The present invention relates to a microwave heating apparatus that can be used as heat source for chemical and/or physical processes.
Furthermore, the invention relates to a method that uses this apparatus for carrying out such processes.
As well known, many chemical processes have to be triggered by high temperature, and other processes are strongly accelerated by high temperature. Therefore, in many cases a reacting material is supplied by energy from a heat source. Traditionally, this is made through apparatus that transfer heat to the reacting material by conductivity or convection. However, such apparatus are often inefficient, since they not perform a uniform distribution of temperature in the reacting material or they require long time for bringing the reaction to a predetermined temperature.
In the last years, microwave apparatus are commonly used in research laboratories and in the industry. In this type of apparatus, a quick variation of the electromagnetic field that influences the material cause its direct heating and with a maximum efficiency with respect to traditional heating methods.
A microwave apparatus typically comprises an oven in which the reacting material is put and then irradiated with radio waves at high frequency. Microwaves are generated by a Magnetron that causes an electronic beam to oscillate at a very high frequency, thus creating microwaves, or more recently they are generated by solid state oscillating devices. These apparatus have relevant advantages with respect to traditional heat source. In fact, they are capable of providing an exceptionally quick heating of the reacting material and of quickly achieving higher temperatures than other conventionally used systems.
However, the technology of heating with microwave ovens has some drawbacks.
Firstly, reactors used for this type of technology have to be made of suitable materials, i.e. materials transparent to microwaves. The used microwave reactors are normally closed in containers with metal walls that are scarcely manageable and are accessible in a difficult way. Furthermore, it is not possible to use microwaves in case of reactions that take place at high pressures, since metal reactors are required with high thicknesses, and for these reactions they cannot be crossed by microwaves.
Other drawbacks are the high cost and the high energy consumption required by the microwave technology that strongly limits its diffusion on a large scale.
It is therefore a first feature of the invention to provide a microwave heating apparatus for chemical-physical processes that provides a method for heating a reacting material that is more effective and practical with respect to the devices of prior art.
It is another feature of the invention to provide a microwave heating apparatus for chemical-physical processes that provides an energy saving and that is cheap with respect to apparatus of prior art.
It is also a feature of the invention to provide a microwave heating apparatus for chemical-physical processes for applying the microwave technology also in the field of reactions that take place in a condition of high pressure.
It is also a feature of the invention to provide a microwave heating apparatus for chemical-physical processes for activating chemical reactions in a homogeneous or heterogeneous phase, either continuous or pulsed.
These and other features are accomplished with one exemplary microwave heating apparatus for chemical-physical processes, according to the present invention, said apparatus comprising:
According to the invention, the reaction container has a housing coated with dielectric material transparent to microwaves suitable for receiving the means for transmission. The housing crosses the container for at least one part thereof. The microwave source and the means for transferring is arranged in a reaction station, and a means is provided for conveying the reacting material from a first position, upstream of the reaction station, to the reaction station, and then to a second station downstream of the reaction station. In the reaction station the means for transferring is arranged at least in part within the reaction container and can irradiate directly the reacting material.
Advantageously in the reaction station an actuation means can be provided for moving the means for transferring from a first position, outside of the housing, to a second position inside of the housing, such that in the second position the means for transferring is arranged at least in part within the reaction container and can irradiate directly the reacting material.
Preferably, the reaction container can be a reaction vessel in which the housing is integrated, and the means for conveying is arranged to move the reaction vessel from the first position, upstream of the reaction station, to the reaction station, in which the means for transferring is aligned with the housing of the reaction vessel and is in turn introduced in the housing by the actuation means, and then to the second station downstream of the reaction station.
In a possible embodiment of the invention, the reaction container is a reaction tube in which the housing is integrated to the reaction tube, and the means for conveying is arranged to cause the reaction material to flow in the reaction tube from the first position, upstream of the reaction station, to the reaction station in which the means for transferring is arranged in the housing of the reaction tube, and then to the second station downstream of the reaction station.
In particular, the housing can be integrated to the reaction tube at least in part transversally to the reaction tube.
In a possible preferred embodiment, a plurality of housings is arranged at least in part transversal to the reaction tube, and a plurality of means for transferring is provided arranged in the housings, wherein a control means is further provided to control the irradiation power in the reaction tube according to a desired temperature profile of the reaction material flowing in the reaction tube.
Preferably, the housing can be integrated to the reaction tube coaxially to the reaction tube.
Advantageously, the second station can comprise a nozzle, and the reaction material can be projected through the nozzle into a vacuum chamber where it can be deposited on a deposition substrate.
In an exemplary embodiment of the invention, the apparatus comprises also a means for emitting one form of energy selected from the group comprised of:
or a combination thereof.
Advantageously, the reaction container can provide a coating layer made of a heat-insulating material.
In particular, the apparatus can comprise, furthermore, at least one sensor for measuring a process parameter, for example pressure or temperature, during the development of the reaction.
Advantageously, the apparatus can comprise also a means for mixing the reacting material, for example a mixer of the type with magnetic bar.
Preferably, the means for transferring the microwaves comprises at least one microwave antenna, for example of co-axial type or in a wave guide, which has at an end a connector for being operatively connected to the microwave source, and at the other end a microwave emitter suitable for irradiating the reacting material.
Advantageously, the antenna is coated with a closed sheath of inert material, for example PTFE, glass, ceramics etc., suitable for avoiding a direct contact with the reagents.
In a possible configuration of the invention, the means for transferring the microwaves comprises at least two antennas, which are excited in phase by the source in order to obtain a desired heating configuration. More in detail, the heating configuration is made exploiting the principle of interference of coherent electromagnetic waves emitted by each antenna.
In particular, the end of the antenna at which the transmission of microwaves is performed is of the dipolar type, or monopolar, and has a shape selected from the group comprised of:
In particular, the co-axial microwave antenna comprises:
Advantageously, the microwave antenna can furthermore provide:
Advantageously, the reaction container has a housing in communication with the outside that crosses it at least for a part thereof. The housing is suitable for receiving, in use, the above described means for transmission.
In particular, the housing is of dielectric material transparent to microwaves and prevents from a direct contact of the transmission means with the reacting material.
Advantageously, the reaction container has at least one opening through which it is possible to approach the reacting material for arranging means for measurement, for example of temperature and pressure.
In an exemplary embodiment of the invention, the reaction container comprises:
Advantageously, means are provided for modulating the frequency of microwaves to adjust the power transferred to the reacting material responsive to the type of process.
The microwave apparatus, as above described, increases considerably the control, the speed, the selectivity and the stability of the processes. Furthermore, the power emitted by the antenna is adsorbed by the reacting material allowing the operator to work in safety conditions with respect to the emissions of electromagnetic waves. In case of use of high heating power, to avoid residue emissions out of the reaction container, the latter has a shielding layer that is opaque to microwaves, for example, a film, a varnish, or a metal braiding.
According to another aspect of the invention, a method for heating with microwaves a reacting material in chemical-physical processes comprises the steps of:
generating microwaves by a microwave source of power,
The invention will be now shown with the following description of an exemplary embodiment thereof, exemplifying but not limitative, with reference to the attached drawings wherein:
With reference to
The arrangement of antenna 10 in the reacting material 25 provides a quick and effective heating. Furthermore, it is possible to increase considerably the selectivity, the control and the efficiency of the chemical-physical processes to which the heating technique above described is applied. This allows also to provide a considerable energy saving with respect to apparatus of prior art.
Reaction container 3 can be a common container for research laboratories, for example a sphere with three apertures 6a, 6b and 6c (
In case it is necessary to use high power, it is suitable to have reaction container 3 coated with a shielding layer 35, which is next to the external walls 34 of the container 3 (
This allows to an operator to work in safety conditions.
For mixing effectively the reacting material 25, in reaction container 3 a magnetic bar 21 can be put that is wheeled in the reacting material 25 by a mixer 20.
In case of a sphere 3 the apertures 6a, 6b and 6c can be used for arranging sensors 20 that monitor continuously some process parameters, for example the pressure and/or the temperature (
According to an exemplary embodiment of the invention, it is possible to irradiate the reacting material 25 contained in reaction container 3 through a plurality of antennas, for example two antennas 10a and 10b (
In
In
With reference to
The housing 102 is transparent to microwaves, and permits passage of the microwaves into reaction vial 103, without contact between antenna 110 and any liquid or sample present in the vial, permitting re-usage of the antenna for further treatments in similar vials without the need of cleaning it or replacing it.
Of course, the reaction vial, the housing, the plug can be connected and shaped in any desired way alternative to that of
With reference to
The reactor vials on the belt are submitted to a number of automatic and programmable operations under a plurality of stations 171-174 of a treatment unit 175, that is shown only diagrammatically. Under stations 171-174 vial 103 may be added with samples, carrier fluids, chemicals, as well as fluids or treated samples can be removed. At least one of stations 171-174 can provide a microwave source 104.
With reference to
The conveyor 145 can transport a large number of vials enabling automatic activation of chemical reactions at various microwave power level, at different temperatures and using a selected quantity of reactants. A magnetic stirring bar can be provided, not shown.
With reference to
With reference to
If a desired temperature profile 296 has to be achieved in the fluid, like that shown, for example, in
Advantageously, as shown in
In another exemplary embodiment, shown in
The arrangement described in
From nozzle ejector 305 a jet 316 exits of atomic or molecular species excited by the microwaves field emitted by antenna 310 and directed towards substrate 306, which can be of crystal or amorphous material. The co-axial reactor 303 is held by a metal plate 307 equipped with seals that can keep a high vacuum (not shown). The microwaves reactor 303 is contained in a chamber 308, for example cylindrical, of glass or other material compatible with operations under high vacuum, having an outlet 309 for connection to a high speed pumping system, not shown. In this way, in chamber 308 conditions can be achieved of propagation of atomic or molecular species without that they subject to deviations for hits with residue gas particles.
Chamber 308 is held at one end by a plate 307 and at the other end by a plate 310, with high vacuum sealing means, not shown. The plate 310 holds in the chamber 308 the substrate 306. At inlet 304 of reactor 303 the gas or vapour coming from pressurized containers, for example indicated with 311, 312, 313 reach valves 314 and pressure reduction systems 315 for controlling the flow.
The microwave field generated by antenna 310 crosses the gas or vapour in reactor 303 and excites it, with the production of ions, radicals and atomic or molecular species at high production energy level. Directional jet 16, reaches substrate 6 and coats it with a layer whose thickness increases versus time.
The deposition process may provide that substrate 306 is kept heated by a heater, for example electric, operated by conductors 317 and 318. At least one temperature sensor (not shown) can be provided to control the temperature of the substrate during the process to maintain it at a desired temperature.
A magnetic axial field can be provided produced by a winding 319 in which an electric current can be applied through ends 320 and 321, in order to focus the atomic or molecular species having electric charge.
Electrodes 322 and 323 can be arranged in reactor 303 respectively near nozzle 305 and near substrate 6, to provide an electric field parallel to the desired trajectories of the particles in order to boost jet 16, accelerating the particles in a selective way concerning the species having electric charge, increasing the capacity for controlling the process.
For example, the reactor can be used for depositing a layer of nanocrystal, on a wafer of silicon of some cms of diameter brought to the temperature of about 800C. In this case a flow of methane and hydrogen can be used contained for example in containers 312 and 313. The gaseous mixture, when crossing the reactor 3 with a predetermined flow rate, is excited by antenna 310, for example up to a power of about 1 kW at 2450 MHz. In this way, the Carbon atoms produced by molecular dissociation, reach the substrate and deposit on creating a film of nano-crystal diamond.
The foregoing description of a specific embodiment will so fully reveal the invention according to the conceptual point of view, so that others, by applying current knowledge, will be able to modify and/or adapt for various applications such an embodiment without further research and without parting from the invention, and it is therefore to be understood that such adaptations and modifications will have to be considered as equivalent to the specific embodiment. The means and the materials to realise the different functions described herein could have a different nature without, for this reason, departing from the field of the invention. It is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation.
Number | Date | Country | Kind |
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PI2004A000097 | Dec 2004 | IT | national |
PCT/IB2005/003782 | Dec 2005 | IB | international |
This application is a continuation-in-part of U.S. application Ser. No. 11/722,723, filed Jan. 30, 2008, which is a 371 of International application number PCT/IB2005/003782, filed Dec. 14, 2005, which claims priority to Italian Application No. PI2004A000097, filed Dec. 24, 2004.
Number | Date | Country | |
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Parent | 11722723 | Jan 2008 | US |
Child | 13293028 | US |