CN206580883U - A kind of diamond-like carbon film-coating Preparation equipment - Google Patents

Abstract

The utility model provides a diamond-like coating preparation equipment, comprising: a vacuum cavity, a heat tracing device, a diffuser, and a flow controller; wherein, one end of the flow controller is provided with an inlet pipe, and the other end is provided with a first outlet pipe, The first outlet pipe is connected to the diffuser; the diffuser is connected to the vacuum cavity through the second outlet pipe, and the heat tracing device is respectively arranged on the first outlet pipe and the second outlet pipe. Two outlet tubes. By adding a diffuser and a heat tracing device, the doping of the liquid precursor in the preparation process of the diamond-like coating is realized, thereby improving the thermal stability and reducing the internal stress of the film. Further, by setting the cleaning device, the substrate’s The cleaning link is integrated with the preparation of the diamond-like carbon coating, which further improves the efficiency of the preparation.

Description

A diamond-like coating preparation equipment

technical field

The utility model relates to a diamond-like coating manufacturing technology, in particular to a diamond-like coating preparation equipment.

Background technique

Diamond-like carbon (DLC) coatings have high hardness, high chemical stability, high thermal conductivity, low friction coefficient, good dielectric properties and excellent spectral characteristics. Machinery, medicine and other fields have been widely used.

In the prior art, plasma-enhanced chemical vapor deposition technology is mostly used to prepare DLC coatings. This technology has the characteristics of low deposition temperature, good winding, and good uniformity of film thickness deposited on large-area substrates. It is widely used in Preparation of DLC thin films.

However, using the existing technology, there are also many problems in practical applications: 1) the internal stress of the film is large, and the bonding force with the substrate is poor, which is prone to cracking and peeling of the film; 2) poor thermal stability .

Utility model content

The utility model provides a diamond-like coating preparation device, which is used for reducing the stress of the diamond-like coating and improving the thermal stability of the diamond-like coating.

The first aspect of the utility model provides a diamond-like coating preparation equipment, including: a vacuum cavity, a heat tracing device, a diffuser, a flow controller and a cleaning device;

Wherein, one end of the flow controller is provided with an inlet pipe, and the other end is provided with a first outlet pipe, and the first outlet pipe is connected to the diffuser; the diffuser is connected to the vacuum chamber through the second outlet pipe. Body conduction, the heat tracing device is respectively arranged on the first outlet pipe and the second outlet pipe;

The cleaning device includes a cleaning chamber, a carrier plate, a cleaning nozzle and a cleaning liquid storage tank;

Wherein, the cleaning chamber and the vacuum chamber are sealed and docked through the first port, and the cleaning nozzle is aligned with the carrier plate and connected to the cleaning liquid storage tank; the carrier plate is used to carry the substrate .

Preferably, the vacuum cavity is provided with two circular electrodes.

Preferably, the inside of the diffuser is provided with: a source bottle, a thermocouple and at least two radiation heating tubes;

The at least two radiant heating tubes are respectively connected to the thermocouples.

Preferably, the at least two radiant heating tubes are distributed around the source bottle.

Preferably, a first port and a second port are arranged on the first surface of the diffuser, the first port is used to connect with the first outlet pipe, and the second port is connected to the second outlet pipe connect.

Preferably, the thermocouple is arranged at the lower end of the first port and the second port.

Preferably, the heat tracing device is connected to the thermocouple.

Preferably, the first outlet pipe is provided with a first switch; the second outlet pipe is provided with a second switch.

Preferably, there are at least two diffusers.

Preferably, the cleaning device further includes: a drying module; the drying module includes: a dry gas injector and a dry gas storage tank;

Wherein, the dry gas injector is aimed at the carrier plate and connected to the dry gas storage tank.

The diamond-like coating preparation equipment provided in this embodiment realizes the doping of the liquid precursor in the preparation process of the diamond-like coating by adding a diffuser and a heat tracing device, thereby improving the thermal stability and reducing the internal stress of the film, further Specifically, by setting up a cleaning device, the cleaning of the substrate is integrated with the preparation of the diamond-like coating, which further improves the efficiency of the preparation.

Description of drawings

Fig. 1 is the structural representation of a kind of diamond-like coating preparation equipment provided by the utility model embodiment;

Fig. 2 is the structural representation of another diamond-like coating preparation equipment provided by the embodiment of the present invention;

Fig. 3 is the stress test schematic diagram of the diamond-like coating preparation equipment provided by the utility model;

Fig. 4 is the Raman spectrum schematic diagram of the sample at different temperatures of the diamond-like coating preparation equipment provided by the utility model;

5 is a schematic diagram of the relationship between the carrier gas flow and hardness of the diamond-like coating preparation equipment provided by the present invention;

6 is a schematic diagram of the DLC surface roughness under different carrier gas flow rates of the diamond-like coating preparation equipment provided by the present invention;

Fig. 7 is a schematic structural diagram of another diamond-like coating preparation equipment provided by the present invention.

detailed description

Fig. 1 is a schematic structural diagram of a diamond-like coating preparation equipment provided by an embodiment of the present invention. Referring to Fig. 1, the equipment includes: a vacuum cavity 10, a heat tracing device 11, a diffuser 12, a flow controller 13 and a cleaning device 14 ;

Wherein, one end of the flow controller 13 is provided with an inlet pipe 13a, and the other end is provided with a first outlet pipe 13b, and the first outlet pipe 13b is in communication with the diffuser 12; The pipe 12a communicates with the vacuum cavity 10, and the heat tracing device 11 is respectively arranged on the first outlet pipe 13b and the second outlet pipe 12a.

The cleaning device includes a cleaning chamber 14-1, a carrier plate 14-2, a cleaning nozzle 14-3 and a cleaning liquid storage tank 14-4;

Wherein, the cleaning chamber 14-1 is sealed and docked with the vacuum chamber 10 through the first port 14-5, and the cleaning nozzle 14-3 is aligned with the carrier plate 14-2, and the cleaning liquid The storage tank 14-4 is connected; the carrier tray 14-2 is used to carry the substrate.

Specifically, the substrate is ultrasonically cleaned for 15 minutes in a cleaning solution composed of alcohol and acetone.

The diamond-like coating preparation equipment provided in this embodiment realizes the doping of the liquid precursor in the preparation process of the diamond-like coating by adding a diffuser and a heat tracing device, thereby improving the thermal stability and reducing the internal stress of the film, further Specifically, by setting up a cleaning device, the cleaning of the substrate is integrated with the preparation of the diamond-like coating, which further improves the efficiency of the preparation.

Specifically, a sliding track may be provided between the vacuum chamber 10 and the cleaning chamber 14-1 for connecting the carrying tray 14-2 so that the connecting tray 14-2 can slide from the cleaning chamber 14-1 to Vacuum cavity 10; then slide from the vacuum cavity 10 to the cleaning cavity 14-1. The sliding track passes through the above-mentioned first port 14-15.

On the basis of Fig. 1, Fig. 2 is a schematic structural diagram of another diamond-like coating preparation equipment provided by the embodiment of the present invention, referring to Fig. 2, wherein the vacuum cavity 10 is provided with two circular electrodes 10-1 .

The inside of the diffuser 12 is provided with: a source bottle 12-1, a thermocouple 12-2 and at least two radiation heating tubes 12-3;

Specifically, the source bottle 12-1 is filled with a liquid reactant, and the thermocouple 12-2 is in contact with the surface of the source bottle 12-1.

The at least two radiant heating tubes 12-3 are respectively connected to the thermocouples 12-2.

Specifically, the thermocouple 12-2 obtains the temperature data of the source bottle 12-1, and this embodiment may further include a processor for controlling the at least two radiation heating tubes 12-1 according to the temperature data obtained by the thermocouple 12-2. 3 heating temperature.

The at least two radiant heating tubes 12-3 are distributed around the source bottle 12-1.

A first port and a second port are arranged on the first surface of the diffuser, the first port is used for connecting with the first outlet pipe, and the second port is connected with the second outlet pipe.

The thermocouple is arranged at the lower end of the first port and the second port.

The heat tracing device 11 is connected to the thermocouple 12-2.

Specifically, a thermocouple 12-2 is arranged between the source bottles 12-1 and 12-3. In addition, a thermocouple can also be set between the first lead-out pipe 13b and the heat tracing device 11 to obtain the temperature data of the first lead-out pipe 13b; Thermocouples, used to obtain the temperature data of the second outlet pipe 12a;

Specifically, the heat tracing device 11 is wound around the pipeline for heating the first outlet pipe 13b and the second outlet pipe 12a, and a thermocouple 12-2 is usually used to detect the first outlet pipe 13b and the temperature of the second outlet pipe 12a.

The first outlet pipe is provided with a first switch a; the second outlet pipe is provided with a second switch b.

There are at least two diffusers 12 .

Further, the equipment is equipped with RF source, vacuum system, gas control system and tail gas treatment system. The frequency of the RF source is 13.56MHz, and the gas control system is equipped with 8 flow controllers (MFC). For this device, the reactants or reaction precursors are usually gases, and for silicon doping, the gaseous precursor silane should be selected under normal conditions, which is easier to achieve the doping reaction, but silane is flammable and explosive at room temperature , artificially difficult to control. Therefore, the liquid precursor tetramethylsilane (TMS) is selected, but it is difficult to realize the liquid substance entering the vacuum chamber to participate in the reaction by using the gas control system. In order to achieve the doping of liquid precursors, this embodiment adds at least two diffusers, and the inside and outside of the diffuser are equipped with a temperature control system. Specifically, the temperature control system consists of the above thermocouple, at least two radiation heating tubes As well as the heat tracing device, the two added diffusers are connected to the MFC, so that the carrier gas can be used to bring the heated reaction precursor into the vacuum chamber to participate in the doping reaction. The example uses argon (Ar) as the carrier gas, n-butane (C4H10) as the reaction gas, and tetramethylsilane (TMS) as the reaction precursor. The Si substrate was ultrasonically cleaned in a mixture of alcohol and acetone for 15 minutes, dried with nitrogen and placed in a vacuum chamber.

Fig. 3 is the stress test schematic diagram of the diamond-like coating preparation equipment that the utility model provides, and the test result of stress is as shown in Fig. 3, can find out from the figure, along with the increase of the flow rate of carrier gas, the stress of film layer is decreasing small. This is because as the flow rate of the carrier gas increases, the content of TMS participating in the reaction increases, so that the content of Si in the film layer increases, and the doped Si atoms replace the C atoms and enter the lattice of the DLC film. The radius is large and the electronegativity is small, so it is not easy to generate sp2 bonds, but combines with C to form sp3 bonds. Therefore, doping Si in DLC can increase the content of SP3 bonds in DLC films, thereby increasing the ratio of sp3/sp2 in DLC films. However, the bond energy of C-Si (3.12ev) is less than that of C-C (3.61ev), so the surrounding carbon bond distortion of the DLC film becomes relaxed after Si doping, thereby reducing the internal stress of the DLC film. In addition, in the Si-doped DLC thin film, since Si exists in sp3 structure, when Si enters the film layer, the free hydrogen content in the film layer is reduced, thereby reducing the internal stress of the film layer.

This experiment uses the following method to test the thermal stability of Si-doped DLC thin films. The prepared samples are subjected to high-temperature annealing treatment, and the processed samples are subjected to Raman spectrum testing. Through the changes in the spectral curves, the thickness of the film layer can be obtained. thermal stability. Figure 3 shows the Raman spectra of the samples after annealing at different temperatures under the condition of a carrier gas flow rate of 5 sccm, and the graphitization temperature ranges under other carrier gas flow rates are shown in Table 1.

Table 1 - Sample graphitization temperature at different carrier gas flow rates

carrier Graphitization temperature (°C) 5 400～450 10 460～480 15 500～530 20 540～570 25 580～600 30 600～630

Fig. 4 is the Raman spectrum schematic diagram of the sample under the different temperatures of the diamond-like coating preparation equipment that the utility model provides, as can be seen from Fig. 4, for the DLC film that generates under the condition of 5 sccm for the carrier gas flow rate, when the temperature reaches 400～ Between 450°C, the film begins to graphitize. When the temperature is further increased, the graphitization of the film layer is intensified; the remaining graphitization temperature ranges are shown in Table 1. For the DLC film formed under the condition of carrier gas flow rate of 30 sccm, the graphitization temperature reaches above 600°C. It shows that with the increase of doped Si content in the film layer, the graphitization temperature of DLC film increases, indicating that the thermal stability of the film layer is improved. This is because the presence of Si increases the stability of the sp3 bond in the film layer, improves the disordered state of the amorphous carbon-based film, and increases the potential barrier of the metastable state, so higher energy is required to cross the barrier to form The stable graphite structure requires a high temperature to graphitize. In addition, the more Si content in the film layer, the lower the free hydrogen content in the film layer. Therefore, it is more difficult to resolve and release hydrogen in the film layer, which further increases the energy required for graphitization. Therefore, the higher the Si content in the film layer, the higher the thermal stability of the film.

Fig. 5 is a schematic diagram of the relationship between the carrier gas flow rate and the hardness of the diamond-like coating preparation equipment provided by the present invention. The hardness test results are shown in Fig. 5, and it can be seen from Fig. 5 that as the carrier gas flow rate increases, the hardness of the film layer decreases. It can be seen from Figure 5 that when the carrier gas flow rate is 0-5 sccm, the hardness of the film layer decreases slowly, and when it changes between 5-25 sccm, the hardness decreases rapidly, and when it changes between 25-30 sccm, the hardness decreases again. become slower. Since silicon atoms combine with C to form sp3 bonds, the content of sp3 bonds in the DLC film is increased, thereby increasing the ratio of sp3/sp2 in the DLC film. But the bond energy of C-Si is smaller than that of C-C, so the hardness of the film decreases. When the carrier gas flow rate is 0-5 sccm, the doped reactants are less, and the content of C-Si formed is less, so the hardness of the film layer decreases slowly, and when it changes between 5-25 sccm, with the doping With the increase of gas, the content of C-Si in the film layer increases rapidly, so the hardness decreases rapidly, and when it changes between 25-30sccm, due to the high content of doping gas, part of the doping gas may be The vacuum pump is taken away, and the hardness drop becomes slower again.

Figure 6 is a schematic diagram of the DLC surface roughness under different carrier gas flow rates of the diamond-like coating preparation equipment provided by the utility model, with reference to Figure 6, in order to determine the influence of the doping amount of Si on the surface morphology of the sample, AFM is carried out on the sample According to the test results in Figure 5, it can be seen that as the Si content in the film layer increases, the surface roughness of the film layer decreases gradually. This is due to the doping of Si, which leads to a great change in the ratio of sp3 and sp2 bonds in the DLC film. The existence of Si greatly limits the formation of sp2 bond structure, thereby inhibiting the rapid growth of sp2 graphite clusters and improving the surface finish of the film.

Further, on the basis of FIG. 1, FIG. 7 is a schematic structural diagram of another diamond-like coating preparation equipment provided by the present invention. Referring to FIG. 7, the diamond coating preparation equipment also includes: the drying module, specifically, the The drying module includes: a dry gas injector 14-6 and a dry gas storage tank 14-7;

Specifically, the dry gas injector 14-6 is aimed at the carrier plate 14-2, and is connected to the dry gas storage tank 14-7.

Wherein, the drying gas may be nitrogen, and nitrogen is used to dry the substrate carried on the carrier plate 14 - 2 , and then the substrate is placed in the vacuum chamber 10 .

Preferably, the drying module may also include a drying gas collecting device or a vacuum pump, for collecting the drying gas or sucking the drying gas away through the vacuum pump.

Optionally, in order to realize the sealing function of the first port 14-5, a possible implementation method: a sealing partition 15 is provided at the first port 14-5, and when the sealing partition 15 is in a closed state, the first port is realized 14-5 sealing; when the sealing partition 15 is in an open state, then carry out the movement of the carrying tray 14-2.

Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present utility model, and are not intended to limit it; although the present utility model has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand : It is still possible to modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements to some or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions depart from the various embodiments of the present invention Scope of technical solutions.

Claims (10)

1. a kind of diamond-like carbon film-coating Preparation equipment, it is characterised in that including：Vacuum cavity, heating device, diffuser, flow Controller and cleaning device；

Wherein, described flow controller one end is provided with ingress pipe, and the other end is provided with the first delivery line, first delivery line and institute State diffuser conducting；The diffuser is turned on by the second delivery line and the vacuum cavity, and the heating device is set respectively In on first delivery line and second delivery line；

The cleaning device includes cleaning chamber, carrier, cleaning sprayer and cleaning fluid storage tank；

Wherein, the cleaning chamber is docked with the vacuum cavity by first port sealing, and the cleaning sprayer alignment is described Carrier, and in cleaning fluid storage tank connection；The carrier is used for carrying substrates.

2. diamond-like carbon film-coating Preparation equipment according to claim 1, it is characterised in that the vacuum cavity is provided with two Individual circular electrode.

3. diamond-like carbon film-coating Preparation equipment according to claim 1, it is characterised in that the diffuser inside is set Have：Source bottle, thermocouple and at least two radiant heaters；

At least two radiant heater is connected respectively at the thermocouple.

4. diamond-like carbon film-coating Preparation equipment according to claim 3, it is characterised in that at least two radiation heating Pipe is distributed in around the source bottle.

5. diamond-like carbon film-coating Preparation equipment according to claim 3, it is characterised in that first port is set with second port The first face of the diffuser is placed in, the first port is used to be connected with first delivery line, the second port and institute State the connection of the second delivery line.

6. diamond-like carbon film-coating Preparation equipment according to claim 5, it is characterised in that the thermocouple is arranged at described The lower end of first port and the second port.

7. diamond-like carbon film-coating Preparation equipment according to claim 3, it is characterised in that the heating device and the heat Galvanic couple is connected.

8. diamond-like carbon film-coating Preparation equipment according to claim 1, it is characterised in that first delivery line is provided with First switch；Second delivery line is provided with second switch.

9. diamond-like carbon film-coating Preparation equipment according to claim 1, it is characterised in that the diffuser is at least two It is individual.

10. diamond-like carbon film-coating Preparation equipment according to claim 1, it is characterised in that the cleaning device also includes： Irradiation modules；

The irradiation modules, including：Dry gas injector and dry gas storage tank；

Wherein, dry gas injector is directed at the carrier, and in dry gas storage tank connection.