Classifications

• • C—CHEMISTRY; METALLURGY
  • C23—COATING 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
  • C23C—COATING 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
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/44—Chemical 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
  • C23C16/458—Chemical 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 supporting substrates in the reaction chamber
  • C23C16/4582—Rigid and flat substrates, e.g. plates or discs
  • C23C16/4583—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally
  • C23C16/4584—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally the substrate being rotated
• • C—CHEMISTRY; METALLURGY
  • C23—COATING 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
  • C23C—COATING 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
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/44—Chemical 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
  • C23C16/50—Chemical 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
  • C23C16/513—Chemical 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 plasma jets
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
  • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
  • H01J2237/2001—Maintaining constant desired temperature

Definitions

• This invention relates to temperature control during material deposition and, more particularly, to controlling temperature of a substance being deposited on a surface.
• the invention is especially applicable to deposition of diamond by plasma jet on a rotating surface.
• a plasma of a hydrocarbon and hydrogen can be obtained using electrical arcing, and the resultant plasma focused and accelerated toward a substrate, using focusing and accelerating magnets, so that polycrystalline diamond film is deposited on the substrate.
• Figure 1 illustrates a prior art type of configuration wherein a rotatable mandrel 110, coupled with a rotary union 115, is rotated, such as by a belt or gear drive (not shown), and coolant fluid can be circulated through the mandrel, in the direction indicated by the arrows, or in the opposite direction.
• a disc-shaped spacer 150 and substrate 170 are shown as being mounted on the rotating mandrel.
• temperature at the deposition surface of a disc-shaped substrate can vary substantially in the radial direction, due to factors such as variation in heating by the beam as a function of its cross section.
• the present invention is directed to an apparatus and technique for use in systems where a substance is being deposited on a mandrel or substrate, and where it is desirable to control temperature at the deposition surface. In many applications it is desirable to obtain spatial and temporal temperature uniformity over the deposition surface, but the invention is also applicable to situations where it is desirable to obtain a particular temperature pattern at the deposition surface.
• the deposition technique may require heating or cooling of the deposition surface, with cooling being necessary or desirable for most plasma deposition applications, such as deposition of synthetic diamond film, which is an important application of the invention.
• the invention is also particularly advantageous in systems where the mandrel (which may have a substrate mounted thereon) is rotated during deposition.
• 5,204,144 discloses a plasma jet deposition system wherein the deposition surface is rotated at a relatively high rate, and this facilitates obtaining temperature uniformity on the surface, particularly where the depositing plasma jet has a smaller cross-sectional area than the surface on which the substance (e.g. diamond) is being deposited.
• temperature uniformity in the radial direction could stand improvement, and a feature of the invention achieves this objective.
• an apparatus for depositing a substance which comprises: a mandrel rotatable on an axis; a spacer mounted on the mandrel; a substrate mounted on the spacer; means for directing, toward the substrate, a plasma containing constituents of the substance being deposited; the spacer having a thermal conductance in its thickness direction that varies with radial dimension.
• the thermal conductance of the spacer in the thickness direction varies by at least 5 percent from minimum to maximum.
• An advantage of the summarized feature of the invention is that the radial temperature profile on the deposition surface can be better controlled. For example, in a situation where the center of the substrate tends to be hotter than the outside thereof, and where temperature uniformity is desired, a spacer having greater thermal conductance toward the center can provide effectively greater heat exchange near the center (by providing a higher thermal conductance path for heat exchange with the cooled mandrel near the center of the substrate), or vice versa for the opposite situation.
• the spacer comprises a disc having concentric grooves therein.
• the metal will generally have much higher thermal conductivity than the open space of the grooves, so by providing, for example, more groove volume near the center of the spacer, the thermal conductance thereof will be higher toward the periphery of the spacer.
• the thermal conductance of the spacer in the thickness direction, can vary linearly or non-linearly with radial dimension.
• the radial heat flux characteristic at the deposition surface is determined, and a spacer is provided that has a thermal conductivity in its thickness direction that varies in accordance with (i.e., inversely with, for most situations) the determined radial heat flux characteristic.
• a method for depositing diamond film that includes the following steps: providing a deposition chamber; providing, in the chamber, a rotating mandrel; directing a plasma containing a hydrocarbon gas and hydrogen gas toward the mandrel; and controlling temperature on the surface of the mandrel by passing coolant fluid radially through the mandrel at several angular reference positions in the mandrel.
• the step of passing coolant fluid radially through the mandrel comprises providing radial bores through the mandrel at several angular reference positions.
• the fluid is hydrogen, and the fluid enters the environment of the chamber after passing radially through the mandrel to the periphery of the mandrel. Since most of the environment of the chamber is hydrogen, permitting hydrogen gas to enter the chamber does not contaminate the deposition environment. An advantage of this feature is that it becomes unnecessary to return the heat exchange fluid through a rotating seal, as the hydrogen in the chamber is ultimately handled by the vacuum system that controls the chamber pressure.
• the fluid is passed through the mandrel at an angle with respect to the surface of the mandrel. Preferably, the angle is at least 2 degrees with respect to the plane of the mandrel surface. In this manner, heat exchange can be varied radially. For example, depending on the direction of the taper with respect to the mandrel surface, the heat exchange can be concentrated either more toward the center of rotation of the mandrel or more toward the periphery of the mandrel.
• Figure 1 is a simplified cross-sectional diagram which illustrates a prior art rotating mandrel assembly with heat exchange.
• FIG. 2 is a schematic diagram, partially in block form, of an apparatus in accordance with the invention, and which can be used to practice the method of the invention.
• Figure 3 is a plan view of a spacer in accordance with an embodiment hereof.
• Figure 4 is a cross-sectional view of the Figure 3 spacer, as taken through a section defined by arrows 4-4 of Figure 3.
• Figure 5 is a plan view of another spacer, in accordance with an embodiment of the invention.
• Figure 6 is a cross-sectional view of the Figure 5 spacer, as taken through a section defined by the arrows 6-6 of Figure 5.
• Figure 7 is a plan view of another spacer, in accordance with an embodiment of the invention.
• Figure 8 is a cross-sectional view of the Figure 7 spacer, as taken through a section defined by the arrows 8-8 of Figure 7.
• Figure 9 is a cross-sectional view of a spacer in accordance with a further embodiment of the invention.
• Figure 10 is a cross-sectional view of a spacer in accordance with a further embodiment of the invention.
• Figure 11 is a cross-sectional view of a spacer in accordance with a further embodiment of the invention.
• Figure 12 illustrates an example of a graph of incoming heat flux as a function of radial dimension on the substrate disc surface.
• Figure 13-15 are cross-sectional views of spacers having conductances, in the thickness direction, that vary non- linearly with radial dimension, and are inversely matched to the heat flux characteristic of Figure 12.
• Figure 16 is an operational flow diagram of a method in accordance with an embodiment of the invention.
• Figure 17 is a side sectional view of a temperature controlled rotatable mandrel in accordance with a further embodiment of the invention.
• Figure 18 is a cross-sectional view of the mandrel of Figure 17, as taken through a section defined by arrows 17-17 of Figure 17.
• Figure 19 is a side cross-sectional view of a temperature controlled rotatable mandrel in accordance with another embodiment of the invention.
• Figure 20 is a slide cross-sectional view of a temperature controlled rotatable mandrel in accordance with another embodiment of the invention.
• a deposition chamber 100 is the lower section of a plasma jet CVD deposition system 200, evacuated by one or more vacuum pumping systems (not shown).
• the system 200 is contained within a vacuum housing 211 and includes an arc-forming section 215 which comprises a cylindrical holder 294, a rod-like cathode 292, and an injector 295 mounted adjacent to the cathode so as to permit 8 injected fluid to pass over the cathode.
• a cylindrical anode is provided at 291.
• the input fluid may be, for example, a mixture of hydrogen and methane. The methane could alternatively be fed in downstream.
• the anode 291 and cathode 292 are energized by, a source of electrical power (not shown), for example a DC potential.
• Cylindrical magnets, designated by reference numeral 217 are utilized to help control the plasma generation.
• a nozzle, represented at 115, can be used to control beam size, within limitations.
• Optional cooling coils 234, in which a coolant can be circulated, can be located within the magnets.
• a mixture of hydrogen and methane is fed into the injector 295, and a plasma is obtained in front of the arc forming section and accelerated and focused toward the deposition region at which a substrate is located.
• synthetic polycrystalline diamond can be formed from the described plasma, as the carbon in the methane is selectively deposited as diamond, and the graphite which forms is dissipated by combination with the hydrogen facilitating gas.
• suitable types of deposition equipment including, for example, other types of CVD plasma deposition equipment, or physical vapor deposition equipment, can be used in conjunction with the features of the invention to be described.
• a mandrel 110 is rotatable on a shaft 111, and has a spacer 120 and a substrate 170 mounted thereon (by means not shown, bolting or clamping being typical) .
• the mandrel 110 can be cooled by any suitable means, for example by using a heat exchange fluid (e.g. water) that is circulated through the mandrel, as in the prior art arrangement first illustrated in Figure 1.
• the mandrel can be tilted with respect to the direction of the plasma-jet, as disclosed in U.S. Patent No. 5,342,660.
• the heat exchange fluid can be fed and returned through a rotary union, as shown in Fig. 1, and a suitable motor (not shown) can be used for rotating the shaft, as is also disclosed in U.S. Patent No. 5,342,660.
• the rotational drive will conventionally be above the rotary union.
• Figures 3 and 4 illustrate, respectively, a plan view and a cross-sectional view of a spacer disc 120 which may be formed, for example, of metal (for example molybdenum or titanium), graphite, or ceramic, and has a plurality of concentric annular grooves 121 formed therein, such as by machining.
• the grooves can be empty, or can be filled with a material having a different thermal conductivity than the rest of the spacer disc.
• the grooves are uniformly spaced so that variation in thermal conductance in the thickness direction, as a function of radius, will be local, and will result in an overall lower thermal conductance of the spacer (as compared to a solid spacer) , since the open grooves have a lower thermal conductivity than the solid material of the disc.
• This generally symmetrical configuration will tend to result in macroscopically uniform thermal conductance, in the thickness direction, as a function of radial dimension. [The "ripple" in conductance over relatively short radial distance will tend to be smoothed by the remaining spacer thickness and substrate thickness. ]
• Figures 5 and 6 illustrate a configuration that results in greater thermal conductance (and, accordingly, more heat transfer) near the center than near the periphery of the spacer. This is achieved by providing more groove volume (greater cross-sectional area and/or greater groove depth) near the outside of the spacer, such as by providing more grooves or wider grooves or deeper grooves near the periphery. [The illustration of Figure 5 has more grooves near the periphery.]
• the mandrel is cooled relatively uniformly, and if one uses a prior art configuration such as that of Figure 1 (with a solid spacer, or, for example, with no spacer) there may be a substantial radial temperature gradient, which could result in non-uniform diamond deposition and quality.
• a spacer of the type shown in Figures 5 and 6 between a cooled mandrel and a substrate will tend to provide more efficient cooling toward the center of the substrate, as the grooves reduce thermal conduction from substrate to cooled mandrel near the periphery.
• the groove pattern can be designed to obtain the desired thermal conductivity characteristic.
• a supply of spacers, having different thermal conductivity characteristics in their thickness direction, as a function of radial dimension, can be provided for use in different situations and to "match" the inverse of the expected radial temperature gradient on the substrate deposition surface.
• Figures 7 and 8 illustrate the opposite case; that is, a spacer configuration which has relatively less thermal conductivity (in the thickness direction) toward the center of the spacer disc and relatively greater thermal conductivity toward the periphery thereof.
• the grooves are illustrated as being in one surface of the spacer, but it will be understood that other configurations can be provided, for example as shown in Figure 9 where both surfaces of the spacer have grooves, the grooves on the bottom being labelled 122. As shown in Figure 10, the grooves on opposing sides of the spacer need not necessarily align in radial position. Also, it will be understood that other means can be provided for obtaining a radial thermal conductivity variation in the spacer.
• the grooves may be filled with a material, such as a ceramic, metal, graphite or gas, having a different thermal conductivity than the original spacer material.
• Figures 12-15 illustrate further embodiments hereof wherein the thermal conduction of the spacer in its thickness direction, as a function of radial dimension, can be selected to obtain a generally uniform temperature at the deposition surface by providing a thermal conduction in the thickness direction, as a function of radial dimension, that is substantially the inverse of the radial heat flux pattern at the deposition surface.
• Figure 12 illustrates a typical gaussian bell-shaped distribution of incoming heat flux (such as in units of watts per cm 2 ) as a function of radial dimension on the substrate disc surface at which deposition is taking place.
• Figures 13, 14, and 15 illustrate embodiments of spacers (120) which have thermal conduction in their thickness direction, as a function radial dimension, that is an inverse of the heat flux at the deposition surface. Accordingly, these spacers can be used to promote a generally uniform temperature at the deposition surface of the substrate during plasma deposition.
• the thermal conduction characteristic is obtained by using equally spaced grooves (124), with groove depths increasing (non- linearly, in this case) as a function of radial dimension.
• the depths of grooves (124) are the same, but groove widths are increased (again, non-linearly for this case) as a function of radial dimension.
• the spacer 120 has an upper region 1501 formed of a relatively higher thermal conductivity material, and a lower region 1502 formed of a relatively lower thermal conductivity material, so that, again, the thermal conduction in the thickness direction will decrease as a function of radial dimension in a non-linear fashion.
• the interface curve between the materials can be selected to obtain the desired conductance to be the inverse of the heat flux characteristic.
• the material 1501 may be molybdenum
• the material 1502 may be graphite of a type having lower thermal conductivity than molybdenum.
• FIG. 16 illustrates an operational flow diagram of the steps for practicing an embodiment of a method hereof.
• the block 1610 represents the determining of the incoming heat flux characteristic at the deposition surface as a function of radial dimension.
• the incoming heat flux pattern can be determined, for example, by measuring temperature using known pyrometer or spectroscopy techniques, or from direct measurement of temperature at the substrate surface.
• the block 1620 represents providing of a spacer having a thermal conduction in its thickness direction, as a function of radial dimension, that is an inverse of the determined heat flux characteristic. Then, with the spacer provided between the cooled mandrel and the substrate, the block 1630 represents deposition of the substance to be deposited, synthetic diamond being a substance of particular interest herein.
• a fluid coolant is utilized in a mandrel in an advantageous way.
• Figures 17 and 18 illustrate a configuration, which can be used, for example, in the plasma jet deposition system of Figure 2, wherein coolant fluid is passed radially through a mandrel 1710 via radial bores 1715, leaves the mandrel through peripheral openings, and enters the environment of the deposition chamber.
• a fluid that is normally contained in the environment in this case hydrogen gas, the need to return coolant fluid through the fluid through the mandrel is eliminated.
• Figure 19 illustrates a configuration wherein the coolant-carrying bores taper toward the deposition surface as they extend radially, this configuration producing more cooling toward the periphery of the deposition surface than the one shown in Figures 17 and 18.
• the opposite type of taper is shown in Figure 20, which will tend to provide relatively less cooling toward the periphery of the deposition surface.

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• General Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Materials Engineering (AREA)
• Mechanical Engineering (AREA)
• Metallurgy (AREA)
• Organic Chemistry (AREA)
• Physics & Mathematics (AREA)
• Plasma & Fusion (AREA)
• Chemical Vapour Deposition (AREA)
• Crystals, And After-Treatments Of Crystals (AREA)

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Citations (3)

• 1994
  • 1994-11-01 JP JP51452294A patent/JPH10508069A/ja active Pending
  • 1994-11-01 WO PCT/US1994/012605 patent/WO1996013623A1/en not_active Application Discontinuation
  • 1994-11-01 EP EP95901749A patent/EP0792386A4/en not_active Withdrawn

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