JP2004134741A - Control system for sublimation of reactant - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an apparatus and a method for improving the heating of a solid precursor in a sublimation vessel. <P>SOLUTION: In one embodiment, an inactive heat conduction element is dispersed among a group of solid precursors. For example, the heat conduction element can construct powder, beads, rods, and fibers. In the heat conduction, the heat conduction element can be directly heated by microwave energy. <P>COPYRIGHT: (C)2004,JPO

Description

【Technical field】
[0001]
The present invention relates to a solid precursor source used to deposit a thin film on a substrate. More particularly, the present invention relates to increasing the thermal conductivity to a solid precursor in a precursor source device.
[Background Art]
[0002]
Solid precursors are used quite frequently for vapor reactants because, for certain elements, liquid or gaseous precursors are not readily available or exist at all. Such solid precursors are useful in a variety of situations, including but not limited to atomic layer deposition (ALD) and other semiconductor fabrication processes. However, using solid precursors is more difficult than liquid and gaseous precursors.
[0003]
Basically, the handling of solid precursors seems simple. The solid precursor is filled into a container heated to a sufficiently high temperature. The precursor sublimes and the precursor vapor is directed to the reaction space where it is used to deposit a thin film on the substrate surface.
[Disclosure of Invention]
[Problems to be solved by the invention]
[0004]
Precursor powders generally have a much lower thermal conductivity. The thermal conductivity of the bulk precursor may be low and / or there may be empty voids between the precursor particles with little contact with the particle surface. However, this is undesirable for transferring thermal energy to the precursor. The volume of the voids depends on the packing density of the precursor powder. At low pressures, heat transfer by convection is also generally inefficient, especially when the precursor volume consists of very small voids between the precursor particles. Heat transfer by radiation is also generally inefficient because the temperature difference is relatively small and the radiant view factor of the entire powder is essentially zero.
[0005]
If the precursor container is externally heated, the precursor can raise the temperature near the wall of the container sufficiently, but the central portion of the precursor powder is insufficiently heated. This temperature difference results from the fact that it takes a long time to heat the centrally located part of the precursor powder in the precursor container. In addition, sub-centered sublimation of the precursor consumes thermal energy, so that the center of the precursor volume remains at a lower temperature than the powder near the vessel surface throughout the process. During ALD pulsing, this temperature difference may not be sufficient to reach a state of equilibrium in the gas phase of the precursor vessel, thus slowing the rate of recovery of the solid source after prolonged use of the precursor source. It becomes a factor to do. The ALD process is relatively insensitive to small pulse concentration drifts, but significant reductions in recovery rates, such as less than the full surface coverage of the semiconductor wafer (or other substrate) by precursor molecules, can cause problems. there is a possibility.
[0006]
Because of the temperature difference within the precursor container, the precursor sublimates into the gas phase at the high temperature portion of the container volume and condenses back to the solid phase at the low temperature portion of the container volume. Often the top surface of the precursor appears to be cooler than the rest of the precursor. Over time, a hard, dense crust was formed on the surface of the heated precursor, and it was observed that processes using vapor reactants (eg, ALD) resulted in pulse concentration drift. This crust limits the diffusion of precursor molecules from the bulk material to its surface and ultimately into the gas phase. As a result, the observed sublimation rate of the precursor decreases. The solid precursor source works well at first, but then a sufficiently high flow rate from the solid precursor source into the reaction chamber, despite significant amounts of solid precursor remaining in the precursor container It is difficult to obtain precursor molecules of
[0007]
Another problem in the design of sublimation vessels is that the prolonged presence of heated corrosive precursors places a significant burden on those materials that come into contact with the precursors in the precursor vessel.
[Means for Solving the Problems]
[0008]
Preferred embodiments of the present invention provide a means for improving the uniformity of the source temperature throughout the volume of the solid precursor vessel. According to one aspect of the invention, an inert material having a high thermal conductivity is mixed with a solid precursor to improve the thermal conductivity of the precursor. For example, the inert material can include highly thermally conductive particles, fibers, rods, or other elements distributed throughout the precursor container and mixed with the precursor powder.
[0009]
In accordance with one embodiment of the present invention, there is provided a method of producing vapor from a solid precursor for processing a substrate, the method comprising placing a solid precursor group in a container, and applying heat to the entire precursor. Including interspersing the conductive material. Thereby, the thermally conductive material preferably serves to transfer thermal energy to the entire precursor group. The steam is then formed by applying thermal energy to both the thermally conductive material and the solid precursors. In one embodiment, after the formation of the vapor, the vapor is pumped from the container to the reaction chamber and reacts to deposit a layer on the substrate.
[0010]
According to another embodiment, a substrate processing system for forming a vapor from a solid precursor by distributing heat across the precursor is provided. The provided system includes a heat transfer container configured to hold a solid precursor group, wherein the heat transfer element is interspersed with the solid precursor group. A heater for heating both the precursor and the heat transfer element is also provided.
[0011]
According to yet another embodiment, a substrate processing system for forming a vapor from a solid precursor is provided. The system includes a container configured to hold a group of solid precursors, and a microwave oscillator adjacent the container. The oscillator is configured to transfer heat energy in the form of microwave energy to effect heating of the precursor.
[0012]
According to another embodiment, there is provided a mixture for producing steam used in substrate processing. The mixture includes a batch precursor for producing substrate processing vapor and a plurality of heat transfer solids dispersed throughout the batch precursor. The plurality of heat transfer solids collectively increase the thermal conductivity of the precursor for batch processing.
[0013]
Advantageously, realization of the preferred embodiment results in less crust formation on the precursor surface and increased sublimation of the precursor. In addition, improved sublimation rate uniformity throughout the operating life of the precursor batch process reduces the amount of unused precursor. Replenishment of the precursor containers is also necessary, albeit less frequently, ie the material is used efficiently. Another advantage of the present invention is that between pulses, the partial pressure of the reactants in the gas phase of the vessel is reduced to a steady state value (one such value is P0, the saturated vapor pressure of the material). By rapid recovery, the process of using vapors from solid precursors improves the uniformity of the film thickness on the substrate.
[0014]
For purposes of summarizing the invention and the advantages achieved over the prior art, certain objects and advantages of the invention have been described above. Of course, it should be understood that it is not necessary to achieve all such objects or advantages in accordance with any particular embodiment of the present invention. Thus, for example, one skilled in the art may realize one or several of the advantages taught herein without necessarily realizing other objects or advantages that may be taught or suggested herein. It will be appreciated that the invention may be embodied and practiced in an optimizing manner.
[0015]
All of these embodiments are within the scope of the invention disclosed herein. These and other embodiments of the present invention will be readily apparent to those skilled in the art from the following detailed description of the preferred embodiments, taken in conjunction with the accompanying drawings, and the present invention is not limited to any particular embodiment disclosed. However, the present invention is not limited to the preferred embodiment.
BEST MODE FOR CARRYING OUT THE INVENTION
[0016]
Referring to FIG. 1A, a precursor source device 5 is shown in series between a carrier gas source 4 and a reaction chamber 6 configured to receive a substrate 8.
[0017]
FIG. 1B shows a preferred embodiment of a precursor source device 5 for vaporizing a solid precursor, wherein the resulting vapor is used for substrate processing, the device 5 comprising a pressure chamber 10, an inlet 12 and , An outlet 14 and preferably an overpressure relief valve 16. The inlet 12 is preferably attached to the carrier gas supply 4 (FIG. 1A) via the first conduit 2, while the outlet 14 is connected to the reaction chamber 6 (FIG. 1A) via the second conduit 3. Preferably, it is attached to
[0018]
FIG. 2 is a schematic partially cutaway perspective view of the precursor source device 5 of FIG. 1, showing an internal precursor container or crucible 20 within the pressure chamber 10. An internal crucible 20 located in the pressure chamber 10 is used as a precursor container. The shape and dimensions of the crucible 20 are selected according to the volume available in the temperature controlled pressure chamber 10. The material of the crucible 20 can include an inert substance such as quartz glass or silicon carbide. Further, it is preferable to arrange a particle filter 22 at the top of the crucible 20. In an alternative embodiment, a particle filter is located at the container outlet 14 or at the second conduit 3. In a preferred embodiment, a porous crucible wall is used, which acts as a particle filter as the precursor vapor diffuses through the wall.
[0019]
FIG. 3 shows a crust formation in the prior art, which is one of the problems that the preferred embodiment of the present invention seeks to address. FIG. 3 shows a schematic side view of a crucible 20 holding a volume of solid precursor 32. The outer skin 34 is easily formed on the upper surface of the solid precursor 32, and the arrow 36 in FIG. 3 indicates the direction of movement of heat applied to the crucible 20.
[0020]
4 and 5 show yet another preferred embodiment of the present invention. Insert 38 is configured to fit into crucible 20 (FIG. 2) or other container in which the solid precursor is retained. The insert 38 is preferably selected to have good thermal conductivity. The insert 38 includes a heat conducting element 40, i.e., a rod, here, which is machined and attached to the bottom 42 of the container. Preferably, heat flows along the major axis of element 40 and then radially outward toward the material, resulting in efficient and uniform heating of the entire precursor volume. Element 40 is preferably formed, for example, of the highest purity and quality SiC to allow for cleaning and reuse. In another embodiment, the heat conducting element is preferably made of the same material as the container, for example stainless steel. In the illustrated embodiment, this element is formed of graphite coated with SiC, while in other embodiments the element is uncoated. In yet another embodiment, the element is formed from a thermally conductive material other than SiC and graphite.
[0021]
According to one preferred embodiment, the insert 38 of FIGS. 4 and 5 is machined and fitted into the precursor container 20. The precursor is then poured into the container 20. According to another embodiment, the precursor container 20 is first filled with the precursor powder 32 and then the element 40 shown in FIGS. Push so that the lower end of rod 40 contacts the bottom of precursor container 20. In an alternative embodiment, a rod is attached to the bottom of the source container 10 and the source container 10 is filled with the precursor powder 32. In yet another arrangement, each of the plurality of rods is configured to be inserted independently of one another. It is noted that rod density is a function of the heat transfer properties of the solid (ie, a solid with poor heat transfer is desirably of a higher density to have fewer heat transfer paths).
[0022]
According to the embodiment shown in FIGS. 4 and 5, the rod 40 can be positioned on the bottom plate 42. The rods 40 are preferably arranged, for example, in a polar coordinate type layout, so that each precursor group 32 is located within a certain distance from the rod 40 or the base plate 42. The number of vertical rods 40 attached to the plate will vary depending on the physical properties of precursor 32. If the heat transport in the precursor is very poor, more rods can be used.
[0023]
In yet another alternative embodiment, the plurality of thermally conductive elements interspersed with precursors can be formed from fixed elements, such as, for example, rods, laminated screens, sieves, coils, plates, and the like. These units or elements can include both porous and non-porous structures. These fixed units or elements are preferably arranged to maximize the amount of thermally conductive surface in contact with the precursor, while allowing vapor diffusion from the inlet to the outlet of the carrier gas. Preferably, the precursor diffuses through the mixture of powder and heat conducting element. The carrier gas preferably transports the chemical at the top (or headspace) of the container by convection from the inlet to the outlet.
[0024]
FIG. 6 shows a preferred embodiment in which the heat conductive element 46 and the precursor powder 32 are mixed in the crucible 20. In one preferred arrangement, the conductive element 46 is a powder particle, but in an alternative arrangement, the conductive element 46 comprises a larger loose element such as a fiber, strip, flake, pellet, sphere, ring, etc. Can be. The chemical catalysts industry uses elements with similar geometries (beads, pellets, spheres, rings, etc.) each coated with a catalytic material, and thus is suitable for implementing alternative arrangements of the present invention. It is believed that a geometric unit configuration is also provided. These units or elements 46 can include both porous and non-porous structures. This bulking element 46 is preferably arranged to maximize the total amount of thermally conductive surface that contacts the precursor 32. In one preferred embodiment, element 46 is formed from an inert thermally conductive material such as a ceramic, for example, SiC. The shapes and materials from which such elements 46 can be formed are discussed in more detail below.
[0025]
In an alternative embodiment, the plurality of conductive elements 46 are interspersed with a batch of precursor to form a mixture. Preferably, the inclusion of a heat-transferring solid increases the thermal conductivity of the precursor in the batch.
[0026]
Referring to FIG. 7, another embodiment of the present invention using an energy emitter 48 adjacent to the crucible 20 is shown. SiC or another inert energy absorbing material (not shown) is placed together with the precursor material in the precursor container, preferably in the container or crucible 20 shown, so that the precursor (not shown) has energy absorption. Get closer to the material. In one arrangement, it is preferred that the precursor container is also permeable to the emitted energy. Preferably, the wavelength of emitted energy is in the microwave range, but alternative arrangements of the embodiments disclosed herein use emitted energy at other wavelengths.
[0027]
In a preferred operation, the microwave heats the microwave absorbing material and heats the flow from the heated material to the precursor, which may be according to FIGS. In other arrangements, the crucible itself uses microwave energy in the crucible, which absorbs microwave energy, thereby transferring heat from the crucible wall to the precursor. In general, precursors commonly used for depositing thin films do not absorb microwaves and therefore cannot be directly heated by microwaves. However, materials such as SiC absorb microwaves, and the SiC is heated rapidly, thereby allowing the precursor to be heated as uniformly as desired. Similarly, other combinations of energy absorbing materials and energy sources operating at various wavelengths are possible in light of the present disclosure. In yet another arrangement, if the precursor material is capable of directly absorbing electromagnetic energy, such as microwaves, heating the precursor material directly is sufficient to vaporize the desired precursor, and therefore A separate microwave absorbing material can be omitted.
[0028]
It should be understood that in an alternative arrangement of the previous embodiment, the precursor could be injected directly into the bottom of the pressure chamber 10 omitting the inert crucible. Preferably, the surface of the pressure chamber 10 in which it is located is sufficiently inert. In an alternative embodiment, the particle filter is also preferably located at the top of the precursor powder or in a conduit (not shown) between the precursor source and the reaction chamber. In embodiments using a crucible, the crucible can be formed with porous walls to serve as a filter, thereby reducing the need for a separate particle filter. According to one preferred embodiment, the thermally conductive material is mixed with the precursor, but in another preferred embodiment, the machining is performed before, during, or after the precursor is charged into the chamber. Place the inserted insert in the chamber.
[0029]
Size and shape of inert heat conductive material
The heat-conducting material or element can be used in a variety of shapes, such as, for example, powders and fibers, irregular strips, and machined articles.
[0030]
The particle size of the inert powder is chosen according to the application, as will be appreciated by those skilled in the art. Precursor source containers that do not contain any particulate filters should preferably be filled with a conductive inert element (eg, SiC powder) that is coarse enough to prevent dusting of the material. The precursor source vessel with the filter can be filled with a wide range of conductive particles, with the smallest particles being preferably blocked by the particle filter. One advantage of using small inert conductive particles is that very small voids in the precursor powder can be filled, increasing the packing density and the thermal conductivity of the precursor volume. One purpose of one preferred embodiment is to make the thermal conductivity of the precursor powder uniform and high.
[0031]
According to a preferred embodiment, the thermal conductivity of the mixture of the conductive element and the precursor is lower than the pure conductor material and higher than the pure precursor. For example, an inert thermally conductive material may be added to a solid precursor to form a solid mixture, and therefore preferably about 10-80% by volume of the thermally conductive material in the precursor / conductor mixture, more preferably the mixture About 30 to 60% by volume of the thermally conductive material is present therein. Re-use of conductors is possible, but is a challenge, especially if the conductor has a very small particle size.
[0032]
In another embodiment, fibers of an inert conductive material, such as carbide or carbon, are used. The fiber preferably conducts heat efficiently along the fiber within the volume of the precursor, and also preferably provides heat to the precursor located near the fiber. The fibers are preferably cut into strips of about 1-20 mm in length, and are mixed with the aforementioned precursors. For example, suitable SiC fibers are commercially available from Reade Advanced Materials, USA. The selected heat conducting fibers preferably distribute heat from the walls of the heater or precursor vessel to the precursor.
[0033]
According to yet another embodiment, it is preferred to use a machined part of an inert conductive material, thereby obtaining certain benefits. The use of larger machined parts makes it relatively easy to recover the thermally conductive material after use. Further, the heat conducting material can be cleaned and reused many times. Therefore, an expensive heat conductive material with very high purity can be economically used. The machined article may take the form of, for example, a rod or plate (shown in FIGS. 4 and 5), or a combination of such shapes and other shapes, such as along the length of the rod or other extension. It can take any shape, including screens mounted at various levels.
[0034]
In some embodiments, a combination of a machined article and a smaller thermally conductive strip is used. The machined product preferably conducts heat transport over a long distance from the wall of the heater or heated precursor container to the volume of the precursor, while bulked heat transfer units (such as beads, powders, fibers, etc.) ) Is preferably mixed with the precursor to distribute heat locally to the precursor. In one arrangement, a thermally conductive material in powder form is used in combination with a thermally conductive material in fiber form. Another arrangement uses a rod with a powdered thermally conductive material. In view of the disclosure contained herein, one of ordinary skill in the art will readily appreciate other combinations of thermally conductive material forms and materials that are also considered advantageous.
[0035]
In selecting the added inert material used according to the present invention, good thermal conductivity is desirable. Preferably, the inert material for this has a thermal conductivity of at least about 50 W / mK, more preferably at least about 80 W / mK at room temperature for the applications indicated in this patent application. , Most preferably, has such a high conductivity under the conditions of use.
[0036]
Silicon carbide
In one preferred embodiment, silicon carbide (SiC) is used to form an inert material added to the crucible or container. SiC is a very hard material, has high thermal conductivity, negligible vapor pressure, and has very good resistance to chemicals at high temperatures. Performance, Materials, Inc. of the United States. According to the above, the thermal conductivity of SiC is 250 W / m · K at room temperature and about 120 W / m · K at 400 ° C. A wide range of grades of SiC of varying purity are commercially available. It is known that the color of silicon carbide (SiC) correlates with its purity. According to Reade Advanced Materials of the United States, the purity of black SiC is up to about 99.2%, the purity of dark green SiC is about 99.5%, and the purity of light green SiC is about 99.7%. %. SiC is available in the form of powders, coarse particles, crystals, granules, wafers, fibers, platelets, bars, and strips of any shape. Common impurities in SiC produced from silica sand and coke are SiO2, elemental Si, free C, and Fe2O3. Such impurities are preferably minimized so that possible contamination in processes using precursors is reduced. Thus, in a preferred embodiment, it is preferred that the inert conductive material be greater than 99% pure.
[0037]
There are several commercial sources for high purity SiC. For example, 99% pure SiC is available from Atlantic {Equipment} Engineers, USA, in all grit sizes. Poco @ Graphite, Inc. of the United States. In addition, very high purity SiC is produced by a chemical vapor infiltration (CVI) method in which pure graphite is brought into contact with vapor of silicon monoxide (SiO) (Chemical Reaction Scheme 1). The impurity amount of SiC is within the ppm level.
[0038]
SiO (g) + 2C → SiC + CO (g) Reaction formula 1
Cerac, Inc. of the United States. Sells vacuum deposited grade (99.5%) SiC strips with dimensions in the range of 3-12 mm.
[0039]
Other materials
Some other suitable inert carbides are commercially available. The thermal conductivity of transition metal carbides is generally about 50% lower than that of SiC, and the conductivity of transition metal carbides is often sufficient to provide improved sublimation. Atlantic Equipment Engineers in the United States includes tungsten carbide (WC), vanadium carbide (VC), tantalum carbide (TaC), zirconium carbide (ZrC), hafnium carbide (HfC), molybdenum carbide (MoC), niobium carbide (NbC), and We sell titanium carbide (TiC) powder. The purity of the carbide powder is generally 99.8-99.9%. Such metal carbides also have useful stoichiometry other than 1: 1 metal to carbon.
[0040]
Furthermore, boron carbide having a sufficiently high thermal conductivity (for example, B₄Alternative carbides such as C) can be used, but it is preferred that boron carbide not be used in applications susceptible to boron impurities.
[0041]
Another suitable inert, conductive material is PocoFoam ™, manufactured by Poco @ Graphite, USA, which is a very light carbon foam with a thermal conductivity in the range of 100-150 W / m · K. It is.
[0042]
Coated material
When selecting a material to form a thermally conductive material, it is undesirable to utilize a material that has a high thermal conductivity, but cannot be used directly in a solid precursor container without modification. . For example, a potential material may have the desired thermal conductivity, but the material reacts with the precursor during processing, ie, during sublimation. Therefore, the material selected to be in direct contact with the precursor is preferably inert. In certain preferred embodiments, coating a material that has high thermal conductivity and is not inert with an inert material allows for the use of materials that are considered undesirable when used alone. For example, graphite and silicon are both good conductors of heat. Graphite is very soft and readily forms solid particles that can contaminate substrates in the reaction chamber. Therefore, in order to reduce the number of particles emitted from graphite, it is preferable to form a hard inert coating on the surface of graphite. Similarly, silicon is an efficient reducing agent when the native oxide on the silicon surface is destroyed. The inert coating deposited on the silicon surface preferably prevents the reaction of the silicon with the precursor.
[0043]
In particular, graphite or silicon can be coated with SiC in certain preferred embodiments. Other suitable coating materials include boron carbide, niobium carbide (NbC), tantalum carbide (TaC), titanium carbide (TiC), tungsten carbide (WC), zirconium carbide (ZrC), molybdenum carbide (MoC), vanadium carbide ( VC) and hafnium carbide (HfC). Such metal carbides also have useful theoretical quantities other than 1: 1. In one embodiment, the impure carbide is preferably coated with a thin high-purity CVD carbide coating that prevents contamination of the precursor in the precursor container. In this embodiment, the impurities in the CVD carbide coating are in the parts per million (ppm) range and therefore do not significantly contaminate the precursor or substrate. Transition of TiN (NbN), Tantalum Nitride (TaN), Titanium Nitride (TiN), Tungsten Nitride (WN), Zirconium Nitride (ZrN), Molybdenum Nitride (MoN), Vanadium Nitride (VN), Hafnium Nitride (HfN) Metal nitrides serve as another example of a suitable inert coating on a thermally conductive material surface. Further, in one embodiment, silicon nitride is formed on the silicon surface, and thus the silicon portions and pieces are passivated.
[0044]
The following examples, including the methods performed and the results obtained, are provided for purposes of illustration only and are not meant to limit the invention.
[0045]
Example
Example 1
HfCl via a sequential self-saturating surface reaction₄And H₂HfO from the alternately sent pulse of O₂For deposition of ASM @ International, N.B., Bilthoven, The Netherlands. V. A Pulser® 3000 @ ALCVD ™ reactor, commercially available from Co., Ltd., was used. HfCl for this pulse₄Steam was supplied from a solid source. HfCl₄A mixture of $ 157.6 g and 99.5% SiC @ 200.8 g (obtained from Orkla @Exolon, Norway) was charged to the source vessel. This mixture contains about 100 cm of each precursor³Was included. Thus, the mixture of precursor material and conductive element was a 1: 1 mixture by volume.
[0046]
As a result, the supply source temperature could be reduced from 200 to 205 ° C. (without filling with carbide) to 180 ° C. (with filling with carbide). This may be because the precursor sublimation rate was faster and more stable, thus improving the rate of source recovery (i.e., the time after pulsing where sufficient steam was generated for the next pulse). The deposition of thin films from batches of the same precursor has been possible for a longer time than without carbide loading. By adding SiC, HfO on the substrate₂The film thickness uniformity was improved. Use of the SiC conductive filler did not affect the number of particles on the wafer.
[0047]
Example 2
In the glove box, ZrCl₄Powder and boron carbide (B₄C) The powder was mixed. The mixture was charged into a glass source boat. The source boat containing the mixture was then placed in a glass tube that served as a carrier tube. ZrCl₄The end of the tube was covered with Parafilm so that the tube was not exposed to room air and moisture. The tube was removed from the glove box by ASM International International N.D. V. Was transferred to the F120 @ ALD reactor, the source boat was transferred from the carrier tube to the source tube (pressure vessel) of the reactor, and inert nitrogen gas was discharged from the source tube. After the loading of the source boat was completed, the substrate was placed in the reaction chamber of the reactor, and the reactor was evacuated with a mechanical vacuum pump to a vacuum. The reactor pressure was adjusted to about 3-10 mbar with flowing inert nitrogen gas. The reaction chamber was heated to the deposition temperature and the reactor ZrCl₄The reactant zone was also heated to sublimation temperature. ZrO₂The thin film is made of ZrCl4 and H₂Deposited from successive alternating pulses of O vapor. ZrCl₄Sublimation rate is between boron carbide and ZrCl₄It was found that mixing was clearly faster. Boron carbide helped transfer thermal energy throughout the precursor volume.
[0048]
Although the present invention has been disclosed in terms of certain preferred embodiments and examples, those skilled in the art will appreciate that the present invention is not limited to the particular disclosed embodiments and other alternative embodiments and / or uses of the invention and its obvious uses. It will be understood that the present invention extends to various modifications. Therefore, the scope of the invention disclosed herein should not be limited by the particular disclosed embodiments, but should be determined solely by a fair reading of the following claims.
[Brief description of the drawings]
[0049]
1A is an external view of a precursor source device disposed in series between a gas source and a reaction chamber. FIG.
FIG. 1B is a schematic side view of the precursor source device of FIG. 1A, constructed in accordance with a preferred embodiment.
FIG. 2 is a schematic partially cutaway perspective view of the precursor supply device of FIG. 1B, showing a precursor container in a pressure chamber.
FIG. 3 is a schematic side view of a prior art precursor container, with an outer skin formed on the top surface of a volume of solid precursor, and arrows indicating the direction of heat flow.
FIG. 4 is a schematic top view of a container insert with a heat conducting rod attached to a container base, constructed according to a preferred embodiment.
FIG. 5 is a schematic perspective view of the insert of FIG.
FIG. 6 is a schematic side view of a precursor source device having a thermally conductive unit interspersed with precursors, according to a preferred embodiment.
FIG. 7 is a schematic partially broken perspective view of a precursor source device having adjacent microwave units, according to an embodiment of the present invention.

Claims (41)

A method of producing vapor from a solid precursor for processing a substrate, comprising:
Placing the solid precursors in a container;
Interspersing the precursors in the heat conducting material and forming a vapor by applying thermal energy to both the heat conducting material and the solid precursors;
Passing steam from the vessel to the reaction chamber. The method of claim 1, further comprising reacting the vapor to deposit a layer on the substrate. The method of claim 1, wherein the step of interspersing the solid precursors with the thermally conductive material comprises forming a solid mixture having about 10% to 80% by volume of the thermally conductive material in the mixture. . The method of claim 1, wherein the step of interspersing the solid precursors with the thermally conductive material comprises forming a solid mixture having about 30% to 60% by volume of the thermally conductive material in the mixture. . A substrate processing system for forming a vapor from a solid precursor by distributing heat to the precursor, comprising:
A container configured to hold a group of solid precursors;
A plurality of heat conducting elements interspersed with the solid precursors,
A system comprising: a heater configured to transfer thermal energy to both the heat conducting element and the precursor. The system of claim 5, wherein the container is a heat transfer container. 6. The reaction chamber of claim 5, further comprising a reaction chamber fluidly connected to the vessel, the chamber configured to provide a suitable environment for the reaction of vapor emanating from the vessel to deposit a layer on a substrate. System. The system according to claim 7, wherein the reaction chamber is a chemical vapor deposition chamber (CVD). The system according to claim 7, wherein the reaction chamber is an atomic layer deposition chamber (ALD). 6. The system of claim 5, wherein the solid precursors are in powder form. The system according to claim 5, wherein the heat conducting element is formed from a substance that is substantially inert to the reaction in the vessel. The system of claim 5, wherein the heat conducting element has a coating that is substantially inert to reactions in the vessel. The system of claim 5, further comprising a vacuum chamber surrounding the container. The system of claim 5, wherein the heater is a microwave oscillator configured to transfer microwave energy to the heat transfer element. The system according to claim 5, wherein the heat conducting element is a plurality of rods configured to be inserted into the container. The system of claim 15, wherein the rod is mounted on a base plate configured to be inserted into the container. 16. The system of claim 15, wherein the rod is attached to a base of the container. The system of claim 15, wherein the plurality of rods are each configured to be inserted independently of one another. 6. The system of claim 5, wherein the heat conducting element is a fiber composed of interspersed solid precursors contained within the container. The system according to claim 5, wherein the heat conducting element is in powder form. The system of claim 5, wherein the heat conducting element comprises carbon. 22. The system of claim 21, wherein said heat conducting element comprises a metal carbide. 22. The system of claim 21, wherein said heat conducting element comprises a transition metal carbide. 22. The system of claim 21, wherein said heat conducting element comprises boron carbide. 22. The system of claim 21, wherein said heat conducting element comprises silicon carbide (SiC). The system of claim 5, wherein the heat conducting element comprises a rod and powder combination. The system of claim 5, wherein the heat conducting element comprises a rod and fiber combination. The system of claim 5, wherein the thermal conductivity of the heat conducting element is at least about 50 W / mK at room temperature. The system of claim 5, wherein the thermal conductivity of the heat conducting element is at least about 80 W / mK at room temperature. A substrate processing system for forming a vapor from a solid precursor, comprising:
A container configured to hold a group of solid precursors;
A microwave oscillator adjacent to the container, the oscillator configured to transfer heat energy in the form of microwave energy to effect heating of the precursor. 31. The system of claim 30, further comprising a plurality of heat conducting elements interspersed with solid precursors, wherein the heat conducting elements readily absorb the microwave energy. 31. The system of claim 30, wherein the solid precursors are formulated to be directly heated by the microwave energy transmitted from the microwave oscillator. 31. The system of claim 30, wherein the container is made to be directly heated by microwave energy transmitted from the microwave oscillator. A mixture for producing steam used in substrate processing,
Precursors for batch processing to generate substrate processing steam;
A mixture comprising a plurality of heat transfer solids interspersed with a batch of precursors, which collectively increase the thermal conductivity of said batch of precursors. 35. The mixture of claim 34, wherein the plurality of heat transfer solids are selected from the group consisting of powders, spheres, irregularly shaped strips, and machined parts. 35. The mixture of claim 34, wherein the plurality of heat transfer solids are selected from the group consisting of rods, screens, sieves, coils, and plates. 35. The mixture of claim 34, wherein the plurality of heat transfer solids are formed from a material selected from the group consisting of metal carbides, transition metal carbides, boron carbide, and silicon carbide. 35. The mixture of claim 34, wherein the plurality of heat transfer solids are substantially inert to a desired reaction used in the substrate processing. 35. The mixture of claim 34, wherein the plurality of heat transfer solids are coated with a material that is substantially inert to a desired reaction used in the substrate processing. The plurality of heat transfer solids are configured to conduct heat from the precursor proximate an edge of the precursor batch to a precursor substantially centrally located in the precursor batch. 35. The mixture of claim 34. 35. The mixture of claim 34, wherein the plurality of heat transfer solids absorb microwave energy generated from a microwave oscillator and emit heat to a solid precursor.

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