Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D7/00—Sublimation
  • B01D7/02—Crystallisation directly from the vapour phase
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
  • B01D3/10—Vacuum distillation

Definitions

• the invention relates in particular to a device for evaporating or sublimating a substance with a subsequent deposition of the substance on the gas phase, for example for cleaning or separation purposes ,
• the invention also relates to methods for the gas phase processing of a substance, such as. B.
• Gas phase occurs in materials that can form a crystal structure, for additional purification.
• a conventional sublimation system consists of a multi-zone tubular furnace through which an inner tube passes as a substrate for deposition (see, for example, US 2003/0089305).
• the temperature of the inner tube is adjusted from the outside to provide the desired evaporation or deposition.
• This technique has the advantage of a simple structure.
• the disadvantage is that temperature gradients occur in the inner tube. Accordingly, the composition of the deposited substances also has a gradient.
• the area of the inner tube with the best quality material must be selected. Further disadvantages of this technique are the inaccurate and unreliable temperature control in the heating zones and the low material throughput, which is disadvantageous especially for large-scale technical applications.
• WO 01/70364 proposes the sublimation of organic materials in a three-segment apparatus which is provided by an electromagnetic induction heated Rezi- patient wall.
• the inside of the recipient wall serves as a substrate for the deposition.
• This technique improves the accuracy and reproducibility of the temperature setting.
• the disadvantage is the low material throughput.
• the object of the invention is to provide an improved vacuum device with a deposition device for depositing a substance from the gas phase, with which the disadvantages of the conventional techniques are overcome and which has a broader application.
• the vacuum device should be characterized in particular by an improved temperature setting, the ability to high material throughput and a flexible adaptability to different
• the object of the invention is also in the provision of improved methods for the gas phase processing of substances such. B. for physical cleaning or separation of substances.
• the object is achieved by a vacuum device having at least one deposition device which has a deposition body in the volume of which an inner surface is formed by a plurality of cavities.
• the inner surface of the deposition body serves as a substrate for receiving a substance from the gas phase.
• the temperature of the deposition body is adjustable by a plurality of heating elements, which are in the volume of the deposition Body are arranged evenly distributed.
• the inner surface of the deposition body can be tempered directly with the heating elements.
• at least one extended surface having a predetermined temperature is created directly in vacuum.
• the size of the deposition bodies and their inner surface can be selected depending on the specific application. According to the invention, a high mass throughput is thus made possible, without having to remove restrictions in the accuracy and reproducibility of the temperature setting. According to the invention, in particular the cleaning of medium and large amounts of substances and the direct control and regulation of the deposition temperature on the inner surface of the deposition body is made possible.
• the term "substance” here includes any material that can be deposited thermally by vaporization or sublimation in the gas phase and by condensation from the gas phase.
• the material usually contains several components, of which a pure target substance to be separated or separated from each other The condensation from the gas phase can lead to the solid or to the liquid state.
• “Gas phase processing” of the substance denotes any working or production process in which the substance or one of its components is at least temporarily converted into the gas phase.
• heating element here comprises any component provided in the deposition body which is suitable for direct temperature control of the inner surface of the deposition body, Preferably, the heating elements are firmly embedded in the deposition body. certain distribution of the heating elements be advantageous.
• the heating elements can be fixed as separate components in the deposition body. However, a variant in which the heating elements and the deposition body are formed from a common material is preferred.
• the inner walls of the separator body are used as heating elements.
• This embodiment of the invention has the advantage that the heating elements simultaneously serve as substrates for the deposition of the substance from the gas phase.
• the heat transfer is improved and additional support materials avoided, which could worsen the response to the temperature setting with the heating elements.
• the vacuum device can have a plurality of separation devices with deposition bodies whose temperatures can be set separately. According to the invention, a fractionated separation of various constituents of a substance to be purified or separated is thus made possible.
• the deposition body of the deposition device is thermally insulated in the vacuum device.
• each deposition body of the environment in particular from the walls of the vacuum device or of adjacent parts such. B. from adjacent deposition bodies or other parts of the vacuum device are thermally decoupled.
• the formation of the temperature gradients occurring in the conventional techniques is avoided, so that the selectivity of the deposition of various constituents of the substance to be processed is increased.
• the thermal insulation of the deposition bodies is achieved by being surrounded on their sides towards the wall of the vacuum device by free spaces which, depending on the operating mode of the vacuum Device evacuated or filled with inert gas.
• the mechanical support of the deposition body is made by guide elements made of a material with low thermal conductivity such. B. ceramics.
• advantages of the invention include the ability to choose the material of the deposition body depending on the desired application.
• the deposition body is made of a metal, e.g. As tungsten, tantalum, molybdenum, copper, gold, silver or stainless steel (eg., Stainless steel foam)
• tungsten tungsten
• tantalum molybdenum
• copper gold
• silver stainless steel
• the deposition body is made of a ceramic, in particular advantages for the thermal stability of the deposition body can result.
• ceramics are often particularly suitable as inert substrates for organic substances.
• Preferred ceramics include silicon carbide, boron nitride, alumina, boron nitrite titanium diborite, and aluminum nitrite, or combinations thereof. Further advantageous modifications consist in providing a composition of one or more metals or several ceramics for forming the deposition body. In each of the cases mentioned, or even when using other materials for producing the deposition body, its inner surface may be provided with an inert coating (eg enamel) in order to avoid interactions in the substance to be processed with the deposition body. Furthermore, the radiator may contain graphite or consist entirely of graphite. In the first case, for example, a composition with a graphite-coated ceramic or with a ceramic, in which graphite is embedded, may be provided.
• the heating elements are designed for active heating of the deposition body.
• the heating elements are directly applied with an electric current to convert directly electrical energy into thermal energy.
• This embodiment of the invention has particular advantages in terms of rapid response of the temperature setting.
• the heating elements can, for. B. connected directly to at least one power source.
• actively operating heating elements can be induction elements in which a current flow is induced by an external electromagnetic action.
• the at least one deposition body of the vacuum device according to the invention has a three-dimensional internal structure, through which cavities and the inner surface are formed.
• the internal structure may vary depending on the amount of material to be deposited or the desired one
• deposition bodies Shaping the deposition body to be selected.
• Particularly preferred are deposition bodies in which the inner cavities are formed by pores, lamellae (parallel partitions, optionally with webs), honeycombs, open-pore foam, a composition of fibers or a combination of these structures.
• the internal structure of the deposition body can be freely dimensioned depending on the conditions of a concrete Abscheidungsaufgäbe.
• As the pores can be selected depending on the phase behavior of the coating material and the desired deposition amount.
• the inner structure is dimensioned such that capillary forces lead to the homogeneous retention of the material in the deposition body. Accordingly, it may be advantageous if the cavities of the radiator in at least one spatial direction have a characteristic size in the range of 1 micron to 1 mm.
• the appropriate dimensioning of the internal structure may be selected by one skilled in the art depending on the deposition conditions. For the separation of materials which have the liquid phase during the deposition, additional liquid lines and / or collecting vessels can be provided in the vacuum device.
• the deposition body according to a variant of the invention has the lamellar structure, which is formed by thin-walled, planar lamellae, there are advantages for the deposition of the substance from the gas phase.
• the inner surface of the deposition body is essentially a flat surface, through which a homogeneous deposition and in particular a crystallization during the deposition is promoted.
• the vacuum device has a plurality of deposition devices, these are preferably all equipped with a lamellar ⁇ structure. This provides advantages for the substance transport in the gas phase through the deposition bodies reached. Directed gas phase flow can pass between the deposition bodies without hindrance.
• the inner fins of the deposition body are inclined relative to its outer surface.
• Adjacent deposition bodies are preferably arranged such that the inclination of the respective slats is oriented differently. Thereby, a free passage of a gas phase flow along a reference direction formed by the juxtaposition of the deposition body can be avoided.
• the at least one deposition body is equipped with a detachable electrical connection.
• the detachable electrical connection is preferably a plug connection, the parts of which can be connected to one another or separated from one another by a deformation of a wall region of the vacuum device which is dependent on the internal pressure of the vacuum device.
• the deformable wall portion In the evacuated state of the vacuum apparatus, the deformable wall portion is displaced towards the inside of the vacuum apparatus under the effect of an external pressure (atmospheric pressure), so that the part of the plug connection disposed in the wall portion joins with the other part of the plug connection provided on the deposition body comes into contact.
• the deformable wall region is preferably a bellows.
• the vacuum device according to the invention can generally be connected via a heated steam line to a reservoir of the substance which is to be processed, in particular to be separated.
• a heated steam line to a reservoir of the substance which is to be processed, in particular to be separated.
• an evaporator device is provided for transferring the substance into the gas phase in the vacuum device according to the invention.
• this creates a compact construction with the evaporator and separation devices.
• a cold trap device is furthermore provided in the vacuum device in order to collect volatile constituents of the substance to be processed.
• impurities in the deposition of substances in the deposition bodies can thus be avoided.
• the separation device and at least one of the evaporator device and the cold trap device are constructed as modules which can be separated from one another.
• Each module consists of a module housing and a arranged in this inner component te, such.
• the module housings of the individual devices form the recipient wall of the vacuum device.
• the modules can be arranged vacuum-tightly adjacent to one another.
• a modular system is provided which allows any extension or modification required for the actual application of the invention and which, for example, serves to process larger quantities of material or more fractions, e.g. B. to be able to clean or separate or to provide for various materials that are part of the substance to be revised, optimal internal surfaces and geometries for deposition.
• the modular vacuum device is created in particular for cleaning various, even larger amounts of a material by fractional evaporation with simultaneous recrystallization with defined adjustable and controllable temperatures on the inner surfaces of the deposition body.
• the vacuum device according to the invention is particularly well suited for the purification or separation of organic materials and in particular organic dyes or other organic substances which have solid state semiconductor properties.
• the vacuum device according to the invention can be equipped with a plurality of modules, each with a deposition body whose temperature is set for deposition of the respective desired component.
• the vacuum device may be designed for a material throughput of a few grams to a few hundred grams or more.
• the modular design also allows the constant adaptation of the Abscheidungskör- to a variety of tasks and the use of experimental bodies, eg. B. with an internal gradient structure for the investigation of the deposition behavior of substances.
• the modules of the depositing means on the one hand and the evaporator means and / or the cold trap device are 'on the other hand, arranged above one another as a stack.
• the stack construction is advantageously easy to operate.
• the modules may be arranged in accordance with the moving direction of the substance in the gas phase by the convection given in the vacuum device.
• the module of the evaporator device is initially provided on the bottom, above which the separation device (s) are provided with one or more modules corresponding to one or more deposition bodies and at the top the cooling trap device with the cold trap.
• the module housings of the individual modules preferably all have the same shape. Particularly preferred is a shape with a circular cross section, so that the modules can be arranged in each case in the form of a cylinder jacket fitting over each other.
• the individual modules of the vacuum device are gas-tight in the operating state of the vacuum device and in particular vacuum-tightly connected to each other.
• known per se screw or clamp connections can be provided at the edges of the modules.
• an embodiment of the invention is particularly preferred in which the module housings of the modules in the evacuated state of the vacuum device are pressed against each other in a vacuum-tight manner by the action of the external pressure.
• the vacuum device can be easily assembled by stacking the modules and adapted to the current task before startup and before evacuation. In order to produce a vacuum-tight bond, the assembly must then be evacuated from the modules (with end plates at the top and bottom sides).
• a separator device is provided between the evaporator device and the deposition device.
• the separator device may simply be formed by a substantially empty module housing which is inserted between the modules of the evaporator and separator devices.
• the module housing only contains a ring of a material with low thermal conductivity as a support for the deposition body arranged above.
• at least one radiation shield can be provided in the separation device, with which heat radiation from the evaporator device to the deposition device is reduced. With the separator device, the accuracy of the temperature adjustment in the lowermost deposition device is improved.
• this device is equipped with a sensor device which makes it possible to monitor the deposition process and / or the yield of the precipitate.
• the sensor device preferably contains at least one of the following sensors. If at least one temperature sensor is provided, the temperatures in the deposition bodies or other parts of the vacuum apparatus may be continuously measured and used to control a cleaning or separation operation. When providing at least one mass sensor, the material throughput can be monitored continuously and the temperature control of the evaporator and / or deposition devices can be controlled. Finally, the provision of at least one chemical sensor of Vor ⁇ be part to the occurrence of volatile substances such. As solvents or gases (eg., Oxygen, nitrogen substance or water) and the components of the substance to be processed.
• solvents or gases eg., Oxygen, nitrogen substance or water
• the o. G. Problem solved according to a further aspect of the invention by a method for gas phase processing of a substance, wherein the substance or components thereof is deposited from the gas phase in at least one deposition body used in the invention.
• the heating elements With the heating elements, the temperature of the inner surface of the at least one deposition body is adjusted so that the substance or the respective component is deposited on the inner surface.
• Other constituents of the vaporized substance which do not condense at the set temperature remain in the gas phase.
• a stationary temperature adjustment is carried out for the separation of certain substances or certain constituents of a substance mixture at a respective deposition body.
• a temperature adjustment takes place with a temperature profile that changes as a function of time (variable operation).
• variable operation according to a preferred embodiment of the invention, an adjustment of temperatures or of specific time profiles depending on the signals of the sensor device can be provided. This allows the targeted driving through temperature regime, such. B. temperature ramps for optimal control of the cleaning process and the yield.
• Another object of the invention is the use of the vacuum device according to the invention for the purification or separation of organic materials. Further details and advantages of the invention will be described below with reference to the accompanying drawings. Show it:
• FIG. 1 shows a schematic sectional view of a preferred embodiment of the vacuum device according to the invention
• FIG. 2 shows a cross-sectional view of a module of the deposition device provided according to the invention
• Figure 3 is a plan view of a deposition body used in an embodiment of the invention.
• FIG. 4 shows a sectional view of the deposition body shown in FIG. 3;
• FIG. 5 shows an illustration of the plug connection for the detachable electrical connection of a deposition body.
• a preferred embodiment of the invention comprises a combination of at least one deposition device with deposition bodies used according to the invention with an evaporator device and a cold trap device in a vacuum device.
• the illustrated combination is not necessarily intended to practice the invention.
• Objects of the invention are also constructed according to vacuum devices, the only a separation device z. B. with single deposition body or containing only the combination of a deposition device with an evaporator device.
• vacuum device generally refers to any outwardly gas- or vacuum-tight apparatus that can be evacuated or filled with an inert gas.
• the vacuum device contains components which are known from vacuum technology, such as vacuum gauges or venting valves, which are not used here Individual will be described.
• FIG. 1 shows the cross-sectional view of the vacuum device 100 according to the invention with an evaporator device 10, a separator 50, two deposition devices 20.1, 20.2, each having a deposition body 21, 22, a cold trap device 30 and a sensor device 40.
• Each of these devices has a module housing 60 in shape a cylinder jacket with lower and upper projections 61, 62 on.
• the module housings 60 form a stack which is closed at the bottom by a lower end plate 71 and at the top by an upper end plate 72.
• a vacuum flange 73 is provided to which a vacuum pump 74 is connected.
• the vacuum pump 74 comprises a per se known vacuum pump system, which preferably produces a hydrocarbon-free vacuum in the technical sense, such.
• B. a turbomolecular pump or a diaphragm pump.
• the vacuum pump maintains a working pressure below 10 "5 mbar.
• the module housings 60 each contain an inner part which fulfills the function of the corresponding module. Between the superimposed inner parts (for example, separating bodies 21, 22) are spacers 67, which are the same early thermal insulation of the internal parts with each other and their mechanical coupling serve.
• the module housing 60 are constructed substantially identical.
• the lower projection 61 of a module housing 60 rests in each case on the upper projection 62 of the module housing 60 arranged underneath.
• the lower projection 61 rests on a correspondingly shaped step on the lower end plate 71.
• the module housing 60 the evaporator device
• thermocouple In the module housing 60 are all electrical or material flows through connections, such. B. the shown in Figures 2 and 5 in more detail electrical connection 65 or the coolant line 66 for the cold trap device 30 is arranged. A separate terminal in the module housing 60 may further be a flange for passing a thermocouple.
• the module housing 60 shown in Figure 1 each have a height of approx. 5 to 15 cm and an inner diameter of approx. 5 to 30 cm up.
• the inner parts have a square cross-section with a diagonal slightly smaller than the inner diameter of the module housing 60, and a height which is the height of the module housing 60 minus the thickness of the spacers 67, the simultaneous thermal insulation of the inner parts and their mechanical Serve coupling.
• the inner part is arranged in each case. 2 schematically with a square transverse
• the inner part shown in FIG. 1, for example the deposition body 21, is arranged separately from the inner wall of the module housing 60 and thereby thermally separated from the module housings 60 in the evacuated state by the evacuated space.
• radiation shields may be provided between the inner portion and the module housing 60 for thermal isolation (not shown).
• the mechanical adjustment of the inner part within the module housing 60 is performed by guide elements 66 made of a material with low bathleit- ability, z. B. a ceramic.
• the guide elements 66 are, for example, rails. They allow the internal parts as needed, for. B. for filling or for removal can be easily removed from the module housings 60.
• the evaporator device 10 includes an evaporator 11.
• the evaporator 11 is a thermal evaporator with a heater such. B. with a directly heated cuvette or with a heater which is described in unpublished patent application DE 10 2005 013 875.6.
• the separator 50 merely includes a ring 51 of a low thermal conductivity material, e.g. As a ceramic, which rests on the upper side of the evaporator 11 and the upper side forms a support for the Abscheidungs- body 21 of the deposition device 20.
• the ring 51 serves for the thermal decoupling between the evaporator 11 and the lower deposition body 21.
• sieves for capturing unwanted evaporation products such as e.g. B. flakes may be provided.
• the deposition devices 20.1, 20.2 comprise two modules corresponding to two deposition bodies 21, 22, whose inner structure is layered Includes cavities between slats shown schematically.
• the fins are inclined relative to the vertical axis of the vacuum device 100, as will be explained in more detail below with reference to Figures 3 and 4.
• Each deposition body 21, 22 contains homogeneously distributed heating elements (not shown), which can be acted upon via an electrical connection 65 (see FIG. 2) with a heating current.
• the cold trap device 30 includes a known per se
• Cooling trap 31 which is cooled, for example. With tap water or other coolant.
• a mass sensor 41 is arranged, which serves to measure a deposition rate and z.
• B. contains a vibrating beam thickness gauge.
• FIGS. 3 and 4 show further details of the deposition body 21 in plan view (FIG. 3) and in a sectional view along the line IV-IV (FIG. 4) shown in FIG.
• the deposition body 21 comprises a closed outer wall 23 and fins 24 in which heating elements 25 are arranged.
• the lamellae run obliquely from the underside 26 of the deposition body 21 to its upper side 27. Between the lamellae 24, cavities 28 are formed.
• the surfaces of the fins 24 form the inner surface of the Abscheidungskör- pers 21 and thus the substrate for receiving the substance from the gas phase.
• a gap 29 is provided which contains an opening which extends from the underside 26 to the upper side 27.
• the heating elements 25 can be connected to an external power source (not shown) via the electrical connection 65 illustrated in FIG.
• the heating elements 25 comprise, for example, a Resistance heating insulated from the lamellae 24 (eg heating wires from Kantal, product designation).
• the side length a of the outer walls 23 is z. B. 10 cm, while the height b of the deposition body 21 rd. 6 cm.
• the thickness of the fins 24 is z. B. 6 mm.
• the slats consist z. B. of copper or stainless steel.
• a surface coating z. B. be provided from Ni, ceramic or enamel.
• a quantity of up to 100 g of an organic material such.
• B. Alq3 (tris) 8-hydroxyquinoline) aluminum are deposited.
• the deposition bodies 21, 22 arranged one above the other according to FIG. 1 are arranged in such a way that the inclination of the slats 24 points in different directions, it is advantageously achieved that, apart from the intersection of the slit 29, no continuous gas phase flow through the deposition bodies 21 22 can be made.
• the substance flowing in the gas phase from the evaporator 11 thus impacts with great effectiveness on the inner surface of the deposition bodies 21, 22.
• the electrical connection 65 comprises a plug connection with a socket 65. 1 on the side of the deposition body 21 and plug contacts 65. 2, which are connected to electrical leads leading to the outside.
• the socket 65.1 and the plug contacts 65.2 form a detachable plug connection, which is decided as follows only in the evacuated state of the vacuum device 100.
• FIG 5 three lines are shown.
• a passage for a thermocouple or another temperature measuring device may be provided.
• venting causes the spring force of the spring bellows 69 releasing the contacts, so that the inner elements such. B. the deposition body 21 can be easily removed.
• the lines each contain a spring area 65.3.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Crystallography & Structural Chemistry (AREA)
• Physical Vapour Deposition (AREA)
• Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Priority Applications (3)

Applications Claiming Priority (1)

Publications (1)

Family

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Family Applications (1)

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Cited By (2)

Citations (5)

• 2005
  • 2005-04-19 WO PCT/EP2005/004175 patent/WO2006111180A1/de active Application Filing
  • 2005-04-19 DE DE112005003542T patent/DE112005003542A5/de not_active Withdrawn
• 2006
  • 2006-04-18 TW TW095113727A patent/TW200710237A/zh not_active IP Right Cessation

Patent Citations (5)

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