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

A kind of diamond-like carbon film-coating Preparation equipment Download PDF

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Publication number
CN206580883U
CN206580883U CN201720039885.5U CN201720039885U CN206580883U CN 206580883 U CN206580883 U CN 206580883U CN 201720039885 U CN201720039885 U CN 201720039885U CN 206580883 U CN206580883 U CN 206580883U
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China
Prior art keywords
diamond
carbon film
delivery line
preparation equipment
coating preparation
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Expired - Fee Related
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CN201720039885.5U
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Chinese (zh)
Inventor
杨永亮
李娜
岳莉
张泓筠
黄庆新
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Kaili University
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Kaili University
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Abstract

The utility model provides a kind of diamond-like carbon film-coating Preparation equipment, including:Vacuum cavity, heating device, diffuser, flow controller;Wherein, described flow controller one end is provided with ingress pipe, and the other end is provided with the first delivery line, and first delivery line is turned on the diffuser;The diffuser is turned on by the second delivery line and the vacuum cavity, and the heating device is respectively arranged on first delivery line and second delivery line.By increasing diffuser and heating device, realize the doping of liquid precursor in diamond-like carbon film-coating preparation process, so as to improve heat endurance, reduce the internal stress of film, further, by setting cleaning device, the cleaning link of substrate is prepared with diamond-like carbon film-coating and combined, the efficiency of preparation is further increased.

Description

A kind of diamond-like carbon film-coating Preparation equipment
Technical field
The utility model is related to diamond-like carbon film-coating manufacturing technology, more particularly to a kind of diamond-like carbon film-coating Preparation equipment.
Background technology
DLC (Diamond-like carbon, abbreviation DLC) plated film have high hardness, high chemical stability, High thermal conductivity factor, low coefficient of friction, preferable dielectric properties and excellent spectral characteristic, optics, electricity, machinery, The fields such as medical science are widely used.
In the prior art, many to prepare DLC plated films using PECVD, the technology has deposition The characteristics of film thickness uniformity that temperature is low, winding degree is good and is deposited on extensive substrate is good, is widely used in DLC The preparation of film.
But, using existing technology, there is also problems in actual applications:1) internal stress of film is big, with base Piece and adhesion is poor, be also easy to produce film peeling and peeling;2) poor heat endurance.
Utility model content
The utility model provides a kind of diamond-like carbon film-coating Preparation equipment, for reduce diamond-like carbon film-coating stress and Improve the heat endurance of diamond-like carbon film-coating.
One side of the present utility model provides a kind of diamond-like carbon film-coating Preparation equipment, including:Vacuum cavity, heat tracing 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 Turned on the diffuser;The diffuser is turned on by the second delivery line and the vacuum cavity, the heating device difference It is arranged 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, the cleaning sprayer alignment The carrier, and in cleaning fluid storage tank connection;The carrier is used for carrying substrates.
It is preferred that the vacuum cavity is provided with two circular electrodes.
It is preferred that the diffuser inside is provided with:Source bottle, thermocouple and at least two radiant heaters;
At least two radiant heater is connected respectively at the thermocouple.
It is preferred that at least two radiant heater is distributed in around the source bottle.
It is preferred that first port and second port are arranged at the first face of the diffuser, the first port be used for The first delivery line connection, the second port is connected with second delivery line.
It is preferred that the thermocouple is arranged at the lower end of the first port and the second port.
It is preferred that the heating device is connected with the thermocouple.
It is preferred that first delivery line is provided with first switch;Second delivery line is provided with second switch.
It is preferred that the diffuser at least two.
It is preferred 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.
The diamond-like carbon film-coating Preparation equipment that the present embodiment is provided, by increasing diffuser and heating device, realizes class The doping of liquid precursor in diamond coated preparation process processed, so as to improve heat endurance, reduces the internal stress of film, Further, by setting cleaning device, the cleaning link of substrate is prepared with diamond-like carbon film-coating and combined, further Improve the efficiency of preparation.
Brief description of the drawings
A kind of structural representation for diamond-like carbon film-coating Preparation equipment that Fig. 1 provides for the utility model embodiment;
The structural representation for another diamond-like carbon film-coating Preparation equipment that Fig. 2 provides for the utility model embodiment;
The stress test schematic diagram for the diamond-like carbon film-coating Preparation equipment that Fig. 3 provides for the utility model;
The Raman spectrum of sample shows under the different temperatures for the diamond-like carbon film-coating Preparation equipment that Fig. 4 provides for the utility model It is intended to;
The carrier gas flow of diamond-like carbon film-coating Preparation equipment and the relation of hardness that Fig. 5 provides for the utility model are shown It is intended to;
DLC tables under the different carrier gas flows for the diamond-like carbon film-coating Preparation equipment that Fig. 6 provides for the utility model The schematic diagram of surface roughness;
The structural representation for another diamond-like carbon film-coating Preparation equipment that Fig. 7 provides for the utility model.
Embodiment
A kind of structural representation for diamond-like carbon film-coating Preparation equipment that Fig. 1 provides for the utility model embodiment, reference Fig. 1, the equipment includes:Vacuum cavity 10, heating device 11, diffuser 12, flow controller 13 and cleaning device 14;
Wherein, described one end of flow controller 13 is provided with ingress pipe 13a, and the other end is described provided with the first delivery line 13b First delivery line 13b is turned on the diffuser 12;The diffuser 12 passes through the second delivery line 12a and the vacuum cavity 10 Conducting, the heating device 11 is respectively arranged on the first delivery line 13b and the second delivery line 12a.
The cleaning device includes cleaning chamber 14-1, carrier 14-2, cleaning sprayer 14-3 and cleaning fluid storage tank 14-4;
Wherein, the cleaning chamber 14-1 is docked with the vacuum cavity 10 by first port 14-5 sealings, described clear Wash shower nozzle 14-3 and be directed at the carrier 14-2, and in the cleaning fluid storage tank 14-4 connections;The carrier 14-2 is used for Carrying substrates.
Cleaned 15 minutes specifically, substrate carries out ultrasonic wave in the cleaning fluid that alcohol and acetone are constituted.
The diamond-like carbon film-coating Preparation equipment that the present embodiment is provided, by increasing diffuser and heating device, realizes class The doping of liquid precursor in diamond coated preparation process processed, so as to improve heat endurance, reduces the internal stress of film, Further, by setting cleaning device, the cleaning link of substrate is prepared with diamond-like carbon film-coating and combined, further Improve the efficiency of preparation.
Specifically, a sliding rail can be set between vacuum cavity 10 and cleaning chamber 14-1, for connecting carrier 14-2 so that this meets carrier 14-2 can slide into vacuum cavity 10 from cleaning chamber 14-1;Slided again by vacuum cavity 10 Move to cleaning chamber 14-1.The sliding rail passes through above-mentioned first port 14-15.
On the basis of Fig. 1, another diamond-like carbon film-coating Preparation equipment that Fig. 2 provides for the utility model embodiment Structural representation, reference picture 2, wherein, the vacuum cavity 10 is provided with two circular electrode 10-1.
The diffuser 12 is internally provided with:Source bottle 12-1, thermocouple 12-2 and at least two radiant heater 12-3;
Specifically, source bottle 12-1 dress liquid reactants, and thermocouple 12-2 is contacted with source bottle 12-1 surfaces.
At least two radiant heaters 12-3 is respectively at the thermocouple 12-2 connections.
Specifically, thermocouple 12-2 obtains source bottle 12-1 temperature data, the present embodiment can also include processor, be used for The temperature data obtained according to thermocouple 12-2 controls the heating-up temperature of at least two radiant heaters 12- 3.
At least two radiant heaters 12-3 is distributed in around the source bottle 12-1.
First port is arranged at the first face of the diffuser with second port, and the first port is used for and described first Delivery line is connected, and the second port is connected with second delivery line.
The thermocouple is arranged at the lower end of the first port and the second port.
The heating device 11 is connected with the thermocouple 12-2.
Specifically, being provided with thermocouple 12-2 between the bottle 12-1 and 12-3 of source.In addition, the first delivery line 13b with Thermocouple can also be set between heating device 11, the temperature data for obtaining the first delivery line 13b;Second delivery line 12a Thermocouple can also be set between heating device 11, the temperature data for obtaining the second delivery line 12a;
Specifically, heating device 11 is wound on around pipeline, for for the first delivery line 13b and second delivery line 12a is heated, and usual thermocouple 12-2 is used for detecting the first delivery line 13b and the second delivery line 12a temperature.
First delivery line is provided with first switch a;Second delivery line is provided with second switch b.
The diffuser 12 at least two.
Further, the equipment is equipped with RF sources, vacuum system, gas control system and exhaust treatment system.Wherein RF The frequency in source is 13.56MHz, and gas control system is equipped with 8 flow controllers (MFC).For the equipment, reactant or reaction Predecessor is generally all gas, and for silicon doping, gaseous precursors silane should be selected under normal condition, it is easier to real Existing doping reaction, but silane is inflammable at normal temperatures, explosive, and artificial is difficult control.So the predecessor tetramethyl of selection liquid Silane (TMS), but liquid is difficult to realize into vacuum chamber participation reaction using gas control system.In order to realize before liquid The doping of thing is driven, embodiment adds at least two diffusers, the inside and outside of diffuser is furnished with temperature control system, tool The temperature control system of body is made up of thermocouple above, at least two radiant heaters and heating device, two of addition Diffuser is connected with MFC, thus can using deliver gas by the pre-reaction material after heat bring into vacuum chamber participate in adulterate Reaction.Example is that delivery gas, normal butane (C4H10) be that reacting gas, tetramethylsilane (TMS) are before reacting with argon gas (Ar) Drive thing.Si substrates carry out ultrasonic wave in the mixed liquor of alcohol and acetone and cleaned 15 minutes, and are put into vacuum after being dried up with nitrogen Room.
The stress test schematic diagram for the diamond-like carbon film-coating Preparation equipment that Fig. 3 provides for the utility model, the test of stress As a result as shown in figure 3, it can be seen that the increase of the flow with delivery gas, the stress of film layer is reducing.This be because With the increase of carrier gas flow, to participate in the TMS of reaction content increase so that Si content increase, doping in film layer Si atoms instead of C atoms and enter in the lattice of DLC film, because the radius of silicon atom is larger and electronegativity is smaller, institute To be difficult to generate sp2 keys, but sp3 keys are combined into C.Therefore the Si that adulterated in DLC can increase SP3 keys in DLC film Content, so as to improve the ratio of sp3/sp2 in DLC film.But C-Si (3.12ev) bond energy is less than C-C (3.61ev) key Can, thus DLC film mix after Si around the distortion of carbon key relaxed, so as to reduce the internal stress of DLC film.In addition, Si In DLC film of adulterating, because Si exists with sp3 structures, therefore when Si enters film layer, reduce the free hydrogen content in film layer, So as to reduce the internal stress of film layer.
Test of this experiment to the heat endurance of Si doping DLC films uses following method, and the sample of preparation is carried out The high temperature anneal, carries out Raman spectrum tests by the sample after processing, by the change of the curve of spectrum, can obtain film layer Heat endurance.Carrier gas flow is given in Fig. 3 under the conditions of 5sccm, sample is carried out after different temperatures annealing Graphitization temperature scope under Raman spectrum, remaining carrier gas flow is as shown in table 1.
Sample graphitization temperature under table 1- difference carrier gas flows
carrier Graphitization temperature (DEG C)
5 400~450
10 460~480
15 500~530
20 540~570
25 580~600
30 600~630
The Raman spectrum of sample shows under the different temperatures for the diamond-like carbon film-coating Preparation equipment that Fig. 4 provides for the utility model It is intended to, figure 4, it is seen that be the DLC film that generates under the conditions of 5sccm for carrier gas flow, 400 are reached when temperature~ When between 450 DEG C, film starts graphitization.When temperature is further raised, the aggravation of film layer graphitization;Remaining graphitization temperature scope As shown in table 1.Be the DLC film that generates under the conditions of 30sccm for carrier gas flow, graphitization temperature reach 600 DEG C with On.Show the increase of the content with the Si that adulterated in film layer, DLC film graphitization temperature is improved, and shows the heat endurance of film layer Improve.Because Si presence increases the stability of sp3 keys in film layer, the unordered shape of amorphous carbon-base film is improved State, adds metastable potential barrier, it is therefore desirable to which higher energy can just cross the graphite-structure of potential barrier formation stable state, so Need high temperature could graphitization.The content of Si in other film layer is more, and the content of the free hydrogen in film layer is lower, because This, to discharge hydrogen more difficult for parsing in film layer so that the energy that graphitization needs further is improved.So Si contents are got in film layer Height, the heat endurance of film is higher.
The carrier gas flow of diamond-like carbon film-coating Preparation equipment and the relation of hardness that Fig. 5 provides for the utility model are shown It is intended to, hardness test result is as shown in figure 5, as shown in Figure 5 with the increase of carrier gas flow, the hardness of film layer is reduced.By Fig. 5 understands that carrier gas flow is in 0-5sccm, and the hardness decline of film layer is slower, and when changing between 5-25sccm, firmly Quickly, hardness declines and becomes slower the decrease speed of degree when changing between 25-30sccm.Because silicon atom is combined into C Sp3 keys, add the content of sp3 keys in DLC films, so as to improve the ratio of sp3/sp2 in DLC film.But C-Si bond energys are small In C-C bond energy, so the hardness reduction of film.Carrier gas flow is in 0-5sccm, and the reactant of doping is less, is formed C-Si content it is less, therefore film layer hardness decline it is slower, and when changing between 5- 25sccm, with impurity gas Increase, C-Si content soon increases in film layer, so the decrease speed of hardness is quickly, and in 25-30sccm anaplasia During change, because the content of impurity gas is higher, possible part impurity gas is taken away by vavuum pump, and hardness declines becomes slower again.
DLC tables under the different carrier gas flows for the diamond-like carbon film-coating Preparation equipment that Fig. 6 provides for the utility model The schematic diagram of surface roughness, reference picture 6, to determine Si influence of the doping for sample surface morphology, AFM is carried out to sample Test, from Fig. 5 results:With the increase of Si contents in film layer, the surface roughness of film layer is gradually reduced.This is due to Si Doping, cause the ratio of the sp3 and sp2 keys in DLC film to generate very big change, Si presence greatly limit sp2 The formation of bond structure, so as to inhibit the fast-growth of sp2 graphite clusters, improves the surface smoothness of film layer.
Further, on the basis of Fig. 1, Fig. 7 is prepared for another diamond-like carbon film-coating that the utility model is provided and set Standby structural representation, reference picture 7, diamond coated Preparation equipment also includes:The irradiation modules, specifically, described dry Dry module includes:Dry gas injector 14-6 and dry gas storage tank 14-7;
Specifically, dry gas injector 14-6 is directed at the carrier 14-2, and in the dry gas storage tank 14- 7 connections.
Wherein, dry gas can be nitrogen, and the substrate for being carried on carrier 14-2 is dried up with nitrogen, afterwards will In substrate setting and vacuum cavity 10.
Preferably, the irradiation modules can also include dry gas collection device or vavuum pump, for dry gas to be entered Row collect or, dry gas is taken away by vavuum pump.
Optionally, in order to realize first port 14-5 sealing function, a kind of possible implementation:In first port 14-5 sets sealing dividing plate 15, when sealing dividing plate 15 is closed, realizes first port 14-5 sealing;When sealing every When plate 15 is in open mode, then carrier 14-2 movement is carried out.
Finally it should be noted that:Various embodiments above is only limited to illustrate the technical solution of the utility model, rather than to it System;Although the utility model is described in detail with reference to foregoing embodiments, one of ordinary skill in the art should Understand:It can still modify to the technical scheme described in foregoing embodiments, or to which part or whole Technical characteristic carries out equivalent substitution;And these modifications or replacement, the essence of appropriate technical solution is departed from this practicality newly The scope of each embodiment technical scheme of type.

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.
CN201720039885.5U 2017-01-13 2017-01-13 A kind of diamond-like carbon film-coating Preparation equipment Expired - Fee Related CN206580883U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110846616A (en) * 2019-12-18 2020-02-28 杨永亮 Hood simulation piece for hard film deposition and adjusting device thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110846616A (en) * 2019-12-18 2020-02-28 杨永亮 Hood simulation piece for hard film deposition and adjusting device thereof
CN110846616B (en) * 2019-12-18 2024-02-23 皖西学院 Head cover simulation piece for hard film deposition and adjusting device thereof

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Granted publication date: 20171024

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