CN101403101A - Quick solid-ceramic coating ion plating apparatus - Google Patents

Abstract

The invention discloses a rapid hard ceramic coating ion plating device. The device comprises a vacuum chamber surrounded by a furnace wall. The circular arc target is divided into 2N columns, N≥1, evenly distributed on the furnace wall, the cylindrical high-power rotary arc target is located in the center of the vacuum chamber, the circular arc target and The space between the central high-power cylindrical arc targets is the ion plating deposition area, and the workpiece racks are distributed in the ion plating deposition area. This kind of equipment makes full use of the high ionization rate of the arc ion plating technology, greatly improves the deposition efficiency of ceramic coatings, and overcomes the shortcomings of the prior art, such as the need to add expensive ion sources to improve adhesion. It has the advantages of high coating efficiency, low coating cost and convenient operation. It can meet the requirements of ultra-thick ceramic coating in industry. It has a good application prospect in industrialized mass production.

Description

A fast hard ceramic coating ion plating device

technical field

The invention relates to a rapid hard ceramic coating ion plating device, which belongs to the technical field of coating.

Background technique

Chromium electroplating is widely used in aerospace, machinery, electronics, chemical industry, hardware and other industries, and is the most widely used surface coating. However, the wastewater discharged from the chromium electroplating process contains a variety of heavy metals, especially the carcinogenic hexavalent chromium, which seriously pollutes the surrounding environment. With the increasing emphasis on environmental protection, developed countries have completely banned the use of electrochrome plating technology, and all of them have been subcontracted to developing countries including China, which has caused serious pollution to the environment. In response to the increasingly serious environmental problems, the country has adopted more stringent environmental policies. Recently, it is stipulated that the production of chromic anhydride, the most critical raw material for chromium plating, should be gradually reduced in China, which will lead to the closure of many electroplating enterprises.

In order to seek alternative technologies, a lot of work has been done at home and abroad for a long time. Mainly concentrated in electroless nickel phosphorus plating, thermal spraying, brush plating. There is a certain degree of pollution in the electroless nickel-phosphorus plating process, and the hardness is low (Hv 500-600); the efficiency of thermal spraying is high, but there are certain requirements for the substrate material, the sprayed material is limited, and the sprayed surface is rough, requiring two Secondary processing; brush plating has better adhesion than electroplating, and it has a better effect on parts with relatively simple shapes. It plays a good role in the repair of large shafts of large mechanical equipment, but it cannot be used for workpieces with complex shapes. An effective coating that cannot be compared in performance to electrochrome plating. It is a development trend in recent years to use non-polluting physical vapor deposition technology (Physical Vapor Deposition: PVD) to plate ceramic coatings instead of traditional electroplated chromium coatings. Many research institutions at home and abroad have made many beneficial attempts, including electronic Beam evaporation, ion beam sputtering, cathodic arc deposition, and magnetron sputtering. Among them, the efficiency of electron beam evaporation coating is high, but its coating has strong directionality, poor uniformity, low adhesion, and is not conducive to the preparation of complex-shaped workpieces; the coating prepared by traditional magnetron sputtering method has no droplet problem, At the same time, the preparation temperature is low, and it can be prepared on various substrate materials (such as steel, non-ferrous metals, plastics, etc.), but there are fewer energy-carrying ions, and the coating rate is low, making it difficult to prepare thick films. In the above method, the growth rate of the coating decreases after reaching a certain thickness during thick film preparation, and at the same time, the coating will fall off due to the increase of stress, so large-scale industrial production cannot be carried out.

Due to the characteristics of high ionization rate, fast deposition rate, high ion energy and low cost, arc ion plating technology can prepare thin films with large area, good density and excellent crystallization at room temperature. The preparation method is simple and the process parameters are easy to control. , suitable for industrial production, is the main preparation technology of hard coating at present. However, the number of targets in conventional arc ion plating equipment is small, and the vacuum chamber is large, resulting in relatively low plasma density in the entire equipment, and poor deposition rate, hardness and adhesion of the coating. The deposition rate is generally below 3 microns/hour. Among the existing electroplating products, many products require a coating of 80-100 microns. In order to meet the replacement requirements, the thickness of the PVD ceramic coating must be more than 20 microns. The existing conventional arc ion plating coating equipment has a relatively low deposition rate. Low, basically unable to meet the requirements of thick coating.

Contents of the invention

The purpose of the present invention is to overcome the shortcomings of coating deposition rate, hardness and poor adhesion in existing arc ion plating equipment, and provide a fast hard ceramic coating ion plating device, which has better ion plating effect and thick film plating capabilities.

The technical scheme for realizing the object of the present invention is: a kind of rapid ceramic coating ion plating device, at least comprises the vacuum chamber that is surrounded by furnace wall, and vacuum chamber is provided with vacuum port, and furnace wall side is provided with furnace door, and vacuum chamber is provided with There is a circular arc target and a high-power rotary arc target controlled by a magnetic field. The circular arc target is divided into 2N columns, N≥1, evenly distributed on the furnace wall. The high-power rotary arc target is located in the center of the vacuum chamber. The circular arc target The space between the high-power rotary arc target and the high-power rotary arc target is the ion plating deposition area, the workpiece rack is distributed in the ion plating deposition area, and the circular arc target and the high-power rotary arc target are respectively connected to the power supply.

The above-mentioned circular arc targets are divided into four rows and evenly distributed on the furnace wall. There is a magnet behind the circular arc target, and a coil behind the high-power rotating arc target. The magnetic field is generated by electrifying the coil. The high-power rotating arc target is cylindrical, and its current range is 150-300A. The diameter of the circular arc target is 60-100mm, and there are 12-16 circular arc targets. The circular arc target and the high-power rotary arc target are made of Cr, Zr or Ti. The height of the vacuum chamber is 0.5-1.5 meters, and the diameter is 700-900mm. All ion plating deposition areas are annular areas. A plurality of heaters are arranged near the furnace wall in the vacuum chamber. And a driving mechanism is arranged under the workpiece rack, and an autorotation turntable and a revolution turntable driven by the drive mechanism, the workpiece rack is installed on the autorotation turntable, and the autorotation turntable is installed on the revolution turntable.

It can be seen from the above technical scheme that the vacuum chamber of the present invention is equipped with a circular arc target, a cylindrical high-power rotating target and an independent workpiece holder. The circular arc target is evenly distributed on the vacuum furnace wall, and the cylindrical high-power rotating arc target is located in the vacuum furnace. In the center, the workpiece holder is located in the ion plating deposition area between the circular arc target and the cylindrical arc target. In the vacuum chamber, there are 12-16 arc targets in total. Through this layout, the magnetic field tightly confines the plasma between the circular arc target and the high-power arc target, and the plasma density is greatly increased. When the complex workpiece is coated, due to the high ionization rate of the arc target, the workpiece is immersed in the plasma, the effect of ion bombardment is very significant, and the uniformity of the coating is well guaranteed.

In the present invention, the space between the arc target and the magnetron target is an annular ion plating deposition area. Due to the high ionization rate of the arc target, the magnetic field tightly confines the plasma between the arc target and the magnetron target, so that the deposition The plasma density of the region is greatly improved. In conventional coating equipment, due to the small number of targets, the workpiece must rotate for revolution and rotation during coating. When the workpiece faces the target, the coating is deposited, but when the tool turns in front of the target and away from the target, the coating cannot be performed. process, so the coating rate is low, and the preparation of thick coatings cannot be carried out. However, in this coating device, since the entire wall of the vacuum chamber is filled with targets, and there are targets in the middle of the vacuum chamber, the workpiece can face more targets during coating. And when it turns to face the target in the middle of the vacuum chamber, it is still coating, and there is almost no free non-coating time, so the deposition rate of the coating is more than twice as fast as that of conventional equipment. In addition, when coating various complex workpieces, the workpiece is completely immersed in the plasma, the effect of ion bombardment is very significant, and the uniformity of the coating is well guaranteed.

In the invention, the workpiece frame is driven by the driving mechanism to rotate and revolve in the annular ion plating deposition area, which improves the uniformity of the coating. A heater is installed on the wall of the vacuum chamber, which can easily adjust the temperature in the vacuum chamber.

The present invention is different from the coating equipment commonly used at home and abroad. It fully utilizes arc ion technology and cylindrical high-power rotating arc target technology. It can not only prepare various single thick coatings such as TiN, CrN, ZrN, etc., but also prepare multiple Thick coatings such as TiAlN, CrAlN, etc., have improved the uniformity of coating thickness, improved coating quality, and improved coating adhesion. It is very convenient to carry out research and production of various coatings. The present invention can adopt computer to carry out automatic control and semi-automatic control production process, and its comprehensive performance is greatly improved. Therefore, the invention not only makes the application field wider and has higher production efficiency, but also ensures the uniformity of equipment coating in a wide range, higher coating quality and stronger adhesion.

In a word, the equipment provided by the present invention fully embodies the advantages of various advanced coating technologies, overcomes the shortcomings of many existing preparation systems, and has the characteristics of high coating efficiency, low coating cost, and convenient operation. It can conveniently carry out large-scale industrial production and has great application value.

Description of drawings

Fig. 1 is a structural schematic diagram of the present invention.

Fig. 2 is a surface topography diagram of a CrN thick coating prepared by the device of the present invention.

Fig. 3 is the CrN coating cross-sectional scanning electron microscope morphology figure prepared under the condition of 30 minutes with the device of the present invention

Fig. 4 is a cross-sectional scanning electron microscope morphology diagram of a CrN coating prepared by the device of the present invention under the condition of 120 minutes.

In the figure 1. Furnace door, 2. Vacuum exhaust port, 3. Heater, 4. High-power rotating arc target, 5. Workpiece rack, 6. Circular arc target

Detailed ways

The technical scheme of the present invention is further described below in conjunction with specific embodiment:

As shown in Fig. 1, the vacuum chamber of the fast hard ceramic coating ion plating device provided by the present invention is surrounded by furnace walls, the height of the vacuum chamber is 0.5-1.5 meters, and the diameter is 700-900mm. A furnace door 1 is provided on the side of the vacuum chamber to facilitate loading and unloading of workpieces. The vacuum chamber is equipped with a vacuum port 2, through which the vacuum pumping unit can vacuum the vacuum chamber. The vacuum pumping unit can be composed of a diffusion pump and a mechanical pump, or a molecular pump, and the ultimate vacuum can reach 8×10 ^-4 Pa. Circular arc targets are evenly distributed on the furnace wall in 6 points and four rows. The diameter of the circular arc targets is 60-100mm. There are magnets behind the circular arc targets, and there are 12-16 circular arc targets. The center of the vacuum chamber The part is a high-power rotating arc target 4, and a coil is arranged behind the high-power rotating arc target. The magnetic field is generated by electrifying the coil. 300A, the arc movement is controlled by the high-speed rotating magnet in the target. The circular arc target and the high-power rotating arc target are made of Cr, Zr or Ti. Multiple heaters 3 are installed on the furnace wall, which can easily adjust the temperature in the vacuum chamber. The space between the circular arc target 6 and the high-power rotary arc target 4 is the ion plating deposition area, the ion plating deposition area is an annular area, the workpiece rack 5 is distributed in the ion plating deposition area, and a driving mechanism is provided under the workpiece rack 5, As well as the autorotation turntable and the revolution turntable driven by the drive mechanism, the workpiece holder 5 is installed on the autorotation turntable, and the autorotation turntable is installed on the revolution turntable. The drive mechanism can be a gear transmission mechanism driven by a common DC motor. The speed of the gear transmission mechanism is adjusted by a frequency converter. The revolving large gear is driven by a DC motor, and the entire workpiece frame revolves. The self-rotating pinion gear meshes with the revolving gear, and the workpiece is driven by the revolving gear to rotate; the structure of the coating can be adjusted by adjusting the rotating speed, and the uniformity of the coating can be improved. The sample is installed on the workpiece frame 5, and revolves and rotates between the central cylindrical high-power rotating arc target 4 and the circular arc target 6 on the furnace wall. This layout greatly increases the plasma density in the vacuum chamber, and the workpiece is completely immersed in the plasma. The coating deposition rate, hardness and adhesion are greatly improved.

The specific examples of use of the fast hard ceramic coating ion plating device provided by the invention are as follows:

The experimental target is 99.95at.% high-purity Cr, Ti or Zr target; the coated samples are respectively hard alloy and CNC wire cutting machine and cut into 20mm×50mm×1mm stainless steel sheets, which are pre-grinded, polished and strictly cleaned After treatment, put it into the deposition system for CrN coating preparation. The substrate negative bias voltage is continuously adjustable from 0 to 1200V. The working gas is _N2 and Ar, controlled by mass flow meter. The substrate speed is adjustable.

Example 1: Under the condition of 0.5Pa and negative 150V bias, the metal Cr target arc discharge controlled by the magnetic field is used to prepare a pure Cr metal transition layer; then nitrogen gas is introduced, and the air pressure rises to 2.3Pa, and all arc targets and arc targets on the furnace wall are opened. The rotating target in the middle uses nitrogen gas to react with Cr evaporated from the target surface to form CrN. The nitrogen gas flow rate is 200-600 sccm; the current of a single circular arc target metal target on the furnace wall is 60-80A. The center rotating target current is 250-300A.

The magnetic field of the circular target on the furnace wall to control the movement of the arc is generated by a magnet placed behind the arc target. A uniformly distributed magnetic field with a strength of 50 Gauss is generated on the target surface.

The above-mentioned glow discharge cleaning is carried out at 350-400°C in an argon environment; after the glow cleaning is completed, the cathode arc discharge of the metal Cr target is carried out under the condition of 0.5Pa, and the deposition thickness of the metal transition layer is 100-200 nanometers; the CrN coating The layer thickness is 20-30 microns. The flow rate of nitrogen gas is 200-600 sccm, and that of argon gas is 10-50 sccm. The preparation temperature is 400-450°C, and the bias voltage is negative 150V.

Example 2: Under the condition of 0.5Pa and negative 200V bias, the metal Ti target arc discharge controlled by the magnetic field is used to prepare a pure Ti metal transition layer; The rotating target uses nitrogen gas to react with Ti evaporated from the target surface to form TiN. The nitrogen gas flow rate is 100-250 sccm; the current of a single circular arc target metal target on the furnace wall is 40-60A. The center rotating target current is 180-250A.

The magnetic field of the circular target on the furnace wall to control the movement of the arc is generated by a magnet placed behind the arc target. A uniformly distributed magnetic field with a strength of 50 Gauss is generated on the target surface.

The above-mentioned glow discharge cleaning is carried out at 350-400°C in an argon environment; after the glow cleaning is completed, the cathode arc discharge of the metal Ti target is carried out under the condition of 0.5Pa to deposit the metal Ti transition layer with a thickness of 100-200 nanometers; TiN Coating thickness is 15-20 microns. The flow rate of nitrogen gas is 100-200 sccm, and that of argon gas is 10-50 sccm. The preparation temperature is 400-450°C, and the bias voltage is negative 200V.

Example 3: Under the condition of 0.5Pa and negative 100V bias voltage, a metal Zr target arc discharge controlled by a magnetic field is used to prepare a pure Zr metal transition layer; then feed nitrogen, and the air pressure rises to 1.5Pa, and all arc targets and arcs on the furnace wall are opened. The rotating target in the middle uses nitrogen gas to react with Zr evaporated from the target surface to form ZrN. The nitrogen gas flow rate is 150-350 sccm; the current of a single circular arc target metal target on the furnace wall is 80-110A. The center rotating target current is 200-280A.

The magnetic field of the circular target on the furnace wall to control the movement of the arc is generated by a magnet placed behind the arc target. A uniformly distributed magnetic field with a strength of 50 Gauss is generated on the target surface.

The above-mentioned glow discharge cleaning is carried out at 350-400° C. under an argon atmosphere; after the glow cleaning is completed, metal Zr target cathode arc discharge is carried out under the condition of 0.5 Pa to deposit a metal Zr transition layer with a thickness of 100-200 nanometers; ZrN Coating thickness is 25-30 microns. The flow rate of nitrogen gas is 150-300 sccm, and that of argon gas is 10-50 sccm. The preparation temperature is 400-450°C, and the bias voltage is negative 200V.

Figure 2 shows the surface morphology of the CrN thick coating prepared by this device. It can be seen from the surface that there are certain holes and particles, which are the defects of the arc method itself.

Figure 3 and Figure 4 are scanning electron microscope pictures of the cross-sectional morphology of the coating prepared at a preparation time of 30 minutes and 60 minutes respectively. It can be seen from Figure 3 that a CrN coating with a thickness of about 5 microns can be deposited in 30 minutes. It can be seen from Figure 4 that after 120 minutes of deposition, a CrN coating of nearly 20 microns can be obtained. Reaching a growth rate of nearly 10 microns per hour can meet the requirements for rapid preparation of industrial ceramic coatings.

Claims (9)

1. quick solid-ceramic coating ion plating apparatus, at least comprise the vacuum chamber that surrounds by the furnace wall, vacuum chamber is provided with vacuum orifice, furnace wall one side is provided with fire door, it is characterized in that: the high-power rotating arc target that is provided with the control of circular electric arc target and magnetic field in the vacuum chamber, circular electric arc target is divided into the 2N row, N 〉=1, be evenly distributed on the furnace wall, high-power rotating arc target is positioned at the centre of vacuum chamber, space between circular electric arc target and the high-power rotating arc target is the ion-plating deposition district, and work rest is distributed in the ion-plating deposition district, and circular electric arc target is connected with power supply respectively with high-power rotating arc target.

2. quick solid-ceramic coating ion plating apparatus according to claim 1 is characterized in that: the back of circular electric arc target is provided with magnet, is provided with coil behind the high-power rotating arc target, and magnetic field is produced by coil electricity.

3. quick solid-ceramic coating ion plating apparatus according to claim 1 is characterized in that: circular electric arc target is divided into four row, is evenly distributed on the furnace wall, and the large power electric arc target is cylindricality, and its range of current is 150～300A.

4. quick ion film plating deposition apparatus according to claim 1 and 2 is characterized in that: circular electric arc target diameter is 60-100mm, is provided with 12-16 circular electric arc target, and circular electric arc target and high-power rotating arc target target are Cr, Zr or Ti.

5. quick ion film plating deposition apparatus according to claim 1 and 2 is characterized in that: the power supply of high-power rotating arc target is the high power contravariant intermediate frequency power supply.

6. quick solid-ceramic coating ion plating apparatus according to claim 1 and 2 is characterized in that: the vacuum chamber height is a 0.5-1.5 rice, and diameter is 700-900mm.

7. quick solid-ceramic coating ion plating apparatus according to claim 1 and 2 is characterized in that: all the ion-plating deposition district is an annular region.

8. quick solid-ceramic coating ion plating apparatus according to claim 1 and 2 is characterized in that: a plurality of well heaters are installed on the furnace wall.

9. quick solid-ceramic coating ion plating apparatus according to claim 1 and 2, it is characterized in that: the work rest below is provided with driving mechanism, and by the rotation rotating disk of drive mechanism and the rotating disk that revolves round the sun, work rest is installed on the rotation rotating disk, and the rotation rotating disk then is installed on the revolution rotating disk.

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