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EP3818189A1 - Verfahren und vorrichtung zur diamantsynthese durch cvd - Google Patents

Verfahren und vorrichtung zur diamantsynthese durch cvd

Info

Publication number
EP3818189A1
EP3818189A1 EP19730385.2A EP19730385A EP3818189A1 EP 3818189 A1 EP3818189 A1 EP 3818189A1 EP 19730385 A EP19730385 A EP 19730385A EP 3818189 A1 EP3818189 A1 EP 3818189A1
Authority
EP
European Patent Office
Prior art keywords
substrate
plasma
diamond
electrodes
chamber
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP19730385.2A
Other languages
English (en)
French (fr)
Inventor
Horacio Tellez Oliva
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Diarotech
Original Assignee
Diarotech
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Diarotech filed Critical Diarotech
Publication of EP3818189A1 publication Critical patent/EP3818189A1/de
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C23C16/272Diamond only using DC, AC or RF discharges
    • 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
    • C23C16/50Chemical 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 using electric discharges
    • C23C16/503Chemical 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 using electric discharges using DC or AC discharges
    • 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
    • C23C16/50Chemical 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 using electric discharges
    • C23C16/505Chemical 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 using electric discharges using radio frequency discharges
    • C23C16/509Chemical 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 using electric discharges using radio frequency discharges using internal electrodes
    • 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
    • C23C16/50Chemical 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 using electric discharges
    • C23C16/517Chemical 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 using electric discharges using a combination of discharges covered by two or more of groups C23C16/503 - C23C16/515
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32009Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32018Glow discharge
    • H01J37/32027DC powered
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32009Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32018Glow discharge
    • H01J37/32036AC powered
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32009Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32082Radio frequency generated discharge
    • H01J37/32091Radio frequency generated discharge the radio frequency energy being capacitively coupled to the plasma
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32431Constructional details of the reactor
    • H01J37/3244Gas supply means
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32431Constructional details of the reactor
    • H01J37/3266Magnetic control means
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/32Processing objects by plasma generation
    • H01J2237/33Processing objects by plasma generation characterised by the type of processing
    • H01J2237/332Coating
    • H01J2237/3321CVD [Chemical Vapor Deposition]

Definitions

  • the invention relates to the field of diamond synthesis or any other allotropic form of carbon by chemical vapor deposition.
  • Carbon is a material having several allotropic forms, naturally in the solid state on earth, which are amorphous carbon and three crystallized forms, graphite, diamond and lonsdaleite.
  • the diamond consists mainly of sp 3 hybridized carbon atoms while the graphite consists mainly of sp 2 hybridized carbon.
  • Other allotropic forms exist, in a synthetic state, such as DLC.
  • Diamond is a material with a unique combination of properties, such as resistance to wear, thermal conductivity or electrical insulation, which are very interesting for many technical applications.
  • the rarity and the price of natural diamonds make its use on a large scale impossible and confine it to luxury jewelry.
  • methods of diamond synthesis have been developed, in the hope of facilitating access to this material on a larger scale for technical applications.
  • DLC or “Diamond Like Carbon” is also an interesting material, differentiating from diamond by a proportion of sp 2 hybridization carbon, up to 60%, in sp 3 hybridization carbon.
  • the method of choice for the synthesis of thin diamond layers or DLC on a substrate is chemical vapor deposition or CVD (Chemical vapor deposition) at low pressure.
  • CVD Chemical vapor deposition
  • the diamond is deposited in crystalline form on a substrate placed in a chamber into which a gas carrying carbon atoms is introduced which is transformed into plasma by an energy source.
  • the invention relates first of all to a method of diamond synthesis, in a vapor deposition chamber and on a synthesis substrate, between two plasma generation electrodes, according to which:
  • a gas carrying carbon atoms is introduced into the chamber and a plasma is created near the substrate to generate reactive carbon atoms,
  • the invention also relates to a method of diamond synthesis, in a vapor deposition chamber (1) and on a synthesis substrate (5), between two electrodes (4, 5) for generating plasma, according to which:
  • a gas carrying carbon atoms is introduced into the chamber (1) and a plasma (28) is created near the substrate to generate reactive carbon atoms, process characterized by the fact that the plasma is created by applying, between the two electrodes, a direct current (DC) (6) and an alternating current at radio frequency (RF) (46).
  • DC direct current
  • RF radio frequency
  • the invention also relates, finally, to a method of diamond synthesis, in a vapor deposition chamber (1) and on a synthesis substrate (5), between two electrodes (4, 5) for generating plasma, according to which :
  • a gas carrying carbon atoms is introduced into the chamber (1) and a plasma (28) is created near the substrate to generate reactive carbon atoms,
  • diamond here is meant, and in the following description, all allotropic forms containing carbon in the sp 3 hybridization state, such as in particular diamond, in all its crystalline forms or DLC.
  • the reactive carbon atoms are typically carbon atoms in "activated" form, that is to say radical or ionic.
  • This expression also designates here carbonaceous molecules in an activated form, that is to say radical or ionic.
  • Compressing the plasma consists of guiding, or focusing, the reactive plasma species, such as the radicals and the ions produced between the electrodes, in a restricted region between the two electrodes in order to increase their concentration and, consequently, the probability of reaction shocks between radicals.
  • the increase in the number of shocks also makes it possible to generate UVC, or even infrared, photons which themselves make it possible to generate additional reactive atoms.
  • the combination of these effects makes it possible to considerably improve the speed of deposition of diamond on the substrate.
  • the electrodes between which the plasma is generated are supplied by a source of direct current (DC).
  • DC direct current
  • This energy source is effective in starting the diamond deposit.
  • the thickness of the layer formed becomes substantial, for example from 25-30 ⁇ m, at the temperature prevailing in the chamber, for example example between 300 and 1600 ° C, the diamond layer becomes an electrical insulator sufficient to significantly reduce the passage of energy between the electrodes and therefore decrease the diamond synthesis speed.
  • the applicant proposes a hybridization of the generation of energy and to combine the source of direct current (DC) with a current source by radiofrequencies (RF) and thus to create the plasma by application, between the two electrodes , direct current and alternating current at radio frequency (RF).
  • the direct current (DC) source can be permanent or chopped.
  • the DC / RF ratio can be adjustable during the synthesis, in particular as a function of the thickness of diamond already synthesized, so that the speed of diamond deposition remains constant.
  • the reactive carbon atoms in the plasma, it is possible to apply, near the substrate, a magnetic field.
  • the reactive atoms instead of following a direct trajectory between the electrodes, acquire in addition a movement of loop, or of helical tendency.
  • the reactive atoms thus travel a longer path and gain more speed, increasing the probability of collisions, generating the C-C sp3 hybridization bonds characteristic of diamonds, and therefore the speed of synthesis. This also helps to avoid arcs and holes in the diamond layer or film formed.
  • the plaintiff does not intend to limit the scope of its request to diamond synthesis.
  • the process of the invention can benefit any other material which can be synthesized by chemical vapor deposition, such as, for example, Si-Ge type semiconductors from a silicon-bearing gas and a germanium-bearing gas, or silicon oxides or nitrides.
  • the present invention first relates to the methods of claims 1-3.
  • the invention is not limited here to pure diamond, but can also be applied to doping diamond.
  • the diamond can be doped with boron; then introduced into the chamber, in addition to the gas carrying carbon atoms, a boron-carrying gas such as trimethylborane, boron trichloride or diborane.
  • Diamond can also be doped with nitrogen; is then introduced into the chamber, in addition to the gas carrying carbon atoms, a nitrogen-bearing gas such as dinitrogen, ammonia or methyl amine.
  • the invention also relates to a vapor deposition chamber, provided with a gas inlet and a gas outlet, and inside which are arranged two electrodes for generating plasma connected to a direct current (DC) source, characterized in that plasma compression means are provided between the two electrodes.
  • DC direct current
  • the two electrodes are also connected to a source of alternating current at radio frequency (RF).
  • RF radio frequency
  • the two electrodes are an anode and a cathode, the cathode forming a diamond deposition substrate.
  • Figure 2 schematically illustrates a vapor deposition chamber according to the invention
  • FIG. 3 is a perspective view of the electrodes and of the grid of FIG. 2.
  • a vapor deposition chamber 1 comprises an inlet 2 for gas, an outlet 3 for depressurization, electrodes, an anode 4 and a substrate 5 forming a cathode, connected to the terminals of a DC power supply 6, the circuit being connected to earth 7.
  • a gas carrying carbon atoms for example methane or ethane
  • the pressure in chamber 1 is reduced by applying a vacuum to the output 3 and a voltage is applied between the electrodes 4 and 5.
  • the molecules of the gas carrying carbon atoms are activated to form a plasma in a large volume 8.
  • the volume 8 of plasma extends beyond the area strictly between the electrodes.
  • the energy applied between the electrodes has the particular effect of dissociating certain bonds, such as for example C-H bonds, thus generating reactive species, such as for example carbon and hydrogen radicals.
  • reactive species such as for example carbon and hydrogen radicals.
  • These radicals can then either reassociate themselves with hydrogen radicals, or with other carbon radicals, thus leading to the formation of a CC bond, the hydrogen radicals can also associate with each other to form hydrogen gas which can be evacuated from the room by exit 3.
  • the energy of the CC bond being weaker than that of the CH bond, the reaction equilibrium is thus shifted towards the gradual replacement of all the CH bonds by CC bonds, that is to say the diamond formation.
  • the substrate may also contain species which make it possible to initiate, on contact, the formation of CC bonds.
  • Free radicals are an unstable species with a very long life in a gaseous medium. same if the formation of a molecular bond starting from the pendant bond of the radical is very energetically favorable it requires a shock to three bodies in order to allow the conservation of the momentum. It is therefore a very rare phenomenon. It is quite different on the surface, a gas radical associates easily with a radical center of the surface, because the phonons can then ensure the conservation of the momentum.
  • a sample holder can be placed on the substrate in order to give specific dimensions to the deposit, or to avoid deposit directly on the electrode.
  • the probability of collisions between reactive carbon atoms is directly proportional to the density of the atoms of these reactive carbon atoms in zone 8, which is itself linked to the energy applied between the two electrodes 4 and 5.
  • the electrodes 4 and 5 are here parallel disks whose centers are placed along an axis AA '.
  • the grid 20 is connected to a source of direct current.
  • the electrode 4 could have other forms, such as for example being made up of a single or of a set of points with a spherical end directed along the axis AA ′.
  • the electrode 4 can have a concave, convex or flat shape
  • the chamber 1 is placed under low pressure (pressure below atmospheric pressure) of gas carrying carbon atoms, by opening the gas inlet 2 and applying a vacuum at the outlet 3.
  • Direct current is applied between electrodes 4 and 5, generating a plasma of reactive carbon atoms between the electrodes.
  • a direct current is applied to the grid 20 in order to create around the cylinder which it defines, an electric field having the effect of orienting the reactive carbon atoms of the plasma in a zone 28 defined between the electrodes 4 and 5 and limited in width by the interior of the cylinder formed by the grid 20.
  • Diamond is gradually deposited on the substrate 5, in a homogeneous layer. For the same energy applied between the electrodes 4 and 5 between the devices of FIGS.
  • the plasma extension zone is reduced in the presence grid 20, the plasma is compressed, thereby increasing the density of the reactive carbon atoms.
  • the probability of collisions between reactive carbon atoms and with the surface is thus increased, which makes it possible to increase the speed of formation and deposition of diamond on the substrate, or optionally on a sample holder placed on the substrate.
  • the grid is made with one or more materials with high electronic emissivity.
  • refractory materials such as for example molybdenum or tungsten, to obtain a longer lifetime of the grid and limit the deformation due to the temperatures it can reach.
  • These refractory materials can optionally be doped, for example with thorium, to increase their electronic emissivity. Indeed the peak effect, created on the whole surface of the grid and by each of the elements which compose it, converts it into a structure of a large surface of emission of electrons.
  • the grid 20 shown here is of circular section, but any other section can be envisaged.
  • the shape can be chosen according to the shape of the diamond that one wants to obtain.
  • the grid mesh and / or its height can also be adapted according to the dimensions and / or characteristics of the chamber, the electrodes and / or the chamber.
  • the height of the grid can be the same around the entire periphery of its section or variable, for example in corners, to compensate for electronic effects which would lead to an inhomogeneous deposit of diamond.
  • the grid, the rings or the tube thus defined are plasma compression means which have the function of:
  • Diamond being an electrical insulator, as the layer of diamond deposited on the substrate thickens, it forms a barrier to the direct current passing between the electrodes 4 and 5, in particular when the layer of diamond reaches 25 to 30 ⁇ m thick. Consequently, for the same applied voltage, the density of the reactive carbon atoms in the plasma decreases as a function of the thickness of the diamond layer. The speed of diamond deposition decreases as the thickness of the already formed layer increases.
  • the applicant proposes to combine the source of direct current (DC) with a source of current by radio frequencies (RF) and therefore to create the plasma by application, between the two electrodes, direct current and alternating current at radio frequency (RF).
  • DC direct current
  • RF radio frequencies
  • the electrodes 4 and 5 are connected to a source 46 of alternating current at radio frequency and to a ground 47, in parallel with the circuit comprising the source 6 direct current.
  • the source 46 of alternating current at radio frequency preferably comprises, at its output, a filter preventing the direct current from the source 6 from entering back into the source 46.
  • the source 6 of direct current also preferably comprises, at its output a filter preventing the alternating current at radio frequency from the source 46 from entering back into the source 6.
  • a direct current and an alternating current at radio frequency are applied between the electrodes 4 and 5.
  • the ratio between the two currents can be constant during the synthesis. It has been observed, surprisingly, that the DC / RF ratio has an effect on the crystal form of the diamond depositing on the substrate. For example, in a configuration allowing the formation, on a substrate of ultra-nanocrystals of diamond with the application of a DC current only, the application of RF current in an RF / DC power ratio of 0.05 to 0.3 allows to obtain a deposit formed by larger crystals, that is to say of sub-micrometric dimension at several ten microns.
  • the ratio between the two currents can be variable during the synthesis, in order to optimize the synthesis speed.
  • the RF current can gradually take over from the direct current as the layer of diamond deposited thickens.
  • the DC / RF ratio could for example also be selected according to the properties desired for the deposition.
  • the hybrid power supply system for plasma generating electrodes thus improves the speed of diamond deposition, by compensating for the electrical insulating effect of the diamond already deposited. It also allows you to play on characteristics such as the structure and properties of the deposit.
  • the RF current source can also be connected to the gate 20, in parallel with the direct current source. These sources can be the same as those supplying the electrodes, or separate sources. Each of these sources can be optionally connected via a power regulator in order to modulate the DC / RF power ratio supplied to the grid. This facilitates the emission of electrons from the grid.
  • a magnetic field can be applied to the plasma, preferably near the substrate. This makes it possible to reduce, or even avoid, the presence of holes in the diamond layer / film formed.
  • a permanent magnet 50 generating a magnetic field 51 represented by the dotted lines is placed under the substrate electrode 5.
  • the magnet or electromagnet
  • Electrodes 4 and 5 shown here are only powered by direct current. It is obviously possible to combine direct current with RF current here too.
  • a single magnet is shown here under the substrate 5, but it could be placed near the anode 4. There could also be several magnets, in particular one near the substrate 5 and one near the anode 4.
  • the charged atoms of the plasma 28, moving between the electrodes under the effect of the electric field created between the anode 4 and the cathode 5, are in addition subjected to the magnetic field 51, in the vicinity of the substrate. 5.
  • Their trajectory is thus deviated under the action of the Lorentz force, the effect of the two fields adding up on each charged / reactive atom: the charged atoms will then tend to follow a helical trajectory, longer than in the presence of a single field, forming loops around the magnetic field lines.
  • the addition of the effects of the two fields will also accelerate the movement of the reactive atoms.
  • Reactive atoms traveling faster over a longer trajectory then have a higher probability of collision, which results in an increase in the concentration of activated carbons and ultimately an increase in the rate of formation and deposition of the diamond on the substrate.
  • a permanent magnet has been described here, but any form of magnet, permanent or not, making it possible to generate an appropriate magnetic field in the vicinity of the substrate can be used.
  • the distance between the anode and the substrate / cathode can be adjusted to optimize the deposition.
  • the three elements of the invention the plasma compression means, the hybridization of the current sources and the application of a magnetic field in the vicinity of the substrate, each have, separately, a positive effect on the speed. diamond formation and deposition, linking these three elements by a unique inventive concept. This effect is all the more pronounced as two of these means, or the three means are used in combination, as illustrated in the following example.
  • UVCs generated in situ in the plasma contribute to improving the efficiency of the reaction, by promoting the dissociation of the reagent bonds to form the plasma. It is also possible, for the same effect of places to apply UVC near the substrate, where the plasma is formed. UVC lamps can be arranged in the chemical vapor deposition chamber.
  • photons of frequency and / or particular energies chosen to correspond to an absorption frequency of the material to be synthesized and / or of a reagent, can be sent to the substrate to improve the rate of formation of matter.
  • a 260 mm diameter and 160 mm high CVD chamber contains a 3.2 mm diameter tungsten anode placed approximately 35 mm above a 15 mm by 15 mm silicon substrate forming the cathode.
  • the grid is made of molybdenum and has a diameter of 5 cm in diameter, a height of about 1 cm and a mesh of 1 mm.
  • a transverse magnetic field of 0.02 T is produced by an electromagnet.
  • the two sources are applied here at the same time over the entire duration of the deposition.
  • the carbon-bearing gas introduced into the chamber consists of a mixture of 3% methane in 97% hydrogen.
  • the pressure is brought to approximately 300 mBar and stabilized in order to ensure the stability of the plasma.
  • the temperature in the chamber during the synthesis is approximately 950 ° C., which here corresponds to the optimal temperature for deposition on a silicon substrate.
  • the direct current applied is a direct current of 735 V, with a power of approximately 1200 W ( ⁇ 100W).
  • the simple presence of the grid makes it possible to double the speed of deposition and to homogenize the nature of the film.
  • the combination of the grid and the hybrid DC / RF power source accelerates more than six times the deposition rate.
  • the magnetic field applied here makes it possible to avoid the discharges coming from specific electric arcs and leading to the presence of holes in the diamond deposit and also by itself alone allows to almost double the speed of deposit.
  • the nature of the substrate influences the crystal form of the diamond, depending on whether it is, for example made of silicon, molybdenum, tungsten, titanium or quartz.
  • the plasma compression means can be applied to any other type of synthesis by chemical vapor deposition, at atmospheric pressure or at low pressure, in order to to improve the speed of deposition. It is the same for DC / RF hybridization and / or the application of a magnetic field near the substrate.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Power Engineering (AREA)
  • Chemical Vapour Deposition (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Plasma Technology (AREA)
  • Formation Of Insulating Films (AREA)
EP19730385.2A 2018-07-05 2019-06-18 Verfahren und vorrichtung zur diamantsynthese durch cvd Pending EP3818189A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
BE20185473A BE1026449B1 (fr) 2018-07-05 2018-07-05 Procédé et dispositif de synthèse de diamant par CVD
PCT/EP2019/066079 WO2020007605A1 (fr) 2018-07-05 2019-06-18 Procede et dispositif de synthese de diamant par cvd

Publications (1)

Publication Number Publication Date
EP3818189A1 true EP3818189A1 (de) 2021-05-12

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP19730385.2A Pending EP3818189A1 (de) 2018-07-05 2019-06-18 Verfahren und vorrichtung zur diamantsynthese durch cvd

Country Status (6)

Country Link
US (2) US12227834B2 (de)
EP (1) EP3818189A1 (de)
JP (1) JP7575376B2 (de)
CN (1) CN112384640B (de)
BE (1) BE1026449B1 (de)
WO (1) WO2020007605A1 (de)

Family Cites Families (13)

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US12227834B2 (en) 2025-02-18
BE1026449A1 (fr) 2020-01-29
US20250115991A1 (en) 2025-04-10
CN112384640A (zh) 2021-02-19
JP2021530625A (ja) 2021-11-11
BE1026449B1 (fr) 2020-02-03
WO2020007605A1 (fr) 2020-01-09
CN112384640B (zh) 2024-06-18
US20210172060A1 (en) 2021-06-10

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