CN213538083U - Composite filtering device combining magnetic field and lining bias stepped pipe - Google Patents
Composite filtering device combining magnetic field and lining bias stepped pipe Download PDFInfo
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- CN213538083U CN213538083U CN201822244504.4U CN201822244504U CN213538083U CN 213538083 U CN213538083 U CN 213538083U CN 201822244504 U CN201822244504 U CN 201822244504U CN 213538083 U CN213538083 U CN 213538083U
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Abstract
The invention discloses a composite filtering device combining a magnetic field and a lining bias stepped pipe, belongs to the technical field of surfaces, and aims to solve the problems of pollution of large particles in a multistage magnetic field filtering device to a film and loss in a plasma transmission process. The apparatus of the present invention comprises: the device comprises a bias voltage power supply, an arc ion plating target source and power supply, a multistage magnetic field device and power supply, a lining bias voltage stepped tube device and bias voltage power supply, a movable coil device and power supply, a sample stage, a bias voltage power waveform oscilloscope and a vacuum chamber; and (3) thin film deposition: connecting device, starting system, vacuum degree in the vacuum chamber is less than 10‑4At Pa, introducingWorking gas, starting a film coating power supply, adjusting the energy of the arc plasma by using a bias power supply, eliminating the large particle defect in the arc plasma and improving the transmission efficiency of a filtering device through a lining bias stepped pipe device and a multistage magnetic field device, reducing the loss in a vacuum chamber, setting process parameters, and preparing a film.
Description
Technical Field
The invention relates to a composite filtering device combining a magnetic field and a lining bias stepped pipe, and belongs to the technical field of surfaces.
Background
In the process of preparing the film by arc ion plating, the current density of arc spots is as high as 2.5-5 multiplied by 1010A/m2The molten liquid metal, which is caused to appear at the location of the arc spot on the target surface, is sprayed out in the form of droplets under the action of the local plasma pressure, adheres to the surface of the film or is embedded in the film to form "large particle" (Macroparticles) defects (Boxman R L, gold limit s. Macroparticle contact in lateral coatings: generation, transport and control J]Surf Coat Tech, 1992, 52(1): 39-50.). In the arc plasma, the number of electrons reaching the surface of a large particle per unit time is larger than that of ions because the moving speed of electrons is much larger than that of ions, so that the large particle is negatively charged. With respect to films of micron or submicron thickness, large particle defects of 0.1-10 microns in size, as well as PM2.5, can be a serious detriment to the quality and performance of the film. With the increasingly wide application of thin film materials and thin film technologies, the problem of large particle size defect is solved or not, which becomes the bottleneck of further development of the arc ion plating method, and the application of the arc ion plating method in the preparation of new generation thin film materials is severely restricted.
At present, in order to solve the problem that the arc ion plating method is prone to generate large grain defects when using pure metal or multi-element alloy materials with low melting points, magnetic filtration is mainly adopted to filter out large grains, such as the ceramic material prepared by the Plasma immersion ion implantation device (publication number: CN1150180, published date: 1997 5, 21) in Chinese patent, and the ceramic material prepared by the method is mainly prepared by filtering large grains of pulsed cathode arc by using a 90-degree magnetic filtration bent pipe, American scholars et al (Anders S, Anders A, Dickinson M R, Macgill R A, Brown I G. S-shaped magnetic macroparametric filter for catalytic deposition [ J ]. IEEE Trans Plasma Sci, 1997, 25(4): 670-674.) and Zhan-Nannan university (Zhang Jane Jue, Wu-Shi et al. magnetic filtration Plasma Weiwei et al. the influence of deposition conditions on the non-ferrous metal texture film in Zhan Yu Ju, Zhang Weiwei et al. magnetic filtration Plasma preparation film, 1264- & 1268.) in the article, "S" magnetic filter elbows were made to filter large particles of cathode arcs, and magnetic filtration of Twist filters proposed by American scholars et al (Anders A, MacGill R A. Twist filters for the removal of macro particles from the cathode plasma [ J ]. Surf Coat Tech, 2000, 133- & 134: 96-100.), and Dehua at Shanghai traffic university proposed adjustable open single-and dual-channel electromagnetic coil filters (D; Shanghai traffic university, 2009), which, although effective in filtering and eliminating large particles, have a significant loss in plasma transport efficiency and greatly reduced ion flux density. On the basis of filtering large particles and guaranteeing the efficiency, a straight tube filtering method is proposed in a vacuum cathode arc straight tube filter (publication number: CN1632905, published: 6/29/2005) in China patent, but the filtering effect is reduced. In summary, relevant researchers found by comparing various magnetic filtration methods (Anders A. Applicheches to red catalytic array of macro-and nanoparticles: a Review [ J ]. Surf Coat Tech, 1999, 120-. In addition, a bias electric field suppression method is adopted on the substrate, and when negative bias is applied on the substrate, the electric field can generate repulsion action on negatively charged large particles, so that the generation of large particle defects on the surface of the thin film is reduced. Olbrich et al (Olbrich W, Fessmann J, Kampschult G, Ebberenk J. Improved control of TiN coating properties using a pulsed bias with a pulsed bias [ J ]. Surf COAT Tech, 1991, 49(1-3): 258) 262. and Fessmann J, Olbrich W, Kampschult G, Ebberenk J. capacitive deposition of TiN and Zr (C, N) at low substrate pulsed bias [ J ]. Mat Sci Eng A, 1991, 140: 830.) use of pulsed bias instead of conventional DC bias to form a new technology of pulsed bias ion plating, which not only greatly reduces the surface temperature of large particles but also overcomes the high temperature of the substrate, the internal stress of the film is large, and the like. The theory of influence of bias voltage on the surface morphology of an arc ion plating film [ J ]. Metallurgical Proc, 2003, 39(5): 510) is deeply analyzed aiming at the mechanism of large particle defect reduction caused by pulse bias voltage, and the sheath movement characteristic of arc plasma can be improved, the number of large particle defects on the surface of the film can be reduced, the quality of the film can be improved, the method is widely applied to actual production, but the large particle defects can not be completely eliminated. The domestic scholars (Weiyongqiang, Zongya, Jiangqiang, Wenxianghua, Chengjibifiang, the arc ion plating method combining the magnetic filtration and the pulse bias voltage of the multistage magnetic field straight tube, the publication number is CN103276362A, the publication date is 9, 4 days in 2013) put forward the arc ion plating method combining the magnetic filtration and the pulse bias voltage of the multistage magnetic field straight tube, the large particle defect is eliminated and the transmission efficiency of the plasma is improved through the multistage magnetic field filtering device, however, the problem of contamination of the inner wall of the tube and the loss of plasma on the inner wall of the tube are not well solved, and later-stage related scholars (Weiyongqiang, dawn Asia, Hou army, Liu source, Liu scholarly, Jiangqiang, Yihan Luo. the multistage magnetic field arc ion plating method of the liner bias straight tube, publication No. CN105925940A, published date: 2016, 9/7) proposed the multistage magnetic field arc ion plating method of the liner bias straight tube to solve the problem of contamination of the inner wall of the tube. The scholars also adopt a double-layer baffle device (Zhao Y, Lin G, Xiao J, Lang W, Dong C, Gong J, Sun C. Synthesis of titanium nitride films disposed by a new shield disposed in the deposition [ J ] Appl Surf Sci, 2011, 257(13): 5694-. There are also researchers (Zhang, Hou Junda, Liu Shi, Zhang Ying Smart, magnetic filtration cathode arc plasma source and its film preparation [ J ]. Chinese surface engineering, 2002, 02): 11-15+ 20-12.) refer to the method of Bilek plate (Bilek M M M, Yin Y, McKenzie D R, Mille W I A M W I. Ion transport mechanism in a Filtered Catalytic Vacuum Arc (FCVA) system [ C ]. Proceedings of the channels and electric Insulation in Vacuum, 1996 Proceedings ISDEIV, XVIII International Symposium on, 1996: 962:. 966), and positive bias is applied to the bend of the 90 degree bend magnetic filter device to improve the plasma transmission efficiency.
Disclosure of Invention
The invention aims to solve the problems that the traditional arc ion plating method adopts a high-melting-point target material, a low-melting-point pure metal or multi-element alloy material and a non-metal material (such as graphite) as the target material and is easy to generate large-particle defects, the transmission efficiency of arc plasma is low due to a bent magnetic filtering technology, the use of target material elements is limited, the target material is uniformly ablated, the deposition density and the defects of a film are solved, the space and the deposition position of a vacuum chamber are limited, the shape of a workpiece is limited, the film component pollution is caused by the secondary sputtering of residues of different target materials in a multistage magnetic field device, and the like, the large-particle defects contained in the arc plasma are eliminated by combining a multistage magnetic field filtering method, a mechanical blocking shield of the shape of a lining bias stepped tube device and the combined action of the attraction of a bias electric field, and the, then the movable coil device is used for controlling the transmission direction of the arc plasma transmitted from the multistage magnetic field device and the lining bias stepped pipe device in the vacuum chamber, the film deposition and the film component control adjustment of the surface of the substrate workpiece at any position in the vacuum chamber are realized, the problem of uneven film deposition caused by the limitation of the deposition position or the limitation of the substrate shape caused by the layout design of the space and the target source of the vacuum chamber is solved, the defect of large particles possibly remained in the arc plasma transmitted from the multistage magnetic field device and the lining bias stepped pipe device is thoroughly eliminated, the ion energy is adjusted on the surface of the workpiece under the condition of applying negative bias, a continuous and compact high-quality film is prepared, the addition control of the content of the target element in the film is realized, the production cost of using an alloy target is reduced, the transmission efficiency of the arc plasma is improved, the deposition speed of the film is increased, and the microstructure of the film caused by the defect of, The adverse effects of continuous compact deposition and service performance, a composite filtration device combining a magnetic field and a lining bias stepped pipe is provided.
The device used by the invention comprises a bias voltage power supply (1), an arc power supply (2), an arc ion plating target source (3), a multistage magnetic field device (4), a multistage magnetic field power supply (5), a lining bias voltage stepped tube device (6), a lining bias voltage power supply (7), a movable coil device (8), a movable coil device power supply (9), a rheostat device (10), a sample table (11), a bias voltage power waveform oscilloscope (12) and a vacuum chamber (13);
in the device:
a matrix workpiece to be processed is placed on a sample table (11) in a vacuum chamber (13), a multistage magnetic field device (4), a lining bias stepped pipe device (6), a movable coil device (8) and the vacuum chamber (13) are mutually insulated, the workpiece is placed on the sample table (11), the sample table (11) is connected with a negative electrode output end of a bias power supply (1), an arc ion plating target source (3) is installed on the vacuum chamber (13) and connected with a negative electrode output end of an arc power supply (2), each stage of magnetic fields of the multistage magnetic field device (4) are connected with each output end of the multistage magnetic field power supply (5), a positive and negative connection method can be determined according to the direction of an output magnetic field, the lining bias stepped pipe device (6) is connected with a positive electrode output end of a lining bias power supply (7), the movable coil device (8) is connected with a movable coil device power supply (9) through positive and negative electrode input ends on a flange port, and, the power supply is connected to a loop of a power supply (9) of the movable coil device, and a power supply master control switch and an external water cooling circulation system are started;
and (3) thin film deposition: the vacuum chamber (13) is vacuumized, and the vacuum degree in the vacuum chamber (13) is less than 10-4When Pa is needed, working gas is introduced to 0.01-10 Pa, the bias power supply (1) and the bias power waveform oscilloscope (12) are started, the bias power supply (1) can be direct current, single pulse, multi-pulse, direct current pulse composite or bipolar pulse bias, the output bias amplitude, pulse frequency and pulse width are adjusted, the peak voltage value of the output pulse of the bias power supply (1) is 0-1.2 kV, the pulse frequency is 0 Hz-80 kHz, the pulse width is 1-90%, the working current is 0-400A, and the maximum output power is 200 kW;
starting an arc power supply (2), cleaning the surface of an arc ion plating target source (3) through arc spot movement of an electric arc, and adjusting required process parameters, wherein the current value output by the arc power supply (2) is 10-300A, and the maximum output power is 12 kW;
the multistage magnetic field device (4) is adjusted through the multistage magnetic field power supply (5), arc plasma is kept to be stably generated in the arc ion plating target source (3) and large particle defects are filtered and eliminated, the ablation uniformity of a target material is guaranteed, the utilization efficiency of the target material is improved, the arc plasma passes through the multistage magnetic field device (4) with high transmission efficiency, the multistage magnetic field device (4) adopts a red copper wire with an insulated surface, the diameter and the number of turns of the wire are determined according to passing current and magnetic field strength, the multistage magnetic field power supply (5) supplies power to magnetic fields at all levels respectively and independently, the independent adjustment of the magnetic fields at all levels is realized, and after the structure of the device is determined, the directions and the strengths of the magnetic fields at all levels output by the multistage magnetic field device (4) are adjusted through;
the inner lining bias stepped pipe device (6) can be matched with the multistage magnetic field device (4) to design the outer diameter of the stepped pipe, the structure of the stepped pipe can be matched with the multistage magnetic field device (4) to design the structure, gradient difference and inlet and outlet layout of a 2-stage stepped pipe, a 3-stage stepped pipe or a 4-stage or above stepped pipe, and each stage of stepped pipe is fixedly connected and is connected and fixed in position through a non-magnetic stainless steel rivet; the lining bias stepped pipe device (6) and the multi-stage magnetic field device (4) are movably and insulatively assembled together, and are timely disassembled, cleaned and installed according to the pollution degree of the surface, so that the problems of pollution and difficulty in cleaning of the inner wall of the pipe of the multi-stage magnetic field device (4) in a lining-plate-free state are avoided, and the pollution of thin film components caused by secondary sputtering of pollutants in the lining stepped pipe after the target material is replaced can be effectively avoided; the lining bias voltage stepped pipe device (6) is matched with the magnetic field lengths of all levels of the multistage magnetic field device (4) and the outlets of all levels of the stepped pipes, and the length of the stepped pipeHThe length of the stepped pipe is the same as that of the multistage magnetic field device (4), and the inner diameter of the stepped pipe at the right inlet isD IntoThe inner diameter of the arc ion plating target source (3) is larger than the outer diameter of the arc ion plating target source, and the inner diameter of the multistage magnetic field device (4) is smaller than the outer diameter of the arc ion plating target source, the selection is carried out according to different target materials and process parameters, and the mechanical blocking and shielding of large particles can be realized through the inner diameter change at the inlet and the outlet of the stepped pipe;
the materials of the multistage magnetic field device (4) and the lining bias stepped pipe device (6) are made of non-magnetic and cleaning-resistant 304 stainless steel materials, the multistage magnetic field device (4) determines the length, the inner diameter, the outer diameter, the thickness, the number of turns of a magnetic field and the direction according to the diameter, the cooling distance and the transmission distance of a target material, the lining bias stepped pipe device (6) determines the outer diameter of the stepped pipe according to the inner diameter of the multistage magnetic field device (4), and the stepped pipe is processed according to actual design parameters by selecting proper thickness according to the length and rigidity requirements;
the lining bias voltage power supply (7) is started, the lining bias voltage stepped pipe device (6) keeps direct current, single pulse, multiple pulses, direct current pulse composite or bipolar pulse bias, wherein the single pulse, multiple pulses or bipolar pulse bias can adjust the pulse frequency, the pulse width and the pulse type, the adjustment of the output voltage ensures that the lining bias voltage stepped pipe device (6) attracts large particles, the deposited ions are repelled, the loss of the arc plasma in the pipe transmission process is reduced, the large particle defect of the arc plasma is reduced or even eliminated, the transmission efficiency of the arc plasma and the deposition speed of a film are improved, the voltage parameter of the lining bias voltage power supply (7) is-200 to +200V, and the lining bias voltage power supply is a direct current, single pulse, multiple pulses, direct current pulse composite or bipolar pulse power supply, wherein the pulse type can adjust the pulse frequency, The pulse width and the pulse type can generate periodic or continuous and stable attraction to the large particle defects in the deposition process, thereby greatly reducing the probability that the large particles pass through the multistage magnetic field device (4) and the lining bias stepped pipe device (6);
the power supply (9) of the movable coil device is started, the input current of the movable coil device (8) is adjusted, the adjustment of the magnetic field direction and the magnetic field intensity is realized, the adjustment of the number of coil turns, the coil distance, the shape, the transmission path and the like of the movable coil device (8) is used for controlling the arc plasma transmitted from the multistage magnetic field device (4) and the lining bias stepped pipe device (6), the shape of the movable coil device is matched with the magnetic force line layout and the direction of the magnetic field, the movable coil can adopt a classic 90-degree bending type, and can also adopt a linear and bending and linear combination (the magnetic force line of the linear part is tangent and intersected with the magnetic force line of the bending part), a linear and linear combination (the magnetic force lines of the two linear parts are intersected), a linear, arc and linear combination (the combination of the three sections are intersected and tangent) and a combination of the circular arc, the linear and the circular arc, the circular arc and the straight line part are determined according to the requirements of the space position and the transmission path, so that the circular arc and the straight line part reach the surface of the substrate with higher transmission efficiency, the problem of uneven film deposition caused by the limitation of the deposition position or the limitation of the substrate shape due to the space of a vacuum chamber and the layout design of a target source is solved, and the film is rapidly deposited; the rheostat device (10) adjusts output resistance, positive bias voltage change on the movable coil device (8) is realized, an electric field generated by the positive bias voltage can attract electrons and residual large particles in the arc plasma transmitted from the multistage magnetic field device (4) and the lining bias voltage stepped pipe device (6), the ion number of the arc plasma output from the movable coil device (8) is increased, the transmission efficiency of the arc plasma in the movable coil device (8) is improved, and the residual large particle defect is eliminated; the movable coil device (8) selects a copper tube with low resistance, and the diameter, the thickness and the length of the copper tube are determined according to the number of turns of the movable coil device (8), the diameter of a coil channel, the shape of a coil, the distance between turns of the coil, the size of a vacuum chamber, the transmission path and the transmission distance of arc plasma; the positive electrode and the negative electrode of a power supply (9) of the movable coil device provide proper current for the movable coil device (8) according to the magnetic field intensity, the direction and the cooling system, the input range of the current is 0-2000A, the stability of the whole vacuum system and the proper magnetic field output by the movable coil device (8) are ensured, arc plasma is transmitted according to the path set by the movable coil device (8), the residual large particles are removed, the surface of a matrix is reached with high transmission efficiency, the loss of the arc plasma in a vacuum chamber (13) is avoided, and the rapid deposition of a film is realized;
the arc ion plating target source (3), the multistage magnetic field device (4) and the movable coil device (8) adopt a direct water cooling mode, the problem of temperature rise in the working process is avoided, and an external water cooler system provides enough cooling water flow and cooling temperature to ensure the normal operation of the whole vacuum system.
According to the preparation requirement of the film, relevant process parameters are adjusted to prepare pure metal films, compound ceramic films with different element ratios, functional films and high-quality films with nano multilayer or gradient structures.
The invention has the advantages that: a. by utilizing the matching of the shape of the movable coil device and the layout and direction of magnetic force lines of a magnetic field, the movable coil can adopt a classical 90-degree bending type, and can also adopt typical coil structure combinations such as straight lines, bending, straight line combination (the magnetic force lines of the straight line part are tangent and intersected with the magnetic force lines of the bent part), straight line and straight line combination (the magnetic force lines of the two straight line parts are intersected), straight lines, arcs and straight lines combination (the combination of three sections are intersected and tangent) and arcs, straight lines and arcs combination (the tangency and the intersection among the three parts) and the like, wherein the arcs and the straight line parts are determined according to the requirements of spatial positions and transmission paths, the effective control of an arc plasma transmission path is realized, the large particle defects remained in the multistage magnetic field device and the lining bias stepped pipe device are further eliminated, and the loss of the arc plasma in the transmission, the transmission efficiency of the arc plasma and the deposition speed of the film are further improved by guiding the magnetic field of the movable coil, the problem of uneven film deposition caused by deposition position limitation or matrix shape limitation caused by the layout design of the space and the target source of the vacuum chamber is solved, the film can be prepared at the optimal position of the vacuum chamber, the series resistance value of the movable coil can be adjusted by the rheostat device, the adjustment of the positive bias parameters of the movable coil is realized, the attraction of electrons and residual large particles in the arc plasma is realized, the transmission efficiency of the arc plasma in the movable coil is improved, the residual large particle defect is eliminated, and the deposition speed of the film is increased; b. the multistage magnetic field filtering device can ensure the stable movement of the electric arc on the surface of the target through the constraint of the magnetic field to generate continuous electric arc plasma, the high-efficiency transmission of the electric arc plasma in the multistage magnetic field device is realized through the magnetic lines of force of the multistage magnetic field, the moving path of the electric arc plasma and the large particle defect is changed to realize the separation of the electric arc plasma and the large particle defect, and the large particle defect in the electric arc plasma is further reduced or even eliminated; c. the lining bias stepped pipe device can apply positive bias compounded by direct current, pulse or direct current pulse to continuously or periodically effectively attract large particles and continuously or periodically repel deposited ions, and can also reduce the loss of plasma in the transmission process in the pipe through bipolar pulse oscillation of the positive bias and the negative bias, thereby further improving the transmission efficiency of arc plasma and the deposition speed of a film; d. the lining bias stepped pipe device can eliminate large particle defects in arc plasma by limiting the motion path of the large particle defects through the shape of the lining bias stepped pipe device, through the inner diameter change of an inlet and an outlet of the stepped pipe and the structural combination of the stepped pipe, reduce the probability that the large particles reach the surface of a deposition sample through the stepped pipe device, realize mechanical blocking and shielding of the large particles, be flexibly disassembled and conveniently cleaned, avoid the problem of pollution cleaning of the inner wall of a multi-stage magnetic field device in a lining-free state, and effectively avoid the pollution of film components caused by the secondary sputtering of different targets on the lining stepped pipe pollutants after the target is replaced; e. the pulse bias power supply eliminates the residual large particle defects and adjusts and optimizes the energy of the arc plasma by adjusting the pulse type, the pulse amplitude, the pulse width and the pulse frequency and utilizing the rejection suppression effect of the electric field; f. the microstructure and the performance of the prepared film can be adjusted through pulse bias parameters, the pinning effect of high-energy ions on the growth of the film is realized by utilizing the type, the amplitude, the pulse width and the frequency of the pulse bias, the crystal structure and the stress state of the growth of the film are improved, the bonding strength is improved, and the service performance of the film is improved; g. the film prepared by the composite type filtering device with the combined magnetic field and the lining bias stepped pipe eliminates the defect of large particles in the film, reduces the loss of arc plasma in the filtering device and the vacuum chamber, improves the use efficiency of the arc plasma, realizes the rapid preparation of the film, can ensure that the crystal structure and the microstructure of the film are more compact, and is beneficial to further improving the use performance of the film.
The composite filtering device combining the magnetic field and the lining bias stepped pipe can be combined in a single set or multiple sets, and the combination of multiple types of the multistage magnetic field device (4), the lining bias stepped pipe device (6) and the movable coil device (8) is combined to prepare a pure metal film, a compound ceramic film with different element proportions, a functional film and a film with a nano multilayer or gradient structure, or a single set or multiple sets of the device are adopted and combined to adopt the traditional direct current magnetron sputtering, the pulse magnetron sputtering, the traditional electric arc ion plating, the pulse cathode arc and direct current bias, the pulse bias or the direct current pulse composite bias device to realize the combination of two or more deposition modes to carry out film deposition, so as to prepare the pure metal film, the compound ceramic film with different element proportions, the functional film and a high-quality film with the nano multilayer or gradient structure.
Drawings
FIG. 1 is a simplified assembly diagram of a composite filtration device incorporating a magnetic field and a biased stepped pipe lining in accordance with the present invention; FIG. 2 is a 7-configuration layout of the moving coil; figure 3 is a schematic view of the structure of the lining biased stepped tube device.
Detailed Description
The first embodiment is as follows: the present embodiment is described below with reference to fig. 1, 2 and 3, and the device used in the composite filtering device combining a magnetic field and a lining bias stepped tube in the present embodiment includes a bias power supply (1), an arc power supply (2), an arc ion plating target source (3), a multi-stage magnetic field device (4), a multi-stage magnetic field power supply (5), a lining bias stepped tube device (6), a lining bias power supply (7), a movable coil device (8), a movable coil device power supply (9), a rheostat device (10), a sample stage (11), a bias power waveform oscilloscope (12) and a vacuum chamber (13);
in the device:
a matrix workpiece to be processed is arranged on a sample table (11) in a vacuum chamber (13), a multistage magnetic field device (4) and a lining bias stepped pipe device (6), the movable coil device (8) and the vacuum chamber (13) are mutually insulated, a workpiece is placed on the sample table (11), the sample table (11) is connected with the negative output end of the bias power supply (1), the arc ion plating target source (3) is installed on the vacuum chamber (13) and is connected with the negative output end of the arc power supply (2), each stage of magnetic field of the multistage magnetic field device (4) is connected with each output end of the multistage magnetic field power supply (5), the positive and negative connection method can be determined according to the direction of the output magnetic field, the lining bias stepped pipe device (6) is connected with the positive output end of the lining bias power supply (7), the movable coil device (8) is connected with the movable coil device power supply (9) through the positive and negative input ends on a flange port, and an external water cooling circulation system;
and (3) thin film deposition: the vacuum chamber (13) is vacuumized, and the vacuum degree in the vacuum chamber (13) is less than 10-4When Pa is needed, the working gas is introduced to 0.01 Pa-10 Pa, the bias power supply (1) and the bias power waveform oscilloscope (12) are started, and the bias power supply (1) can be direct current, single pulse or multi-pulseThe method comprises the steps of performing impulse and direct current pulse composite or bipolar pulse bias voltage, adjusting the output bias voltage amplitude, the pulse frequency and the pulse width, adjusting the peak voltage value of the output pulse of a bias power supply (1) to be 0-1.2 kV, the pulse frequency to be 0 Hz-80 kHz, the pulse width to be 1-90%, the working current to be 0-400A and the maximum output power to be 200 kW;
starting an arc power supply (2), cleaning the surface of an arc ion plating target source (3) through arc spot movement of an electric arc, and adjusting required process parameters, wherein the current value output by the arc power supply (2) is 10-300A, and the maximum output power is 12 kW;
the multistage magnetic field device (4) is adjusted through the multistage magnetic field power supply (5), arc plasma is kept to be stably generated in the arc ion plating target source (3) and large particle defects are filtered and eliminated, the ablation uniformity of a target material is guaranteed, the utilization efficiency of the target material is improved, the arc plasma passes through the multistage magnetic field device (4) with high transmission efficiency, the multistage magnetic field device (4) adopts a red copper wire with an insulated surface, the diameter and the number of turns of the wire are determined according to passing current and magnetic field strength, the multistage magnetic field power supply (5) supplies power to magnetic fields at all levels respectively and independently, the independent adjustment of the magnetic fields at all levels is realized, and after the structure of the device is determined, the directions and the strengths of the magnetic fields at all levels output by the multistage magnetic field device (4) are adjusted through;
the inner lining bias stepped pipe device (6) can be matched with the multistage magnetic field device (4) to design the outer diameter of the stepped pipe, the structure of the stepped pipe can be matched with the multistage magnetic field device (4) to design the structures, gradient difference and inlet and outlet layout of a 2-stage stepped pipe, a 3-stage stepped pipe or a 4-stage or above stepped pipe, the stepped pipes of each stage are fixedly connected, and the connection and position fixation are carried out through bolts and nuts of non-magnetic stainless steel; the lining bias stepped pipe device (6) and the multi-stage magnetic field device (4) are movably and insulatively assembled together, and are timely disassembled, cleaned and installed according to the pollution degree of the surface, so that the problems of pollution and difficulty in cleaning of the inner wall of the pipe of the multi-stage magnetic field device (4) in a lining-plate-free state are avoided, and the pollution of thin film components caused by secondary sputtering of pollutants in the lining stepped pipe after the target material is replaced can be effectively avoided; inner lining bias ladder tube device (6) and multistage magnetic field device (4)The lengths of the magnetic fields at all levels are matched with the outlets of the stepped pipes at all levels, and the lengths of the stepped pipesHThe length of the stepped pipe is the same as that of the multistage magnetic field device (4), and the inner diameter of the stepped pipe at the right inlet isD IntoThe diameter of the arc ion plating target source (3) is larger than the diameter of the arc ion plating target source, and the diameter of the arc ion plating target source is smaller than the diameter of the multistage magnetic field device (4), the selection is carried out according to different targets and process parameters, and the mechanical blocking shielding of large particles can be realized through the change of the inner diameters at the inlet and the outlet of the stepped pipe (as shown in figure 3);
the materials of the multistage magnetic field device (4) and the lining bias stepped pipe device (6) are made of non-magnetic and cleaning-resistant 304 stainless steel materials, the multistage magnetic field device (4) determines the length, the inner diameter, the outer diameter, the thickness, the number of turns of a magnetic field and the direction according to the diameter, the cooling distance and the transmission distance of a target material, the lining bias stepped pipe device (6) determines the outer diameter of the stepped pipe according to the inner diameter of the multistage magnetic field device (4), and the stepped pipe is processed according to actual design parameters by selecting proper thickness according to the length and rigidity requirements;
the lining bias voltage power supply (7) is started, the lining bias voltage stepped pipe device (6) keeps direct current, single pulse, multiple pulses, direct current pulse composite or bipolar pulse bias, wherein the single pulse, multiple pulses or bipolar pulse bias can adjust the pulse frequency, the pulse width and the pulse type, the adjustment of the output voltage ensures that the lining bias voltage stepped pipe device (6) attracts large particles, the deposited ions are repelled, the loss of the arc plasma in the pipe transmission process is reduced, the large particle defect of the arc plasma is reduced or even eliminated, the transmission efficiency of the arc plasma and the deposition speed of a film are improved, the voltage parameter of the lining bias voltage power supply (7) is-200 to +200V, and the lining bias voltage power supply is a direct current, single pulse, multiple pulses, direct current pulse composite or bipolar pulse power supply, wherein the pulse type can adjust the pulse frequency, The pulse width and the pulse type can generate periodic or continuous and stable attraction to the large particle defects in the deposition process, thereby greatly reducing the probability that the large particles pass through the multistage magnetic field device (4) and the lining bias stepped pipe device (6);
the power supply (9) of the movable coil device is turned on, the input current of the movable coil device (8) is adjusted, the adjustment of the magnetic field direction and the magnetic field intensity is realized, the adjustment of the number of turns of the coil, the coil distance, the shape, the transmission path and the like of the movable coil device (8) is used for controlling the arc plasma transmitted from the multistage magnetic field device (4) and the lining bias stepped tube device (6), so that the arc plasma reaches the surface of the substrate with higher transmission efficiency, the problem of uneven film deposition caused by the limitation of the deposition position or the limitation of the substrate shape due to the space of a vacuum chamber and the layout design of a target source is solved, and the rapid deposition of the film; the rheostat device (10) adjusts output resistance, positive bias voltage change on the movable coil device (8) is realized, an electric field generated by the positive bias voltage can attract electrons and residual large particles in the arc plasma transmitted from the multistage magnetic field device (4) and the lining bias voltage stepped pipe device (6), the ion number of the arc plasma output from the movable coil device (8) is increased, the transmission efficiency of the arc plasma in the movable coil device (8) is improved, and the residual large particle defect is eliminated; the movable coil device (8) selects a copper tube with low resistance, and the diameter, the thickness and the length of the copper tube are determined according to the number of turns of the movable coil device (8), the diameter of a coil channel, the shape of a coil, the distance between turns of the coil, the size of a vacuum chamber, the transmission path and the transmission distance of arc plasma; the positive electrode and the negative electrode of a power supply (9) of the movable coil device provide proper current for the movable coil device (8) according to the magnetic field intensity, the direction and the cooling system, the input range of the current is 0-2000A, the stability of the whole vacuum system and the proper magnetic field output by the movable coil device (8) are ensured, arc plasma is transmitted according to the path set by the movable coil device (8), the residual large particles are removed, the surface of a matrix is reached with high transmission efficiency, the loss of the arc plasma in a vacuum chamber (13) is avoided, and the rapid deposition of a film is realized;
the arc ion plating target source (3), the multistage magnetic field device (4) and the movable coil device (8) adopt a direct water cooling mode, the problem of temperature rise in the working process is avoided, and an external water cooler system provides enough cooling water flow and cooling temperature to ensure the normal operation of the whole vacuum system.
The output waveform of the bias power supply (1) is direct current, single pulse, direct current pulse composite, multi-pulse composite or bipolar pulse.
The output direct current of the arc power supply (2), single pulse, direct current pulse composite or multi-pulse composite.
The arc ion plating target source (3) adopts high-melting point target materials, low-melting point pure metal or multi-element alloy materials and non-metal materials (such as graphite), and can use a single target, a plurality of targets or a composite target to carry out pure metal thin films, compound ceramic thin films with different element ratios, functional thin films, multi-element multi-layer, superlattice and high-quality thin films with nano multi-layer or gradient structures.
The working gas is argon or the mixed gas of one or more of nitrogen, acetylene, methane, silane or oxygen to prepare pure metal film, compound ceramic film with different element proportions, functional film, multi-component multi-layer, superlattice, nano multi-layer or gradient structure film.
A composite filter device combining a magnetic field and a lining bias stepped pipe utilizes the shape of a movable coil device and the matching of the magnetic line layout and direction of the magnetic field (as shown in figure 1-2), the movable coil can adopt a classic 90-degree bending type, and can also adopt typical coil structure combinations such as straight line and bending, bending and straight line combination (the magnetic line of the straight line part is tangent and intersected with the magnetic line of the bending part), straight line and straight line combination (the magnetic line of the two straight line parts is intersected), straight line, arc and straight line combination (the three parts are intersected and tangent) and arc, straight line and arc combination (the three parts are tangent and intersected) and the like, wherein the arc and the straight line part are determined according to the space position and the requirement of a transmission path, the effective control of an arc plasma transmission path is realized, and the large particle defect remained in the multistage magnetic field device and the lining bias stepped pipe device is further removed, the loss of plasma in the transmission process of the vacuum chamber is reduced, the transmission efficiency of arc plasma and the deposition speed of a film are further improved by guiding the magnetic field of the movable coil, the problem of uneven film deposition caused by the limitation of deposition positions or the limitation of matrix shapes due to the space of the vacuum chamber and the layout design of a target source is solved, the film can be prepared at the optimal position of the vacuum chamber, the series resistance value of the movable coil can be adjusted by the rheostat device, the adjustment of the positive bias parameters of the movable coil is realized, the attraction of electrons and residual large particles in the arc plasma is realized, the transmission efficiency of the arc plasma in the movable coil is improved, the defect of the residual large particles is eliminated, and the deposition speed of the film is increased; the stable movement of the electric arc on the surface of the target material is ensured by utilizing the magnetic field constraint of the multistage magnetic field filtering device, continuous electric arc plasma is generated, the high-efficiency transmission of the electric arc plasma in the multistage magnetic field device is realized through the magnetic lines of the multistage magnetic field, the moving path of the electric arc plasma and the large particle defect is changed to realize the separation of the electric arc plasma and the large particle defect, and the large particle defect in the electric arc plasma is further reduced or even eliminated; the lining bias stepped pipe device is utilized to apply direct current, pulse or direct current pulse composite positive bias to continuously or periodically effectively attract large particles, thereby effectively avoiding the problem of large particles generated by low-melting-point materials, the device can continuously or periodically repel the deposited ions, can reduce the loss of plasma in the transmission process of the tube through the bipolar pulse oscillation of positive and negative bias voltage, further improve the transmission efficiency of arc plasma and the deposition speed of a film, can ensure that the lining bias stepped tube device can be formed by the shape of the device, the large particle defects in the arc plasma are eliminated by limiting the motion path of the large particle defects through the inner diameter change of the inlet and the outlet of the stepped pipe and the structural combination of the stepped pipe, the probability that the large particles reach the surface of a deposition sample through the stepped pipe device is reduced, and the mechanical blocking and shielding effect on the large particle defects is realized; the lining bias stepped pipe device is flexibly disassembled and is convenient to clean, the problem that the inner wall of the pipe of the multistage magnetic field device is polluted and cleaned in a lining-plate-free state is solved, and the pollution of thin film components caused by secondary sputtering of pollutants in the lining stepped pipe after the target material is replaced can be effectively avoided; the pulse bias power supply eliminates the residual large particle defects and adjusts and optimizes the energy of the arc plasma by adjusting the pulse type, the pulse amplitude, the pulse width and the pulse frequency and utilizing the rejection suppression effect of the electric field, improves the interval potential distribution of the plasma near the matrix, fully attracts the arc plasma to move towards a workpiece, and realizes the rapid deposition of the film; the microstructure and the performance of the prepared film can be adjusted through pulse bias parameters, the pinning effect of high-energy ions on the growth of the film is realized by utilizing the type, the amplitude, the pulse width and the frequency of the pulse bias, the crystal structure and the stress state of the growth of the film are improved, the bonding strength is improved, and the service performance of the film is improved; meanwhile, the arc ion plating technology is utilized to generate stable and continuous metal plasma with high ionization rate, which is beneficial to the chemical synthesis reaction of ions with high ionization rate on the surface of a workpiece, and compound ceramic films, functional films, multi-component multi-layer films, super lattices and films with gradient structures or pure metal films with different element ratios are prepared; the film prepared by the composite filtering device of the combined magnetic field and the lining bias stepped pipe eliminates the defect of large particles in the film, reduces the loss of arc plasma in the filtering device and the vacuum chamber, avoids the pollution of the lining stepped pipe residues to the film caused by the replacement of different targets, improves the use efficiency of the arc plasma, realizes the quick preparation of the film, optimizes the energy distribution of the arc plasma by using pulse bias, can ensure that the crystal structure and microstructure of the film are more compact, and is favorable for further improving the use performance of the film.
The second embodiment is as follows: the difference between this embodiment and the first embodiment is that the apparatus can also realize the following additional functions: the method can combine one or more than two devices of the traditional direct current magnetron sputtering, the pulse magnetron sputtering, the traditional arc ion plating and the pulse cathode arc, and then apply a direct current bias voltage, a pulse bias voltage, a direct current pulse composite bias voltage or a bipolar pulse bias voltage device on the workpiece to carry out film deposition to prepare pure metal films, compound ceramic films with different element ratios, functional films and high-quality films with nano multilayer or gradient structures.
The third concrete implementation mode: the difference between the second embodiment and the first embodiment is that the combined magnetic field is connected with the composite filtering device of the lining bias stepped pipe, the arc power supply (2) is turned on, the multistage magnetic field power supply (5) is turned on to adjust the multistage magnetic field device (4), the lining bias power supply (7) is turned on, the lining bias stepped pipe device (6) keeps direct current positive bias, the bias power supply (1) is turned on, the movable coil device power supply (9) is turned on to adjust the movable coil device (8), the rheostat device (10) is used for adjusting output resistance, adjusting process parameters and performing thin film deposition to prepare multilayer structure thin films with different stress states, microstructures and element proportions, and the other parts are the same as those of the second embodiment.
The fourth concrete implementation mode: the difference between the first embodiment and the second embodiment is that a combined magnetic field is connected with a composite filtering device of a lining bias stepped pipe, an arc power supply (2) is started, a multistage magnetic field power supply (5) is started to adjust a multistage magnetic field device (4), a lining bias power supply (7) is started, a lining bias stepped pipe device (6) keeps direct current positive bias, a bias power supply (1) is started, a movable coil device power supply (9) is started to adjust a movable coil device (8), a rheostat device (10) is used for adjusting output resistance, technological parameter adjustment and film deposition, one or more than two methods of traditional direct current magnetron sputtering, pulse magnetron sputtering, traditional electric arc ion plating and pulse cathode arc are combined, and then direct current bias, pulse bias, direct current pulse composite bias or bipolar pulse bias devices are applied to a workpiece to perform film deposition, the rest is the same as in the second embodiment.
The fifth concrete implementation mode: the difference between the first embodiment and the second embodiment is that a composite type filtering device of a combined magnetic field formed by combining 2 sets or more of arc ion plating target sources (3), a multi-stage magnetic field device (4), a lining bias stepped pipe device (6) and a movable coil device (8) and a lining bias stepped pipe can be used for film deposition by taking various pure metal elements and multi-element alloy materials as targets, one or more methods of traditional direct current magnetron sputtering, pulse magnetron sputtering, traditional arc ion plating and pulse cathode arc are combined, and then a direct current bias, a pulse bias or a direct current pulse composite bias device is applied to a workpiece for film deposition to prepare a multilayer structure film with different stress states, microstructures and element ratios.
Claims (1)
1. The composite filtering device for the combined magnetic field and the lining bias stepped pipe is characterized by comprising a bias power supply (1), an arc power supply (2), an arc ion plating target source (3), a multistage magnetic field device (4), a multistage magnetic field power supply (5), a lining bias stepped pipe device (6), a lining bias power supply (7), a movable coil device (8), a movable coil device power supply (9), a rheostat device (10), a sample table (11), a bias power waveform oscilloscope (12) and a vacuum chamber (13);
in the device:
a matrix workpiece to be processed is placed on a sample table (11) in a vacuum chamber (13), a multistage magnetic field device (4), a lining bias stepped pipe device (6), a movable coil device (8) and the vacuum chamber (13) are mutually insulated, the workpiece is placed on the sample table (11), the sample table (11) is connected with a negative electrode output end of a bias power supply (1), an arc ion plating target source (3) is installed on the vacuum chamber (13) and connected with a negative electrode output end of an arc power supply (2), each stage of magnetic fields of the multistage magnetic field device (4) are connected with each output end of the multistage magnetic field power supply (5), a positive and negative connection method is determined according to an output magnetic field direction, the lining bias stepped pipe device (6) is connected with a positive electrode output end of the lining bias power supply (7), the movable coil device (8) is connected with a movable coil device power supply (9) through positive and negative electrode input ends on a flange port, and a rheo, and the power supply master control switch and an external water cooling circulation system are started when the power supply master control switch is connected into a loop of a power supply (9) of the movable coil device.
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