CN106498367A - A kind of compact type vacuum reaction unit for chemical vapor deposition diamond film - Google Patents

A kind of compact type vacuum reaction unit for chemical vapor deposition diamond film Download PDF

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Publication number
CN106498367A
CN106498367A CN201610920789.1A CN201610920789A CN106498367A CN 106498367 A CN106498367 A CN 106498367A CN 201610920789 A CN201610920789 A CN 201610920789A CN 106498367 A CN106498367 A CN 106498367A
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China
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cold water
groove
lid
housing
annular
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CN201610920789.1A
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CN106498367B (en
Inventor
白清顺
王永旭
赵航
余天凯
杜云龙
张庆春
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Harbin Institute of Technology
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Harbin Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45563Gas nozzles
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
    • C23C16/27Diamond only
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4412Details relating to the exhausts, e.g. pumps, filters, scrubbers, particle traps

Abstract

A kind of compact type vacuum reaction unit for chemical vapor deposition diamond film.Belong to the chemical vapour deposition technique field of diamond thin.In order to solve deposition problems of the cvd diamond film on micro- cutter under vacuum condition.Housing upper and lower side connects and composes reative cell with upper lid and bottom seat removable seal respectively, vacuum meter is fixed on lid, the test side of vacuum meter closely penetrates lid and is arranged in housing, the pipeline communicated with housing cavity is fixed with upper lid, needle-valve is fixed on the pipeline of lid, needle-valve is communicated with pipeline, observation window one is fixed with the peep hole one of upper lid, upper lid is provided with multiple cold water annular grooves, an observation window two is respectively fixed with two peep holes two on the side wall of housing, magnetic valve is fixed on the air inlet position of base, wireway one end is connected to inlet box, the other end is communicated with reative cell, air guide valve is installed on wireway, objective table is arranged on reaction interior and is fixed on base.Present invention is mainly used for the micro- tool surface deposition of diamond thin films of deposition cell.

Description

A kind of compact type vacuum reaction unit for chemical vapor deposition diamond film
Technical field
The present invention relates to a kind of vacuum reaction device for chemical vapor deposition diamond film, belongs to diamond thin Chemical vapour deposition technique field.
Background technology
Chemical vapor deposition (CVD) diamond thin is the chemical reaction using methane under the high temperature conditions with hydrogen, leads to Control reaction condition is crossed, in the deposition process that Grown goes out one layer of fine and close diamond thin.During the course of the reaction, can be with Adjust the series of parameters such as hot-wire temperature, the ratio of source of the gas and concentration to improve the quality of the diamond thin for obtaining.Due to this Participation in vapor deposition processes without catalyst, so diamond its heat endurance for generating is closer to natural diamond. Cvd diamond film also has the advantages such as strong, the good, good economy performance of wearability of impact resistance.At present, cvd diamond film is sunk Product can form the cutter coat that low, wear-resistant coefficient of friction, shock resistance, complex-shaped, chip are difficult bonding to tool surface. With the continuous development of modern science and technology, the application of microminaturization technology has more and more wide prospect.Traditional micro- knife Tool typically using high-speed steel or Hardmetal materials etc., as working speed of micro- cutter in milling is very high, can reach Tens of thousands of or even ten tens of thousands of rpms, therefore traditional micro- cutter typically exhibit wear no resistance, cutter life is short, crudy The defects such as difference.The important channel that coating rubbing-layer is the solution problem is applied in micro- tool surface.
CVD film micro cutter of diamond technology is the focus of current micro processing field research.Micro- in cvd diamond film In the preparation process of cutter, for the chemical gas-phase deposition system of the micro- cutter of diamond coatings has many key technologies to need to dash forward Broken, commercialization shaped article at home also without independent intellectual property right comes out at present, so as to cause the micro- knife of cvd diamond film The cost of tool remains high.The vacuum reaction chamber of chemical vapor deposition diamond film is the core apparatus of the system.At present, state The chemical vapor deposition vacuum reaction chamber that can be found in inside and outside document has that installing space is huge, waste of material degree The defects such as the indoor vacuum of high, reaction is difficult to ensure that, processing technology complexity, cooling effect difference, and for similar micro- cutter so Milli machine part can not realize the deposition of diamond thin films of its complex surface.Meanwhile, vacuum reaction chamber requires which has knot again Structure is compact, complete function, be easily installed the basic characteristics such as debugging, good reliability.Thus, develop the side using chemical vapor deposition Method realizes the vacuum reaction chamber of micro- tool surface deposition of diamond thin films device, with urgent and necessity.
Content of the invention
The invention aims to solving deposition problems of the cvd diamond film on micro- cutter under vacuum condition, enter And a kind of compact type vacuum reaction unit for chemical vapor deposition diamond film is provided.
Provided by the present invention for the compact type vacuum reaction unit of chemical vapor deposition diamond film, with vacuum The good, advantage of compact conformation, good cooling results.In chemical vapor deposition processes, reaction room pressure can be controlled in the present invention Near 1Pa, water inlet flow velocity is 0.3m/s, and the gas vent flow velocity of wireway is 0.06m/s.
Above-mentioned purpose is realized, the technical scheme that the present invention takes is as follows:
A kind of compact type vacuum reaction unit for chemical vapor deposition diamond film, its constitute include vacuum meter, Needle-valve, upper lid, housing, base, magnetic valve, infrared radiation thermometer, wireway, air guide valve, objective table and three observation windows;Described Three observation windows be observation window one and two observation windows two respectively;
Described housing top and bottom are connected with upper lid and bottom seat removable seal respectively, by housing, upper lid and bottom seat Combination constitutes reative cell, and described vacuum meter is fixed on cap upper surface, and the test side of described vacuum meter closely penetrates lid On through hole be arranged in housing, be fixed with the pipeline communicated with housing cavity on described upper lid, described needle-valve is fixed on On the pipeline of upper lid, needle-valve is communicated with pipeline, is provided with peep hole one, is provided with observation window at described peep hole one on upper lid One, described observation window one is fixed on cap upper surface, and upper lid is provided with multiple cold water annular grooves, and upper lid is provided with gas port one;
Two peep holes two are provided with the side wall of housing, are provided with an observation window at the peep hole two described in each Two, two described observation windows two are fixed on the lateral wall of housing, and described infrared radiation thermometer is close to one of observation window Two are arranged, and base is provided with gas port two, and described magnetic valve is fixed at the gas port two of base, and magnetic valve one end passes through bottom Gas port two on seat is communicated with reative cell, and the magnetic valve other end is connected with vavuum pump;
Described wireway one end is connected to inlet box, and the wireway other end closely penetrates the gas port one that lid is provided with Lead to into reative cell, air guide valve is installed on wireway, described air guide valve is arranged on the outside of reative cell, described loading Platform is arranged on reaction interior and is fixed on base.
The present invention relative to the beneficial effect of prior art is:
The characteristics of reative cell of the vacuum reaction device of the present invention has compact conformation, air-tightness good;Upper lid with housing it Between and housing and base between the structure that is engaged with annular spacing groove using bulge loop, it is ensured that the indoor each several part of reaction Proper alignment, is easily installed;Multiple coaxial annular cold rinse banks are machined with cold rinse bank inner walls, per two neighboring annular A gap two is machined with the side wall that cold rinse bank is shared, a tank partition wall on the inwall of cold water slot shell, is vertically arranged with Two, tank partition wall two is arranged through all of gap two, and one tank of formation goes out between tank partition wall two and each gap two The mouth of a river, two sink outlets per two neighboring annular cold rinse bank shift to install, by the emulation to kinds of schemes and reality Analysis is tested, the housing of the present invention has the advantages that good cooling results, endless form are reasonable, shorten body of heater cool time;Using Air-flow is then gently caused wireway the reaction zone of reative cell, improves reaction efficiency, shortens the reaction time, and overlay film rate is reachable To 95%, it is ensured that cvd diamond film surface quality.The present invention is applied to the diamond surface CVD of micro- cutter or micro structures Coating process.
Description of the drawings
Fig. 1 is the overall structure of the compact type vacuum reaction unit for chemical vapor deposition diamond film of the present invention Axonometric drawing;
Fig. 2 is the axonometric drawing of housing, wireway, air guide valve, the micro- cutter of deposition cell and objective table assembling;
Fig. 3 is the main sectional view that housing is assembled with upper lid and bottom seat;
Fig. 4 is partial enlarged drawing at the B of Fig. 3;
Fig. 5 is the axonometric drawing of cold water slot shell;
Fig. 6 is the expanded view of cold water slot shell;
Fig. 7 is the axonometric drawing of cold water groove upper cap;
Fig. 8 is partial enlarged drawing at the A of Fig. 1.
In figure, lid 3-1, cold water groove upper cap 3-2, cold water annular groove 3-3, bulge loop one on vacuum meter 1, needle-valve 2, upper lid 3, welding 3-4, one 3-5 of tank partition wall, intake-outlet 3-6, one 3-7 of annular spacing groove, housing 4, welded case 4-1, cold water slot shell 4- 2nd, annular cold rinse bank 4-3, inlet opening 4-4, apopore 4-5, two 4-6 of tank partition wall, sink outlet 4-7, outer 4-8, convex Two 4-9 of ring, observation window 5, one 5-1 of observation window, two 5-2 of observation window, base 6, magnetic valve 7, infrared radiation thermometer 8, objective table 9, poly- The micro- cutter 13 of tetrafluoroethene sealing ring 10, wireway 11, air guide valve 12, deposition cell, vavuum pump 14.
Specific embodiment
Below in conjunction with the accompanying drawings technical scheme is further described, but is not limited thereto, every to this Inventive technique scheme is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should cover In protection scope of the present invention.
Specific embodiment one:As shown in Fig. 1~Fig. 7, a kind of compact for chemical vapor deposition diamond film Vacuum reaction device, which constitutes includes vacuum meter 1, needle-valve 2, upper lid 3, housing 4, base 6, magnetic valve 7, infrared radiation thermometer 8, leads Tracheae 11, air guide valve 12, objective table 9 and three observation windows 5;Three described observation windows 5 are observation window one 5-1 and two respectively Two 5-2 of individual observation window;
Described 4 top and bottom of housing are connected with upper lid 3 and 6 removable seal of base respectively, by housing 4,3 and of upper lid The combination of base 6 constitutes reative cell, and described vacuum meter 1 (by bolt) is fixed on 3 upper surface of upper lid, described vacuum meter 1 Test side closely penetrates the through hole on lid 3 and is arranged in housing 4 that (vacuum meter 1 is used for the vacuum that observes in whole reaction compartment Degree), be fixed with the pipeline communicated with 4 inner chamber of housing on described upper lid 3, described needle-valve 2 (as control reative cell inner chamber with The part of ambient atmos exchange rate) (by bolt) is fixed on the pipeline of upper lid 3, and needle-valve 2 communicates with pipeline that (needle-valve 2 is made For controlling the part of reative cell and ambient atmos exchange rate, flow real-time regulation can be carried out), peep hole is provided with upper lid 3 One, one 5-1 of observation window (for observing the process of whole chemical vapour deposition reaction) is provided with described peep hole one, described One 5-1 of observation window (by CF flanges one and multiple bolts) be fixed on 3 upper surface of upper lid, upper lid 3 is provided with multiple cold water rings Groove 3-3 (leads to cooling water cooling) in cold water annular groove 3-3, and upper lid 3 is provided with gas port one;
Two peep holes two are provided with the side wall of housing 4, are provided with an observation at the peep hole two described in each Two 5-2 of window, described two two 5-2 of observation window (respectively by CF flanges two and multiple bolts) are fixed on the lateral wall of housing 4 On, close to two 5-2 of one of observation window settings, (infrared radiation thermometer 8 is used for measuring reaction interior described infrared radiation thermometer 8 Temperature, two 5-2 of another observation window are used for observing real-time reactiveness), base 6 is provided with gas port two, described electromagnetism Valve 7 (by bolt) is fixed at the gas port two of base 6, and 7 one end of magnetic valve is by the gas port two and reative cell on base 6 Communicate, 7 other end of magnetic valve is connected with vavuum pump 14, and (magnetic valve 7 is vacuumized before being responsible for reaction.If reative cell during the course of the reaction Interior pressure more than 3kPa, then taken away by magnetic valve 7, it is ensured that safety by reaction indoor gas).
Described 11 one end of wireway is connected to inlet box, and what 11 other end of wireway closely penetrated that lid 3 is provided with leads Pore leads to into reative cell (mixed gas are passed through from wireway 11, are flowed into above the micro- cutter 13 of deposition cell along wireway 11), Air guide valve 12 is installed on wireway 11, described air guide valve 12 is arranged on the outside of reative cell and (enters reaction interior Mixed gas flow controls flow by air guide valve 12), described objective table 9 is arranged on reaction interior and is fixed on base 6 On.
The micro- cutter 13 of deposition cell is directly installed on objective table 9, is realized in the presence of mixed gas (hydrogen and methane) (emulation through flow field finds, and compares without wireway, designed wireway 11 for chemical vapor deposition under vacuum condition The flow field near the micro- cutter 13 of deposition cell can be made more to be evenly distributed from top to bottom.Do not affect in installation site simultaneously The visual field of one 5-1 of observation window on lid 3);
11 one end of wireway is connected to inlet box, and the other end is led to into reative cell, mixed gas by the gas port on bell 3 (hydrogen and methane) is passed through from wireway 11, is flowed into above the micro- cutter 13 of deposition cell, by air guide valve along wireway 11 12 control flows.
Needle-valve 2, magnetic valve 7, infrared radiation thermometer 8 and air guide valve 12 used in present embodiment is market purchasing Part.
Specific embodiment two:As shown in Fig. 1, Fig. 3, Fig. 4 and Fig. 7, the one kind described in specific embodiment one is used for changing The compact type vacuum reaction unit of vapor diamond deposition film is learned, described upper lid 3 is by lid 3-1 and cold water groove upper cap in welding 3-2 is constituted, and in described welding, lid 3-1 and cold water groove upper cap 3-2 is disc-shape, covers the external diameter of 3-1 less than cold in welding The external diameter of water groove upper cap 3-2, the upper surface of described cold water groove upper cap 3-2 are machined with multiple concentric with cold water groove upper cap 3-2 Described cold water annular groove 3-3, is provided with gap one on the inboard wall of each cold water annular groove 3-3, per two neighboring cold water annular groove The gap one of 3-3 is separated by 180 ° of settings, and the upper surface of cold water groove upper cap 3-2 is provided with one 3-5 of tank partition wall, described tank every One 3-5 of wall being radially arranged and each cold water annular groove 3-3 are divided into two along cold water groove upper cap 3-2, and one 3-5 of tank partition wall wears Cross in the middle part of the gap one of multiple cold water ring groove 3-3 and by each gap one be separated into two intake-outlet 3-6 (upper lid 3 pass through to Cooling water cooling is passed through in cold water annular groove 3-3).
Specific embodiment three:As shown in Fig. 1, Fig. 3 and Fig. 4, the one kind described in specific embodiment two is used for chemical gas The compact type vacuum reaction unit of phase depositing diamond film, described cold water groove upper cap 3-2 upper surfaces are set near outer edge One 3-7 of annular spacing groove is equipped with, and is provided with one 3-4 of bulge loop, in welding at the neighboring that 3-1 lower surfaces are covered in described welding One 3-4 of bulge loop of lid 3-1 is arranged in one 3-7 of annular spacing groove of cold water groove upper cap 3-2, and covers the bulge loop one of 3-1 on welding 3-4 medial surfaces are engaged with groove face on the inside of one 3-7 of annular spacing groove of cold water groove upper cap 3-2 (to be realized covering 3-1 and cold water in welding Groove upper cap 3-2 is concentric), the groove width of one 3-7 of annular spacing groove of cold water groove upper cap 3-2 is more than one 3-4 of bulge loop for covering 3-1 in welding Thickness, the height of the depth of one 3-7 of annular spacing groove of cold water groove upper cap 3-2 more than one 3-4 of bulge loop for covering 3-1 in welding (guarantee weld lid 3-1 be closely fastened on cold water groove upper cap 3-2), covers 3-1 welding in cold water groove upper cap 3-2 and welding;Weldering Connecting and coaxial described peep hole one is offered on lid 3-1 and cold water groove upper cap 3-2, described one 5-1 of observation window is arranged on 3-1 upper surfaces being covered in welding and being located at peep hole one, one 5-1 of observation window (by CF flanges one and multiple bolts) is fixed on weldering Connect lid 3-1 upper surfaces;Coaxial described through hole and described is offered respectively on lid 3-1 and cold water groove upper cap 3-2 in welding Gas port one.
Specific embodiment four:As shown in Fig. 1~Fig. 3, Fig. 5 and Fig. 6, the one kind described in specific embodiment one is used for changing The compact type vacuum reaction unit of vapor diamond deposition film is learned, described housing 4 is by welded case 4-1 and cold water slot shell 4-2 is constituted, and described welded case 4-1 and cold water slot shell 4-2 are drum, and described cold water slot shell 4-2 is tight It is sleeved on the outside of welded case 4-1 and the two welding, on the inwall of described cold water slot shell 4-2, is machined with multiple coaxial circles Annular cold rinse bank 4-3, is provided with inlet opening 4-4 and apopore 4-5, described inlet opening 4-4 on the side wall of cold water slot shell 4-2 It is arranged in multiple annular cold rinse bank 4-3 in the groove bottom of the annular cold rinse bank 4-3 for being located at bottommost, described apopore 4-5 is arranged in multiple annular cold rinse bank 4-3 in the groove bottom of the annular cold rinse bank 4-3 for being located at top, per adjacent two A gap two is machined with the side wall that individual annular cold rinse bank 4-3 is shared, is vertically arranged on the inwall of cold water slot shell 4-2 Have two 4-6 of tank partition wall, described two 4-6 of tank partition wall to arrange through all of gap two, and two 4-6 of tank partition wall with A sink outlet 4-7, two sink outlets per two neighboring annular cold rinse bank 4-3 are formed between each gap two 4-7 is shifted to install.
(present embodiment is to be machined with multiple annular cold rinse bank 4-3 on the inwall of the cold water slot shell 4-2 of housing 4 Seven annular cold rinse bank 4-3), a gap two is machined with the side wall shared per two neighboring annular cold rinse bank 4-3, Two 4-6 of tank partition wall is vertically arranged with the inwall of cold water slot shell 4-2, and described two 4-6 of tank partition wall passes through all Gap two arrange, and form a sink outlet 4-7 between two 4-6 of tank partition wall and each gap two, per two neighboring Two sink outlet 4-7 of annular cold rinse bank 4-3 are shifted to install.The cooling in each annular cold rinse bank 4-3 can be made Water flows at same direction, and causes the flow of cooling water in per two neighboring annular cold rinse bank 4-3 in opposite direction, so as to increase The flow path of cooling water is added, the cooling scheme is capable of the flowing of efficiently guide cooling water.Cooling water is provided by cooling-water machine.
Specific embodiment five:As shown in figure 3, the one kind described in specific embodiment one is used for chemical vapor deposition Buddha's warrior attendant The compact type vacuum reaction unit of stone film, the top and bottom of described housing 4 are respectively arranged with outer 4-8, upper lid 3 and bottom Connection between seat 6 and housing 4 is respectively adopted the form arrangement uniform in a circumferential direction of multiple screws and fixes, by 3 He of upper lid It is overall that base 6 connects into a closing with housing 4.
Specific embodiment six:As shown in figure 3, the one kind described in specific embodiment five is used for chemical vapor deposition Buddha's warrior attendant The compact type vacuum reaction unit of stone film, under the upper surface and lower end outer 4-8 of the upper end outer 4-8 of described housing 4 Surface is respectively arranged with annular seal groove, is provided with teflin ring 10, shell in the annular seal groove described in each Body 4 seals (ensureing that reative cell has good air-tightness) by teflin ring 10 respectively with upper lid 3 and base 6.
Specific embodiment seven:As shown in figure 3, the one kind described in specific embodiment six is used for chemical vapor deposition Buddha's warrior attendant The compact type vacuum reaction unit of stone film, described 4 lower end of housing are provided with two 4-9 of bulge loop, and described 6 upper surface of base sets Annular spacing groove two is equipped with, two 4-9 of bulge loop of described housing 44 is arranged in the annular spacing groove two of base 6 and (realizes housing 4 Concentric with base 6), and the two 4-9 lateral surfaces of bulge loop of housing 44 are provided with the outer side slot of annular spacing groove two with 6 upper surface of base Face is engaged (realizing that housing 4 is concentric with base 6), and the groove width of the annular spacing groove two of base 6 is more than two 4-9 of bulge loop of housing 4 Thickness, the height of the depth of the annular spacing groove two of base 6 more than two 4-9 of bulge loop of housing 4 (guarantees that 4 lower end of housing is tight It is arranged in the annular spacing groove two of base 6).
Specific embodiment eight:As shown in figure 1, the one kind described in specific embodiment one is used for chemical vapor deposition Buddha's warrior attendant The compact type vacuum reaction unit of stone film, described housing 4 make (being easy to weld) using 304 stainless steels.
The present invention operation principle be:The mixed gas of carbon-source gas (methane) and hydrogen are passed through in vacuum reaction chamber, Control reaction indoor temperature makes mixed gas be heated atom state hydrogen and the excitation state first of successively produce between 700 DEG C~900 DEG C Base, then diamond sp3 hydridization, C-C bond formeds, depositing diamond film on micro- cutter or micro structures.
The course of work is:After each part installation, it is ensured that each several part air-tightness is good.Start water cooling unit to cold rinse bank Supply water in the annular cold rinse bank 4-3 of housing 4-2, open vavuum pump 14 and extract out indoor air is reacted, read on vacuum meter 1 The atmospheric pressure value of detection, maintains near 1Pa.The gaseous mixture of hydrogen and methane is passed through to reaction interior by wireway 11 afterwards Body, adjusts air guide valve 12 and controls reaction rate.In the chemical vapor deposition processes of diamond thin, note observing at three Real time status in 5 outer observation reative cell of window, and with infrared radiation thermometer 8, the indoor reaction temperature of monitoring reaction, control 700 DEG C~900 DEG C between, whole chemical reaction process lasts about greatly 6 hours.
The compact type vacuum reaction unit compact conformation for chemical vapor deposition diamond film of the present invention, reative cell Outline diameter and height are in the range of 300~400mm;The air-tightness of device is good;Reative cell be by housing, base and on The cylindric flat-top closed vessel of lid composition, this structure have the advantages that handling ease, intensity are high, save material and weld seam is few, and From 304 stainless steels for easily welding and roll in selection, air-tightness is further lifted.Additionally, in the design process, upper lid The structure that the annular spacing groove one adopted between housing is engaged with bulge loop one, it is ensured that the proper alignment of the indoor each several part of reaction, It is easy to dismount.

Claims (8)

1. a kind of compact type vacuum reaction unit for chemical vapor deposition diamond film, it is characterised in that:Which constitutes bag Include vacuum meter (1), needle-valve (2), upper lid (3), housing (4), base (6), magnetic valve (7), infrared radiation thermometer (8), wireway (11), air guide valve (12), objective table (9) and three observation windows (5);Three described observation windows (5) are observation window one respectively (5-1) and two observation windows two (5-2);
Described housing (4) top and bottom are connected with upper lid (3) and base (6) removable seal respectively, by housing (4), on Lid (3) and base (6) combination constitute reative cell, and described vacuum meter (1) is fixed on lid (3) upper surface, described vacuum meter (1) test side closely penetrates the through hole on lid (3) and is arranged in housing (4), is fixed with and housing on described upper lid (3) (4) pipeline that inner chamber is communicated, described needle-valve (2) are fixed on the pipeline of lid (3), and needle-valve (2) is communicated with pipeline, upper lid (3) peep hole one is provided with, observation window one (5-1) is provided with described peep hole one, and described observation window one (5-1) is solid Lid (3) upper surface is scheduled on, upper lid (3) are provided with multiple cold water annular groove (3-3), and upper lid (3) are provided with gas port one;
Two peep holes two are provided with the side wall of housing (4), are provided with an observation window at the peep hole two described in each Two (5-2), described two observation windows two (5-2) are fixed on the lateral wall of housing (4), and described infrared radiation thermometer (8) is tight Adjacent one of observation window two (5-2) is arranged, and base (6) is provided with gas port two, and described magnetic valve (7) is fixed on base (6) at gas port two, magnetic valve (7) one end is communicated with reative cell by the gas port two on base (6), and magnetic valve (7) is another One end is connected with vavuum pump (14);
Described wireway (11) one end is connected to inlet box, and wireway (11) other end closely penetrates what lid (3) was provided with Gas port leads to into reative cell, is provided with air guide valve (12) on wireway (11), and described air guide valve (12) is arranged on reaction The outside of room, described objective table (9) are arranged on reaction interior and are fixed on base (6).
2. a kind of compact type vacuum reaction unit for chemical vapor deposition diamond film according to claim 1, It is characterized in that:Described upper lid (3) is made up of lid (3-1) and cold water groove upper cap (3-2) in welding, is covered in described welding (3-1) disc-shape is with cold water groove upper cap (3-2), the external diameter for covering (3-1) in welding is outer less than cold water groove upper cap (3-2) Footpath, the upper surface of described cold water groove upper cap (3-2) are machined with multiple described cold water rings concentric with cold water groove upper cap (3-2) Groove (3-3), is provided with gap one on the inboard wall of each cold water annular groove (3-3), slitting per two neighboring cold water annular groove (3-3) Mouth one is separated by 180 ° of settings, and the upper surface of cold water groove upper cap (3-2) is provided with tank partition wall one (3-5), described tank partition wall One (3-5) being radially arranged and each cold water annular groove (3-3) are divided into two along cold water groove upper cap (3-2), and tank partition wall one (3-5) pass through in the middle part of the gap one of multiple cold water annular groove (3-3) and each gap one is separated into two intake-outlet 3-6.
3. a kind of compact type vacuum reaction unit for chemical vapor deposition diamond film according to claim 2, It is characterized in that:Described cold water groove upper cap (3-2) upper surface is provided with annular spacing groove one (3-7), institute near outer edge Be provided with bulge loop one (3-4) at the neighboring that (3-1) lower surface is covered in the welding that states, cover the one (3- of bulge loop of (3-1) in welding 4) it is arranged in the annular spacing groove one (3-7) of cold water groove upper cap (3-2), and on welding on the inside of the bulge loop one (3-4) of lid (3-1) Face is engaged with groove face on the inside of the annular spacing groove one (3-7) of cold water groove upper cap (3-2), the annular limit of cold water groove upper cap (3-2) Thickness of the groove width of position groove one (3-7) more than the bulge loop one (3-4) for covering (3-1) in welding, the annular limit of cold water groove upper cap (3-2) Height of the depth of position groove one (3-7) more than the bulge loop one (3-4) for covering (3-1) in welding, on cold water groove upper cap (3-2) and welding Lid (3-1) welding;Coaxial described peep hole one is offered on lid (3-1) and cold water groove upper cap (3-2) in welding, described Observation window one (5-1) is arranged in welding and covers (3-1) upper surface and be located at peep hole one, and observation window one (5-1) is fixed on weldering Connect lid (3-1) upper surface;Coaxial described through hole is offered respectively on lid (3-1) and cold water groove upper cap (3-2) in welding With described gas port one.
4. a kind of compact type vacuum reaction unit for chemical vapor deposition diamond film according to claim 1, It is characterized in that:Described housing (4) is made up of welded case (4-1) and cold water slot shell (4-2), described welded case (4-1) drum is with cold water slot shell (4-2), described cold water slot shell (4-2) is closely sleeved on welded case (4- 1) on the outside of and the two welding, multiple coaxial annular cold rinse bank (4- are machined with the inwall of described cold water slot shell (4-2) 3) inlet opening (4-4) and apopore (4-5), are provided with the side wall of cold water slot shell (4-2), and described inlet opening (4-4) sets Put in the groove bottom of the annular cold rinse bank (4-3) for being located at bottommost in multiple annular cold rinse bank (4-3), described water outlet Hole (4-5) is arranged in multiple annular cold rinse bank (4-3) in the groove bottom of the annular cold rinse bank (4-3) for being located at top, Per being machined with a gap two on two neighboring annular cold rinse bank (4-3) shared side wall, cold water slot shell (4-2) interior A tank partition wall two (4-6) is vertically arranged with wall, and described tank partition wall two (4-6) is arranged through all of gap two, And a sink outlet (4-7) between tank partition wall two (4-6) and each gap two, is formed, per two neighboring annular cold water Two sink outlets (4-7) of groove (4-3) shift to install.
5. a kind of compact type vacuum reaction unit for chemical vapor deposition diamond film according to claim 1, It is characterized in that:The top and bottom of described housing (4) are respectively arranged with outer (4-8), upper lid (3) and base (6) and shell Connection between body (4) is respectively adopted the form arrangement uniform in a circumferential direction of multiple screws and fixes, by upper lid (3) and base (6) it is overall that a closing is connected into housing (4).
6. a kind of compact type vacuum reaction unit for chemical vapor deposition diamond film according to claim 5, It is characterized in that:The lower surface of the upper surface of the upper end outer (4-8) of described housing (4) and lower end outer (4-8) is set respectively Be equipped with annular seal groove, in the annular seal groove described in each, be provided with teflin ring (10), housing (4) with upper Lid (3) and base (6) are sealed by teflin ring (10) respectively.
7. a kind of compact type vacuum reaction unit for chemical vapor deposition diamond film according to claim 6, It is characterized in that:Described housing (4) lower end is provided with bulge loop two (4-9), and described base (6) upper surface is provided with annular limit Position groove two, the bulge loop two (4-9) of described housing (44) are arranged in the annular spacing groove two of base (6), and housing (44) The outside groove face that bulge loop two (4-9) lateral surface is provided with annular spacing groove two with base (6) upper surface is engaged, base (6) Thickness of the groove width of annular spacing groove two more than the bulge loop two (4-9) of housing (4), the depth of the annular spacing groove two of base (6) Height more than the bulge loop two (4-9) of housing (4).
8. a kind of compact type vacuum reaction unit for chemical vapor deposition diamond film according to claim 1, It is characterized in that:Described housing (4) is made using 304 stainless steels.
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CN107058972A (en) * 2017-04-17 2017-08-18 哈尔滨工业大学 The micro- cutter coat three-dimensional precise displacement work table applied under hot vacuum environment
CN112210767A (en) * 2020-08-31 2021-01-12 广东鼎泰机器人科技有限公司 Coating machine

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CN102220565A (en) * 2011-06-13 2011-10-19 南开大学 Chemical vapor deposition equipment used for studying light trapping structure of silicon thin-film cell
CN202116642U (en) * 2010-07-23 2012-01-18 上海蓝宝光电材料有限公司 Water-cooling top cap of metal organic chemical vapor deposition equipment
CN104205309A (en) * 2012-05-11 2014-12-10 东京毅力科创株式会社 Gas supply device and substrate processing device

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CN201517131U (en) * 2009-09-16 2010-06-30 湖北师范学院 Apparatus for preparing diamond-like film
CN202116642U (en) * 2010-07-23 2012-01-18 上海蓝宝光电材料有限公司 Water-cooling top cap of metal organic chemical vapor deposition equipment
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Publication number Priority date Publication date Assignee Title
CN107058972A (en) * 2017-04-17 2017-08-18 哈尔滨工业大学 The micro- cutter coat three-dimensional precise displacement work table applied under hot vacuum environment
CN107058972B (en) * 2017-04-17 2019-01-18 哈尔滨工业大学 The micro- cutter coat three-dimensional precise displacement work table applied under hot vacuum environment
CN112210767A (en) * 2020-08-31 2021-01-12 广东鼎泰机器人科技有限公司 Coating machine
CN112210767B (en) * 2020-08-31 2023-02-21 广东鼎泰机器人科技有限公司 Coating machine

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