the L-shaped baffle 1, the first auxiliary anode 3-1 and the second auxiliary anode 3-2 are all insulated from the vacuum chamber 5 through polytetrafluoroethylene.
The method for carrying out in-situ deposition of the PVD coating after low-temperature rapid toughness nitriding by using the device comprises the following steps:
(1) preparing a matrix: prepare the specification as
M2 high-speed steel basal body, and grinding with 180#, 320#, 600#, 800#, 1000#, 1200# metallographic abrasive paper in sequence; then polishing the glass to a mirror surface by utilizing a diamond spray polishing agent; after polishing, the sample was left withoutUltrasonically cleaning in water ethanol, and drying by hot air; then placing the workpiece tray 6 on a rotating frame 4 in a vacuum chamber 5, vacuumizing the vacuum chamber 5, and preheating;
(2) and (3) etching and cleaning the surface of the substrate by plasma: performing plasma (Ar) on the surface of the substrate by adopting an arc enhanced glow discharge technology+、H+) And (5) etching and cleaning. Introducing 200sccm argon gas and 20sccm hydrogen gas into the cavity of the vacuum chamber 5; starting a second metal cathode arc direct current power supply 8-2, a first auxiliary anode direct current power supply 9-1 and a second auxiliary anode direct current power supply 9-2; the metal cathode arc Ti target is used as an electron source, and the current of the direct current end is 85A; the current of the auxiliary anode direct current power supply is 100A; the temperature of the heating pipe is set to 450 ℃; controlling the pulse bias voltage of a substrate bias power supply to be-500V, the duty ratio to be 50 percent and the frequency to be 40KHz, cleaning for 10min, adjusting the pulse bias voltage of a substrate bias power supply 7 to be-200V, the duty ratio to be 80 percent and the frequency to be 40KHz, and cleaning for 20 min;
(3) nitriding the surface of the matrix: after the plasma etching cleaning of the substrate surface, high-purity N with the flow ratio of 50:250 is introduced into the vacuum chamber 52High purity H2Keeping the temperature and air pressure in the vacuum chamber 5 constant, keeping the current 85A at the direct current end of a second metal cathode arc direct current power supply 8-2, the current 100A at the direct current end of a first auxiliary anode direct current power supply 9-1, the current 100A at the direct current end of a second auxiliary anode direct current power supply 9-2 and the pulse bias voltage-200V of a matrix bias power supply, keeping the duty ratio of 80 percent and the frequency of 40KHz constant, and performing 120min ion enhanced nitriding treatment;
(4) deposition of TiN coating: and after the surface of the matrix is subjected to plasma nitriding, depositing a TiN coating in situ. Regulating the nitrogen flow to 800sccm, controlling the gas pressure to be 1Pa, regulating the pulse bias voltage of the substrate bias power supply to-125V, regulating the duty ratio to be 80 percent and regulating the frequency to be 40 KHz; the current 100A at the direct-current end of the second auxiliary anode direct-current power supply 9-1 is kept constant; starting a first metal cathode arc direct current power supply 8-1, wherein the current is 85A; closing a second metal cathode arc direct current power supply 8-2 and a first auxiliary anode direct current power supply 9-1; depositing TiN coating for 120min at the temperature similar to the ion nitriding process.
(5) And (3) cooling: and cooling the cavity by using a furnace body cooling water circulation system, and cooling the workpiece to be below 100 ℃ along with the cavity in a vacuum state.
And (3) after the matrix is taken out, carrying out analysis characterization and performance test:
(1) and testing the crack condition of the nitriding layer by adopting a Rockwell (HRC) indentation method, and evaluating the toughness of the nitriding layer according to the crack condition, wherein the load is 1470N. FIG. 5 is N2:H2And the Rockwell indentation appearance of the surface of the nitriding layer after nitriding treatment when the flow ratio is 50: 250. Radial cracks exist around the indentation, and the indentation test shows that the surface toughness of the nitriding layer is poor.
(2) The film-based bond strength was evaluated by rockwell indentation according to the coating bond standard (VDI standard 3198) using a standard conical diamond indenter with a load of 1470N and a dwell time of 10 s. Fig. 6 is an indentation morphology of a percolated layer/TiN coating prepared on an M2 high speed steel substrate, and it can be seen that the film-substrate bonding strength is good, the coating does not peel off, radial cracks exist around the indentation, and the indentation grade is HF 2.
Embodiment 3 the device for in-situ deposition of PVD coating after low temperature fast ductile nitriding of this embodiment comprises a vacuum chamber 5, a turret 4, a workpiece tray 6, a substrate bias power supply 7, a first metal cathode arc group 2-1, a second metal cathode arc group 2-2, an L-shaped baffle 1, a first auxiliary anode 3-1, a second auxiliary anode 3-2, a first metal cathode arc dc power supply 8-1, a second metal cathode arc dc power supply 8-2, a first auxiliary anode dc power supply 9-1 and a second auxiliary anode dc power supply 9-2; the rotating frame 4 is positioned at the center of the bottom of the vacuum chamber 5, the rotating frame 4 is rotatably connected with the vacuum chamber 5, a first metal cathode arc group 2-1, a second metal cathode arc group 2-2, a first auxiliary anode 3-1 and a second auxiliary anode 3-2 are arranged in the vacuum chamber 5 along the circumferential direction, the first metal cathode arc group 2-1 and the second auxiliary anode 3-2 are oppositely arranged, and the second metal cathode arc group 2-2 and the first auxiliary anode 3-1 are oppositely arranged; an L-shaped baffle plate 1 is arranged between the second metal cathode arc group 2-2 and the rotating frame 4, the anode of a first auxiliary anode direct current power supply 9-1 is connected with a first auxiliary anode 3-1, the cathode is grounded, the anode of a second auxiliary anode direct current power supply 9-2 is connected with a second auxiliary anode 3-2, and the cathode is grounded; a first metal cathode arc direct current power supply 8-1 is connected between the first metal cathode arc group 2-1 and the vacuum chamber 5, and a second metal cathode arc direct current power supply 8-2 is connected between the second metal cathode arc group 2-2 and the vacuum chamber 5; a bias power supply 7 is connected between the rotary frame 4 and the vacuum chamber 5. The rotating frame 4, the first metal cathode arc group 2-1, the second metal cathode arc group 2-2, the L-shaped baffle 1, the first auxiliary anode 3-1 and the second auxiliary anode 3-2 are all insulated from the vacuum chamber 5 through polytetrafluoroethylene.
The method for carrying out in-situ deposition of the PVD coating after low-temperature rapid toughness nitriding by using the device comprises the following steps:
(1) preparing a matrix: prepare the specification as
M2 high-speed steel basal body, and grinding with 180#, 320#, 600#, 800#, 1000#, 1200# metallographic abrasive paper in sequence; then polishing the glass to a mirror surface by utilizing a diamond spray polishing agent; after polishing, placing the sample in absolute ethyl alcohol for ultrasonic cleaning, and drying by hot air; then placing the workpiece tray 6 on a rotating frame 4 in a vacuum chamber 5, vacuumizing the vacuum chamber 5, and preheating;
(2) and (3) etching and cleaning the surface of the substrate by plasma: performing plasma (Ar) on the surface of the substrate by adopting an arc enhanced glow discharge technology+、H+) And (5) etching and cleaning. Introducing 200sccm argon gas and 20sccm hydrogen gas into the cavity of the vacuum chamber 5; starting a second metal cathode arc direct current power supply 8-2, a first auxiliary anode direct current power supply 9-1 and a second auxiliary anode direct current power supply 9-2; the metal cathode arc Ti target is used as an electron source, and the current of the direct current end is 85A; the current of the auxiliary anode direct current power supply is 100A; the temperature of the heating pipe is set to 450 ℃; controlling the pulse bias voltage of a substrate bias power supply to be-500V, the duty ratio to be 50 percent and the frequency to be 40KHz, cleaning for 10min, adjusting the pulse bias voltage of a substrate bias power supply 7 to be-200V, the duty ratio to be 80 percent and the frequency to be 40KHz, and cleaning for 20 min;
(3) nitriding the surface of the matrix: after the plasma etching cleaning of the substrate surface, high-purity N with the flow ratio of 80:20:200 is introduced into the vacuum chamber 52Inert gas Ar, high purity H2Keeping the temperature and the air pressure in the vacuum chamber 5 constant, keeping the current 85A at the direct current end of the second metal cathode arc direct current power supply 8-2, the current 100A at the direct current end of the first auxiliary anode direct current power supply 9-1, the current 100A at the direct current end of the second auxiliary anode direct current power supply 9-2 and the substrate bias constantA voltage power supply 7 keeps constant pulse bias of-200V, duty ratio of 80 percent and frequency of 40KHz, and ion enhanced nitriding treatment is carried out for 120 min;
(4) deposition of TiN coating: and after the surface of the matrix is subjected to plasma nitriding, depositing a TiN coating in situ. Regulating the nitrogen flow to 800sccm, controlling the gas pressure to be 1Pa, regulating the pulse bias voltage of the matrix bias power supply 7 to-125V, regulating the duty ratio to be 80 percent and regulating the frequency to be 40 KHz; the current 100A of the direct current end of the second auxiliary anode direct current power supply 9-2 keeps constant; starting a first metal cathode arc direct current power supply 8-1, wherein the current is 85A; closing a second metal cathode arc direct current power supply 8-1 and a first auxiliary anode direct current power supply 9-1; depositing TiN coating for 120min at the temperature similar to the ion nitriding process.
(5) And (3) cooling: and cooling the cavity by using a furnace body cooling water circulation system, and cooling the workpiece to be below 100 ℃ along with the cavity in a vacuum state.
And (3) after the matrix is taken out, carrying out analysis characterization and performance test:
(1) microstructure observation of the infiltrated layer/TiN coating cross section is carried out by adopting an optical metallographic microscope (OLYMPUS manufactured by model SZX12 manufacturer), and figure 7 is the cross section structure morphology of the deposited TiN coating after nitriding of the M2 high-speed steel matrix. TiN coating thickness about 1.2 μm under metallographic microscope (1000 ×); the thickness of the nitriding layer reaches 55 mu m, and the nitriding layer does not have a compound layer and a network grain boundary structure.
(2) And testing the crack condition of the nitriding layer by adopting a Rockwell (HRC) indentation method, and evaluating the toughness of the nitriding layer according to the crack condition, wherein the load is 1470N. FIG. 8 is N2:Ar:H2And the shape of the Rockwell indentation on the surface of the nitriding layer after nitriding treatment when the flow ratio is 80:20: 200. No obvious cracks are formed around the indentation, and the indentation test shows that the surface of the nitriding layer has excellent toughness.
(3) The film-based bond strength was evaluated by rockwell indentation according to the coating bond standard (VDI standard 3198) using a standard conical diamond indenter with a load of 1470N and a dwell time of 10 s. Fig. 9 is an indentation morphology of a percolated layer/TiN coating produced on a M2 high speed steel substrate, and it can be seen that the film-based bond strength is good, the coating does not peel off, there is only bending crack around the indentation, and the indentation rating is HF 1.
As is clear from the examples and comparative examples, the change of nitriding atmosphere can adjust the nitrogen potential, the increase of hydrogen content leads to the increase of the surface activity of the matrix, the concentration of active nitrogen atoms in the atmosphere is reduced, the generation of a compound layer and a grain boundary vein structure is inhibited, and the surface of the nitriding layer has excellent toughness.
Claims (10)
1. A device for in-situ deposition of a PVD coating after low-temperature rapid tough nitriding is characterized by comprising a vacuum chamber (5), a rotating frame (4), a workpiece tray (6), a matrix bias power supply (7), a first metal cathode arc group (2-1), a second metal cathode arc group (2-2), an L-shaped baffle (1), a first auxiliary anode (3-1), a second auxiliary anode (3-2), a first metal cathode arc direct current power supply (8-1), a second metal cathode arc direct current power supply (8-2), a first auxiliary anode direct current power supply (9-1) and a second auxiliary anode direct current power supply (9-2); the rotating frame (4) is positioned at the center of the bottom of the vacuum chamber (5), the rotating frame (4) is rotatably connected with the vacuum chamber (5), a first metal cathode arc group (2-1), a second metal cathode arc group (2-2), a first auxiliary anode (3-1) and a second auxiliary anode (3-2) are arranged in the vacuum chamber (5) along the circumferential direction, the first metal cathode arc group (2-1) and the second auxiliary anode (3-2) are oppositely arranged, and the second metal cathode arc group (2-2) and the first auxiliary anode (3-1) are oppositely arranged; an L-shaped baffle (1) is arranged between the second metal cathode arc group (2-2) and the rotating frame (4), the anode of the first auxiliary anode direct current power supply (9-1) is connected with the first auxiliary anode (3-1), the cathode is grounded, the anode of the second auxiliary anode direct current power supply (9-2) is connected with the second auxiliary anode (3-2), and the cathode is grounded; a first metal cathode arc direct current power supply (8-1) is connected between the first metal cathode arc group (2-1) and the vacuum chamber (5), and a second metal cathode arc direct current power supply (8-2) is connected between the second metal cathode arc group (2-2) and the vacuum chamber (5); a bias power supply (7) is connected between the rotating frame (4) and the vacuum chamber (5).
2. The device for in-situ deposition of PVD coating after low temperature fast tough nitriding according to claim 1 is characterized in that the rotating frame (4), the first metal cathode arc group (2-1), the second metal cathode arc group (2-2), the first auxiliary anode (3-1), the second auxiliary anode (3-2) and the L-shaped baffle (1) are insulated from the vacuum chamber (5).
3. The device for in-situ deposition of PVD coating after low temperature fast tough nitriding according to claim 1 is characterized in that the first metal cathode arc group (2-1), the second metal cathode arc group (2-2), the first auxiliary anode (3-1) and the second auxiliary anode (3-2) are all fixedly connected with the vacuum chamber (5) through flanges.
4. The apparatus for in-situ deposition of PVD coating after low temperature fast tough nitriding according to claim 1 is characterized in that the first metal cathode arc group (2-1) and the second metal cathode arc group (2-2) are composed of three metal cathode arcs arranged vertically, respectively.
5. The device for in-situ deposition of PVD coating after low temperature fast tough nitriding according to claim 1 is characterized in that the electrical connection end of the first metal cathodic arc group (2-1) is electrically connected with the negative pole of the first metal cathodic arc DC power supply (8-1), the electrical connection end of the second metal cathodic arc group (2-2) is electrically connected with the negative pole of the second metal cathodic arc DC power supply (8-2), and the negative pole of the bias power supply (7) is electrically connected with the electrical connection end of the rotating frame (4); the electric connection end of the vacuum chamber (5) is respectively and electrically connected with the anode of the first metal cathode arc direct current power supply (8-1), the anode of the second metal cathode arc direct current power supply (8-2) and the anode of the bias power supply (7), and the vacuum chamber (5) is grounded.
6. Method for in-situ deposition of PVD coatings after low temperature fast toughness nitriding using the device according to claim 1, characterized in that the method comprises the following steps:
firstly, pretreatment of a substrate surface: grinding and polishing the surface of a substrate, then placing the substrate in absolute ethyl alcohol for ultrasonic cleaning, drying the substrate by blowing, clamping the substrate on a workpiece tray (6) of a rotating frame (4) in a vacuum chamber (5), vacuumizing the vacuum chamber (5), and preheating the substrate;
secondly, plasma etching and cleaning the surface of the substrate: introducing argon and hydrogen into the vacuum chamber (5), and starting a second metal cathode arc direct-current power supply (8-2), a first auxiliary anode direct-current power supply (9-1) and a second auxiliary anode direct-current power supply (9-2); controlling the pulse bias voltage of the substrate bias power supply (7) to be-500V, the duty ratio is 50%, the frequency is 40KHz, after cleaning is carried out for 10min, adjusting the pulse bias voltage of the substrate bias power supply (7) to be-200V, the duty ratio is 80%, the frequency is 40KHz, and cleaning is carried out for 20 min; the current of the direct current end of the second metal cathode arc direct current power supply (8-2) is kept to be 85A in the substrate surface plasma etching cleaning process, and the current of the direct current ends of the first auxiliary anode direct current power supply (9-1) and the second auxiliary anode direct current power supply (9-2) is kept to be 100A;
thirdly, arc plasma assisted nitriding: introducing gas into a vacuum chamber (5), and performing 120min ion nitriding enhancement treatment under the conditions that the temperature in the vacuum chamber (5) is 450 ℃, the gas pressure is 0.45Pa, the direct current end current 85A of a second metal cathode arc direct current power supply (8-2), the direct current end current 100A of a first auxiliary anode direct current power supply (9-1), the direct current end current 100A of the second auxiliary anode direct current power supply (9-2) and a matrix bias power supply (7) are subjected to pulse bias voltage of-200V, the duty ratio is 80%, and the frequency is 40 KHz;
fourthly, in-situ deposition of the PVD coating: regulating the nitrogen flow to 800sccm, controlling the vacuum chamber gas pressure to be 1Pa, regulating the pulse bias voltage of the matrix bias power supply (7) to-125V, regulating the duty ratio to be 80 percent and regulating the frequency to be 40 KHz; the current 100A of the direct current end of the second auxiliary anode direct current power supply (9-2) is kept constant; starting a first metal cathode arc direct current power supply (8-1), wherein the current is 85A; turning off a second metal cathode arc direct current power supply (8-2) and a first auxiliary anode direct current power supply (9-1); and depositing the TiN coating for 120min at the temperature of 450 +/-5 ℃, thus finishing.
7. The method of claim 6, characterized in that in step one, vacuum is applied to 3 x 10 for vacuum deposition-3Pa, preheating the vacuum chamber to 450 ℃.
8. The method of in-situ deposition of PVD coating after low temperature fast toughness nitriding according to claim 6, characterized in that in step two the flow ratio of argon and hydrogen is 200: 20.
9. The method of in-situ deposition of PVD coating after low temperature fast tough nitriding according to claim 6, characterized in that the first metal cathodic arc group (2-1) and the second metal cathodic arc group (2-2) are Ti targets with a purity of 99.5%.
10. The method of in-situ deposition of PVD coating after low temperature fast toughness nitriding according to claim 6, characterized in that the gas in step three is high purity N with a flow ratio of 30:2702And high purity H2Or 80:20:200 of high-purity N2Inert gas Ar and high-purity H2The mixed gas of (1).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115161589A (en) * | 2022-07-25 | 2022-10-11 | 哈尔滨工业大学 | Device and method for in-situ deposition of PVD (physical vapor deposition) coating after ion nitriding of inner wall of pipe |
| CN115161589B (en) * | 2022-07-25 | 2024-01-05 | 哈尔滨工业大学 | Device and method for in-situ deposition of PVD coating after ion nitriding of inner wall of pipe |
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