• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a device for depositing a material layer on a sample within a vacuum chamber, comprising a sample table (100) for arranging at least one sample (103a, 103b, 103c, 103d), an evaporation source (101, 201) connected to a power source for a thread-like evaporation material (102, 202), a quartz crystal (105) for measuring the deposited material layer thickness, and an evaluation device (113) associated with the quartz crystal (105), wherein the evaporation source (101, 201) is associated with an electronic control unit (112) which is associated therewith is arranged to supply to the evaporation source (101, 201) the electric current provided by the current source in the form of at least two current pulses with a pulse length of <1 s, and that the evaluation device (113) is adapted to control the transient decay behavior of the quartz crystal (105) immediately after completion of a current pulse to divert the deposited after each current pulse to consider the material layer thickness. The invention further relates to a method which can be carried out with this device.
    公开号:AT512949A1
    申请号:T50219/2012
    申请日:2012-06-04
    公开日:2013-12-15
    发明作者:Paul Wurzinger；Anton Lang；Felix Redl
    申请人:Leica Microsysteme Gmbh；
    IPC主号:
    专利说明:

    P12609
    COATING METHOD MH AN EVAPORATIVE MATERIAL
    The invention relates to a device for depositing a material layer on a sample within a vacuum chamber, comprising a sample table for arranging at least one sample, an evaporation source connected to a power source for a thread-like evaporation material, a quartz crystal for measuring the deposited material layer thickness, and an evaluation device associated with the quartz crystal , The invention further relates to a method which can be carried out with this device.
    The vaporization of thin filamentous evaporation materials by electric current heating in a vacuum evaporation apparatus has been used for a long time to coat electron microscopic substrates and sample preparations. Prior to examination in a scanning electron microscope (SEM), non-conductive samples and materials are coated with a conductive material, usually gold or carbon. The known method of carbon filament evaporation is widely used in electron microscopy, in particular in the production of impression and amplification films for transmission electron microscopy and very thin conductive surface layers for scanning electron microscopic samples. In the X-ray microanalysis performed in the SEM, which includes the energy dispersive X-ray analysis (EDX) and the wavelength dispersive X-ray analysis (WDX), the samples are previously vapor-deposited with a very thin layer of carbon. Furthermore, the E-lectron Backscatter Diffraction (EBSD) method, a crystallographic technique used in scanning electron microscopy, also requires a very thin layer of carbon deposited on the sample.
    Vacuum evaporation devices for thermally evaporating filamentary evaporation materials, as known in the art, typically include a vacuum chamber in which a sample receiving / sample table with the sample to be coated and an evaporation source connected to a power source are arranged. The samples are vapor-deposited vertically or obliquely with the vaporized material impinging on the surface of the sample mounted horizontally at a predetermined angle to the horizontal plane. -2- P12609
    The flash-like evaporation (also known as "flash method" or "flash evaporation") of a thin carbon filament by heating with high current flow is commonly used for coating preparations and is characterized by ease of handling and low thermal stress of the sample. The lightning-like evaporation often leads to the sudden tearing of the carbon filament remainder. In this case, undiluted fibers and particles can reach the sample and pollute it. In addition, the layer thickness and the layer thickness distribution are determined by the geometric relationships between sample and evaporation source and the thread thickness and can be varied only to a limited extent by the use of different thread sizes and the variation of the distance between the evaporation source and the samples. Another disadvantage of the flash method is that the carbon thread breaks and has to be replaced by a new carbon thread. Such changes are time-consuming and lead to a lower equipment utilization, lower sample throughput and consequently a lower W wirtschaftlichkeit.
    In modified methods, the current flow is limited in time (pulsed), so that not all the carbon filament is evaporated during a pulse. The pulses are thereby limited by short manual switching or by electronic control. In order to evaporate the entire coal thread section, several pulses are usually required. In the pulsed process, the actual evaporated volume of the carbon thread can vary greatly, since different thread sections develop different resistance values after partial evaporation. Since in the pulsed process, the carbon thread does not crack and remains mechanically stable, the amount deposited is lower than in the flash method. In addition, the deposited amount varies per pulse, since the carbon filament less heated with increasing resistance. If the pulses are switched manually, the temporal variation of the pulses is added. Therefore, only poorly defined layer thicknesses can be obtained with the hitherto known processes based on current pulses.
    The measurement of the layer thickness of a deposited layer with the aid of a quartz crystal has also long been known, in particular the sensitivity to environmental influences such as temperature, occupancy of the surface with condensable substances, mechanical stress uneven heating, etc., affecting the accuracy of measurement. The quartz crystal layer thickness measurement is strongly affected by the radiation (light and heat) emitted by the carbon filament during evaporation -3- P12609
    Due to these facts, the coating thickness measurement by means of quartz crystal in a Kohleverdampfungsver drive is therefore applicable at most for checking the reproducibility, but not for accurate measurement of the deposited layer thickness or to limit the coating process.
    The layer thickness, the homogeneity and the electrical conductivity of a carbon layer are of utmost importance for electron microscopic applications. It is therefore essential for most electron microscopic applications that the coatings deposited on the electron microscopic substrates and sample preparations must not exceed or fall short of a predetermined thickness. Insufficiently controlled material deposition and resulting non-uniformity of the layer thickness have a significant effect on the quality of the sample preparation and consequently on the quality of the image resolution. A reproducible layer thickness with highest accuracy is particularly desirable in combination with REM in the EDX / WDX or EBSD analyzes mentioned above.
    It is therefore an object of the invention to improve the above-described methods of filament evaporation so that their advantages such as ease of use and low thermal stress of the samples are retained, the well-known from the prior art disadvantages such as susceptibility to fouling and inaccurate layer thickness measurement, however be eliminated. It is another object of the invention to provide an apparatus for carrying out the improved evaporation method.
    This object is achieved with a device for depositing a material layer on a sample within a vacuum chamber as mentioned above, wherein the device is characterized in that the evaporation source is associated with control electronics, which is adapted to the evaporation source provided by the power source electrical Current in the form of at least two current pulses with a pulse length of &lt; 1 s, and that the evaluation device is adapted to take into account the transient decay behavior of the quartz crystal immediately after completion of a current pulse for deriving the deposited after each current pulse material layer thickness. -4- PI2609
    This object is further achieved by a method for depositing a layer of material on at least one sample within a vacuum chamber, the method being characterized by the steps of: vaporizing at least a portion of filamentary evaporation material by heating by means of electric current, wherein the stream is exposed to the filamentary evaporation material in FIG at least two current pulses with a pulse length of &lt; 1 s, the current pulses being selected such that the filamentary evaporation material does not rupture, measuring the material layer thickness deposited after a current pulse by means of a quartz crystal, taking into account the transient decay behavior of the quartz crystal immediately after completion of a current pulse.
    Thanks to the invention, a well-defined variation of the layer thickness is possible by measuring the layer thickness of the vaporized material deposited with each current pulse. The influence of the signal of the measuring quartz during the current pulse by the radiation (light and heat) is considered according to the invention for the accurate measurement of the layer thickness. In this way, the thickness of the deposited during a pulse layer can be determined with high accuracy and the desired total layer thickness can be adjusted. With the invention, layers can be obtained in a wide range of thicknesses, starting with very small layer thicknesses of less than 1 nm up to large layer thicknesses of 20 nm or more in a small tolerance band. Until the end of the process when the desired total layer thickness is reached, the determined gaps of the individual layers are added up. Furthermore, the invention allows a better reproducibility of the coating.
    Since the current pulses are chosen so that the thread-like evaporation material does not crack, the risk of contamination can be excluded in comparison to the flash method described above. The selected pulse data depends on the thread material used. They can be determined by simple routine tests, depending on the deposition thickness desired per pulse. One skilled in the art will also have no difficulty in translating data known in other similar methods to the disclosed method. -5- PI2609
    The term "filamentous evaporation material" refers to all filamentary materials suitable for thermal evaporation in a vacuum evaporation direction and known to those skilled in the art. The vaporization material may be, for example, carbon (graphite) or tungsten, but all materials, metals and alloys which develop a substantial vapor pressure in solid form (e.g., silver) are contemplated.
    The method and the device according to the invention are particularly advantageous for applying a carbon layer of well-defined thickness to an electron microscope specimen, in particular for applying very thin carbon layers with an accuracy of approximately 0.5 nm, as used for X-ray microanalysis (EDX / WDX ) or the EBSD analysis in combination with REM are necessary. In a preferred embodiment of the invention, the thread-like evaporation material is therefore a carbon thread (graphite thread). In particular, it is possible to use twisted or braided carbon filaments having a thickness of 0.2 g / m to 2 g / m.
    The process is typically carried out under vacuum, the vacuum preferably being better than 1 × 10 -2 mbar. Preferably, the at least one sample is an electron microscopic sample preparation.
    In principle, all oscillating crystals commonly used for layer thickness measurements can be used (eg orientation labels "AT", "SC", "RC") using appropriate holding devices known per se to those skilled in the art. Preferably, quartzes of orientation AT are used, since they have the best temperature behavior at room temperature and do not have to be kept at an elevated temperature. The Quarzplättehen preferably have a diameter of about 14mm, a thickness of about 0.2mm and are metallized on both sides.
    In a preferred variant of the method, the measurement of the material layer thickness takes place immediately after the end of each current pulse. This is particularly advantageous for thinner layer thicknesses with high accuracy and a low tolerance band in the layer thickness distribution. -6- PI2609
    In a further variant of the method, in the production of thick layers, the layer thickness measurement can also take place after several pulses, whereby the overall process is accelerated.
    According to the invention, the transient decay behavior of the quartz crystal after completion of a current pulse when measuring the deposited material layer thickness is taken into account. In a first preferred embodiment, before the measurement of the material layer thickness, the decay of the signal of the quartz crystal to a base level is awaited. This base level is usually reached 4 to 5 seconds after completion of the current pulse. Expediently, the material layer thickness is determined from the difference between the base level of the quartz crystal signal before deposition of the material layer and the base level of the quartz crystal signal after deposition of the material layer. Typically, a quartz oscillates at a frequency of 5 to 6 MHz. The deposition of material on the quartz crystal surface causes a change in the resonant frequency. The difference between the base level of the quartz crystal signal before depositing the material layer and the base level of the quartz crystal signal after depositing the material layer is in the Hz range, e.g. For example, the measured difference for a 1 nm thick carbon layer is typically about 15 Hz.
    As an alternative to the above-mentioned embodiment, in another advantageous embodiment, the evanescent signal of the quartz oscillator is adjusted by an appropriate function (exp ^) and in this way a sufficiently accurate measurement is already achieved during the decay time. The material layer thickness is thus measured using the following steps: measuring the course of the frequency of the quartz crystal as a function of time adjusting a parameterized function that is parametrized with at least one parameter to this profile, and deriving a material layer thickness the at least one parameter.
    The parameter to be adjusted is in a clear functional relationship with the basic level to which the transient decay behavior points, preferably a proportionality. As a further parameter, the time constant of the decay process can be adjusted. -7- PI2609
    The control electronics sends current pulses through at least a portion of the thread-like evaporation material in order to heat it so that the material evaporates from the thread and precipitates as a layer on the sample. The current pulses are selected so that the thread section only partially evaporates and in no way ruptures , Furthermore, the current pulses are selected so that at least two current pulses can be carried out per thread section before the resistance of the thread has become so high due to evaporation of the evaporation material that the current flow is no longer sufficient for further evaporation. Advantageously, the pulse length of a current pulse is 20 ms to 1 s, preferably 50 ms to 500 ms. The current intensity of a current pulse is advantageously chosen so that it is 6 A to 50 A. A well-known variety of electronic control devices for generating current pulses with the pulse data mentioned above is available to the person skilled in the art. The control electronics expediently regulate the current through current limitation when a maximum voltage is applied, through direct current regulation or through adaptive adaptation of the voltage to the resistance measured in the preceding current pulse.
    The control electronics are preferably capable of controlling the flow of current to solid state devices, e.g. Power semiconductor transistors, even at full power to measure directly, to control and / or to switch and can mechanical switching elements, e.g. Power relays, do without.
    In one aspect of the invention, the layer inhomogeneities determined by the vaporization geometry are compensated by changing the positioning of the at least one sample with respect to its position relative to the filamentary vaporization material to be vaporized, which is contained in the vaporization source. This is particularly advantageous when two or more samples are in the recipient at the same time and are processed. In a subaspect, changing the positioning of the at least one sample preferably takes place between two successive pulse pulses. Thus, the one or more samples are shifted for each current pulse so that the determined by the evaporation geometry layer distribution is compensated. As a result, a very uniform and well-defined layer thickness is achieved even with very thin coatings. This is of particular importance in the case of the above-mentioned X-ray microanalysis (EDX / WDX) and the EBSD analysis in combination with SEM. In addition, in this process variant, more than one sample can be simultaneously provided with a uniform material coating, thereby achieving higher efficiency and better equipment utilization. In order to determine the layer thickness exactly, the geometric relationships are taken into account and the layer effectively deposited on the samples is calculated on the basis of the layer thickness measured with the quartz crystal. The ratio of the distances between sample and carbon filament or quartz sensor and carbon filament (essentially square spacing law) and the inclination of the quartz sensor to the source (cos law) are taken into account. Preferably, a measured tabular function or a function parametrically corrected for certain positions in relation to the above-mentioned laws, which is determined by measurement, finds application, since shading and reflection effects can also be taken into account in this way.
    In order to achieve the above-described aspect of compensating for the layer inhomogeneities by changing the positioning of the at least one sample with regard to its position to the filamentary evaporation material, the at least one sample in the device according to the invention is received on a motorized movable sample table Sample table for positioning the at least one sample with respect to the position of the evaporation source designed as a motorized movable shuttle table. In a sub-variant of the sample table comprises a turntable rotatable about a Ehehachse, wherein at least two samples are arranged on the rotatable turntable. Preferably, the samples are offset by the same angle to one another on the turntable. In another variant, the samples are arranged only on one segment of the turntable. Preferably, the quartz crystal is arranged in the center of the turntable.
    In one embodiment, the evaporation source comprises a holder for the filamentary evaporation material having at least two electrical feedthroughs. The electrical feedthroughs are controlled by the control electronics, so that the thread-like evaporation material, which is accommodated between the electrical feedthroughs in the recipient, is heated by the released current pulses and thereby evaporated. When coating several samples or when applying thicker layer thicknesses, the material deposited by only one thread section can be too small. To be able to evaporate more than one thread section, it is advantageous if the holder for the filamentary evaporation material comprises at least three, preferably at least five electrical feedthroughs With at least five electrical -9- PI2609
    Bushings can be provided at least four thread sections. In each case, the control electronics control an adjacent pair of bushings, so that in each case only the thread section, which is received between the pair of bushings, is supplied with current and evaporated. If the resistance of a thread section has become so high due to evaporation of the material that the flow of current is no longer sufficient for further evaporation, the sample table is typically readjusted in order to correct the geometric offset of the two thread sections. Alternatively, the holder of the evaporation source can be arranged displaceably in the recipient.
    Preferably, at least one of the at least one sample is disposed at a distance of 30 mm to 100 mm from the evaporation source. The at least one sample is recorded on the sample table in a suitable sample receptacle known to a person skilled in the art.
    In the following the invention together with further advantages will be explained in more detail by way of non-limiting example, which is illustrated in the accompanying drawings. The drawings show in
    Fig. 1 is a schematic representation of an arrangement with a device according to the invention associated motorized sample stage, which is arranged eccentrically to a source of evaporation
    2 shows a vaporization source with five electrical feedthroughs for a total of four carbon fiber thread sections,
    3 is a schematic representation of the arrangement of FIG. 1 arranged in a recipient,
    4 shows a transient decay function of a quartz crystal, and
    FIG. 5 is a flowchart illustrating a process sequence for carbon fiber evaporation coating. FIG.
    Fig. 1 shows a schematic representation of an arrangement with a device according to the invention associated motorized sample table 100, which eccentric to a -10- PI2609
    The sample stage and the evaporation source 101 in the recipient 111 (shown in FIG. 3) can be arranged in a manner known per se in the recipient 111 by means of a hinged shutter (not shown), spatially separated from one another. wherein the evaporating of the carbon thread, the hinged panel is folded away. The sample table 100 and the evaporation source 101 are arranged in a recipient 111, in which after its evacuation a vacuum of better than lxlO-2 mbar prevails. On the sample table 100, electron microscopic samples / preparations 103a-d are positioned in sample holders (not shown). The samples 103a-d are located at a distance of 30 mm to 100 mm from the evaporation source 101. The evaporation source 101 shown in FIG. 1 comprises two electrical feedthroughs 104a, 104b, which are controlled via control electronics 112 (see FIG. 3), so that the carbon filament 102 received between the electrical feedthroughs 104a, 104b can be heated by high current and thereby evaporated.
    FIG. 2 shows a further embodiment of an evaporation source 201 with five electrical feedthroughs 204a-e. The evaporation source 201 may be used as an alternative to the evaporation source 101 shown in FIG. Between the electrical feedthroughs 204a-e, a carbon filament 202 is threaded through. This results in the example shown a total of four coal filament sections, wherein the control electronics in each case an adjacent pair of bushings 204a-e drives, so that only one thread section is energized and evaporated. The evaporation source 201 is preferably arranged so displaceable in the recipient that the respective thread section to be evaporated is positioned at a suitable distance from the sample in an evaporation position. When the resistance of one thread section has become so high due to evaporation of the material that the flow of current is no longer sufficient for further evaporation, the thread section 201 or sample table 100 can then be moved in a motorized manner in an advantageous embodiment the geometric offset of the thread sections can be compensated.
    Returning to FIG. 1, in the immediate vicinity of the samples 103a-d, a quartz crystal 105 is arranged in the center of the sample table 100 with which the thickness of a deposited layer can be determined by changing the resonance frequency. The -11- PI2609
    Oscillating quartz is realized, for example, as a fitted with a suitable quartz plate probe. Preferably, it is a quartz plate with AT orientation. The measuring head can also be arranged in another geometrically favorable position, e.g. immediately adjacent to the outer circumference of the sample table, if the center of the table is needed to hold samples.
    The control electronics 112 sends current pulses through the carbon filament 102 in order to heat them so that the thread section only partially evaporates and in no way ruptures. In the example shown, the pulse data are chosen so that at least 2, preferably more, current pulses can be carried out per thread section before the resistance of the thread has become so high due to evaporation of the evaporation material that the current flow is no longer sufficient for further evaporation. The pulse data are dependent on the thread material used and include pulse lengths of 20 ms to 1 s, preferably 50 ms to 500 ms, and currents of 6 A to 50 A. The control electronics 112 can be the current through current limitation when applying a maximum voltage, by direct current control or by adaptively adjusting the voltage to the resistance measured in the previous pulse.
    The sample table 100 is embodied as a motorized movable changeover table and comprises a rotary disk 106 which rotates about an axis of rotation L and which is rotatably mounted on an axis 108 by means of a bearing 107 in the recipient 111. The samples 103a-d are preferably arranged at equal angles to one another on the rotary disk 106, but the function of the disclosed method is also ensured in the case of irregular or stochastic arrangement of the samples. The turntable 106 is movable via a drive ratio 110 by means of a motor 109. As a result of the rotational movement, the positions of the samples 103a-d with respect to the evaporation source 101 can be changed, so that the layer distribution determined by the evaporation geometry is compensated. In this way, a larger number of samples can be uniformly coated with a coating of well-defined layer thickness. Changing the positioning usually takes place after each current pulse. The pulse data are expediently chosen such that so many current pulses are carried out per thread section that each of the samples arranged on the rotary disk 106 is vapor-deposited by the same number of current pulses. -12- PI2609
    FIG. 3 shows a schematic representation of the arrangement from FIG. 1, wherein the sample table 100 and the evaporation source 101 are arranged in a recipient 111. The two electrical feedthroughs 104a, 104b are controlled by an electronic control unit 112, so that the carbon filament 102, which is received between the electrical feedthroughs 104a, 104b, can be heated by high current and thereby evaporated. Furthermore, the motor 109 is also controlled by the control electronics 112 in order to position the samples arranged on the motorized movable sample stage 101 as described above for the evaporation source 101. The deposited material layer thickness is determined by means of an evaluation device 113, the transient decay behavior of the quartz crystal 105 being considered in detail as described below in FIGS. 4 and 5. The signal connections between the individual components are shown as dashed lines. FIG. 4 shows a decay function of a quartz oscillator, in which the frequency deviation is shown integrated over the gate time versus the offset (ms) of the gate time to the current pulse. The decay function shown in Fig. 4 was recorded with a quartz crystal having an AT orientation. Typically, a quartz oscillates at a frequency of 5 to 6 MHz. The deposition of material, in the example shown carbon, there is a change in the resonant frequency of the quartz crystal. The difference between the base level of the crystal quartz signal detected before deposition of the carbon layer and the base level of the crystal oscillation signal after deposition of the carbon layer is in the range of Hz, e.g. For example, the measured difference for a 1 nm thick carbon layer is typically about 15 Hz. The signal from the crystal is strongly influenced by the emitted radiation (light and heat) during the current pulse and is seen in FIG. 4 as a steep increase in frequency deviation , This influencing sounds, as can be clearly seen from FIG. 4, after about 4 to 5 seconds to a base level. This base level is in turn compared to the base level measured after the next current pulse. According to the invention, this influence is taken into account for an accurate measurement of the thickness of the deposited layer, wherein the transient decay behavior of the quartz crystal is used after termination of a current pulse.
    In a first possibility, before the measurement of the material layer thickness, the decay of the signal of the quartz crystal to a basic level is awaited. This base level is usually reached 4 to 5 seconds after completion of the current pulse. Conveniently, the material layer thickness will be the difference between the base level of the -13 PI2609
    Oscillation crystal signal before separator »the material layer and the base level of the quartz crystal signal after deposition of the material layer determined.
    Alternatively, in a second possibility of determining the layer thickness, the layer thickness is derived by a fit of the transient decay function (transient measurement curve), whereby a sufficiently accurate measurement is already achieved during the decay time.
    FIG. 5 shows a flowchart for illustrating a process sequence for a coating by means of carbon filament evaporation. The procedure presented in this process provides an ideal uniform distribution of the evaporation material on all sample surfaces. The process is as follows:
    Place, advantageously in even distribution, the samples on the sample table (see sample table 100 in FIG. 1) or in the desired sample table segment. - Clamping the carbon thread in the evaporation source (at least one Fadenab section as in Fig. 1 or more, for example, up to four, thread sections as shown in Fig. 2). - Control of carbon filament evaporation is set in pulse mode - User input: o Desired layer thickness o Sample height correction o Select table segment (entire table, 180 ° segment, 90 ° segment, without rotation)
    Close the recipient and pump off by starting the vacuum pump until the desired vacuum is reached.
    Automatic determination of the occupied thread positions and the thread type by measuring the resistance, which defines further process parameters. ShutteT close - Cleaning of the thread sections by heating to 400-900 ° C (as known per table according to the measured resistance) - Opening the shutter - Evaporation of the carbon thread sections by short current pulses:
    o Voltage depending on thread type 12-30 V -14- PI2609 o Pulse length 50-500ms o After each current pulse, a measurement of the deposited layer thickness with the help of a quartz sensor (eg conventionally used quartz crystal, preferably the orientation AT) considering the transient decay behavior of the quartz crystal as described above. o Turning the sample table into predefined orientation positions to ensure uniform deposition on all samples, such as: For selection whole table: 9 positions at an angle distance of 40 ° are ordered in the order 1-4-7-2-5-8-3- Cycle through 6-9, as long as the current flow indicates the evaporation of the current thread section. For selection of table segments: correspondingly less / closer positions; Select always so that the deposition is balanced as well as possible over the selected segment at any time.
    If the resistance of the current thread section does not permit further evaporation, the changeover to the next thread section, readjustment of the table to correct the geometric offset of the two threads, then continuation of the evaporation process until reaching the desired layer thickness and layer homogeneity.
    Computational determination of the effective uniformly distributed layer thickness from the thickness measurements and termination of the process when the desired layer thickness is reached. - Optional: Automatic venting of the chamber at the end of the process, if desired.
    权利要求:
    Claims (20)
    [1]
    Claims 1. An apparatus for depositing a layer of material on a sample within a vacuum chamber, comprising a sample table (100) for arranging at least one sample (103a, 103b, 103c, 103d), an evaporation source (101, 201) connected to a power source ) for a thread-like evaporation material (102, 202), a quartz crystal (105) for measuring the deposited material layer thickness, and an evaluation device (113) associated with the quartz crystal (105), characterized in that the evaporation source (101, 201) has control electronics (112 ), which is arranged to supply the evaporation source (101, 201) with the electric current provided by the current source in the form of at least two current pulses with a pulse length of &lt; 1 s, and that the evaluation device (113) is adapted to take into account the transient decay behavior of the quartz crystal (105) immediately after completion of a current pulse for deriving the material layer thickness deposited after each current pulse.
    [2]
    2. Device according to claim 1, characterized in that the sample table (100) for positioning the at least one sample with respect to the position of the evaporation source (101,201) is designed as a motorized movable shuttle table.
    [3]
    3. A device according to claim 2, characterized in that the sample table (100) about a rotational axis (L) rotatable turntable (106), wherein at least two samples (103a, 103b, 103c, 103d), preferably offset by equal angles to each other , are arranged on the rotatable hub (106).
    [4]
    4. Apparatus according to claim 3, characterized in that the quartz crystal (105) in the middle of the turntable (106) is arranged.
    [5]
    5. Device according to one of claims 1 to 4, characterized in that the evaporation source (101, 201) has a at least two electrical feedthroughs (104a, 104h, 204a, 204b, 204c, 204d, 204e) having support for the filamentary evaporation material ( 102, 202). -16- PI2609
    [6]
    6. The device according to claim 5, characterized in that the holder for the filamentary evaporation material comprises at least three, preferably at least five electrical feedthroughs (204a, 204b, 204c, 204d, 204e).
    [7]
    7. Device according to one of claims 1 to 6, characterized in that at least one of the at least one sample is arranged at a distance of 30 mm to 100 mm from the evaporation source.
    [8]
    8. Device according to one of claims 1 to 6, characterized in that it is the thread-like evaporation material is a carbon thread.
    [9]
    9. A method of depositing a layer of material on at least one sample within a vacuum chamber, characterized by the steps of: evaporating at least a portion of filamentary evaporation material by electric current heating, the current passing the filamentary evaporation material into at least two current pulses having a pulse length of &lt; 1 s, the current pulses being selected such that the filamentary evaporation material does not rupture, measuring the material layer thickness deposited after a current pulse by means of a quartz crystal, taking into account the transient decay behavior of the quartz crystal immediately after completion of a current pulse.
    [10]
    10. The method according to claim 9, characterized in that the measurement of the material layer thickness takes place immediately after the completion of each current pulse.
    [11]
    11. The method according to claim 9 or 10, characterized in that before the measurement of the material layer thickness, the decay of the signal of the quartz crystal is awaited to a basic level.
    [12]
    12. The method according to claim 11, characterized in that the material layer thickness is determined from the difference between the base level of the quartz crystal signal before depositing the material layer and the base level of the quartz crystal signal after deposition of the material layer. -17- P12609
    [13]
    13. The method according to claim 9 or 10, characterized in that the measuring of the material layer thickness comprises the steps of: measuring the course of the frequency of the oscillating quartz as a function of time, adapting a parameterized function which is parametrized with at least one parameter , to this course, and - deriving a material layer thickness from the at least one parameter.
    [14]
    14. The method according to any one of claims 9 to 13, characterized in that the thread-like evaporation material is a carbon thread
    [15]
    15. The method according to any one of claims 9 to 14, characterized in that the pulse length of a current pulse 20 ms to 1 s, preferably 50 ms to 500 ms.
    [16]
    16. The method according to any one of claims 9 to 15, characterized in that the current strength of a current pulse is 6 A to 50 A.
    [17]
    17. The method according to any one of claims 9 to 16, characterized in that the determined by the evaporation geometry layer inhomogeneities are compensated by changing the positioning of the at least one sample with respect to their position to be evaporated filamentary evaporation material.
    [18]
    18. The method according to claim 17, characterized in that two or more samples are processed simultaneously.
    [19]
    19. The method according to claim 17 or 18, characterized in that the changing of the positioning of the sample takes place between two successive current pulses.
    [20]
    20. The method according to any one of claims 9 to 19, characterized in that it is carried out with a device according to one of claims 1 to 8.
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    EP0151737B1|1990-06-27|Process for controlling and monitoring the incorporation of a doping material into conductive metallic layers during their manufacture
    DE102010023517A1|2011-12-15|Coating system and method for coating a substrate with simultaneous layer monitoring
    EP0547081B1|1995-11-29|Process and device for the analysis and determination of the concentration of elements in the surface region of objects
    DE102007053194B4|2013-12-24|Process for layer deposition
    EP1668356B1|2009-06-17|Method for controlling the treatment of a crystal by means of a liquid
    DE2331751C3|1980-10-02|Method for material-dependent contrasting and device for carrying out this method for light microscopy
    DE102013110722A1|2015-04-02|Plasma-ion-based coating process and plasma probe
    DD266849A1|1989-04-12|DEVICE FOR ACCELERATED ARTIFICIAL AGING OF NON-METALLIC MATERIALS IN NON-TEMPERATURE PLASMA
    DD282475A5|1990-09-12|DEVICE FOR MEASURING THE DEPOSIT RATE AND LIMITING THE COATING PROCESS IN VACUUM COATING SYSTEMS
    WO2008065075A1|2008-06-05|Coating installation comprising a radio device and a measuring device
    DE1157410B|1963-11-14|Method and device for measuring the vapor pressure of substances which evaporate under vacuum
    同族专利:
    公开号 | 公开日
    AT512949B1|2016-06-15|
    US20130323407A1|2013-12-05|
    DE102013009203A1|2013-12-05|
    JP6267442B2|2018-01-24|
    DE102013009203B4|2021-01-14|
    JP2013249538A|2013-12-12|
    KR20130136385A|2013-12-12|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE1023830B|1955-06-23|1958-02-06|Zeiss Carl Fa|Arrangement for oblique vapor deposition of objects for electron microscopy|
    GB2000882A|1977-07-01|1979-01-17|Hitachi Ltd|Vacuum vapour-deposition apparatus|
    US4311725A|1978-08-18|1982-01-19|National Research Development Corporation|Control of deposition of thin films|
    US5536317A|1995-10-27|1996-07-16|Specialty Coating Systems, Inc.|Parylene deposition apparatus including a quartz crystal thickness/rate controller|
    US2079784A|1933-01-19|1937-05-11|Robley C Williams|Plating by thermal evaporation|
    US3699916A|1970-08-05|1972-10-24|Gte Automatic Electric Lab Inc|An apparatus for monitoring of the deposition of metallic films|
    JP2001040466A|1999-07-29|2001-02-13|Komatsu Ltd|Film forming device and film forming method|
    GB0019848D0|2000-08-11|2000-09-27|Rtc Systems Ltd|Apparatus and method for coating substrates|
    EP1460642B1|2003-03-20|2009-03-04|Agfa HealthCare NV|Manufacturing method of phosphor or scintillator sheets and panels suitable for use in a scanning apparatus|
    US20050281948A1|2004-06-17|2005-12-22|Eastman Kodak Company|Vaporizing temperature sensitive materials|
    JP2009185344A|2008-02-07|2009-08-20|Sony Corp|Vapor deposition method, vapor deposition apparatus, and method for manufacturing display device|
    JP5854731B2|2010-11-04|2016-02-09|キヤノン株式会社|Film forming apparatus and film forming method using the same|US6020052A|1996-07-30|2000-02-01|Ysi Incorporated|Laminated membrane structure for polarographic measurement and methods of making said structures|
    EP3091101B1|2015-05-06|2018-10-17|safematic GmbH|Coating unit|
    EP3091561B1|2015-05-06|2019-09-04|safematic GmbH|Sputter unit|
    JP6304181B2|2015-09-09|2018-04-04|トヨタ自動車株式会社|Gas detector|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    ATA50219/2012A|AT512949B1|2012-06-04|2012-06-04|Process for coating with an evaporating material|ATA50219/2012A| AT512949B1|2012-06-04|2012-06-04|Process for coating with an evaporating material|
    KR1020130059515A| KR20130136385A|2012-06-04|2013-05-27|Method for coating with an evaporation material|
    US13/906,469| US20130323407A1|2012-06-04|2013-05-31|Method for coating with an evaporation material|
    DE102013009203.5A| DE102013009203B4|2012-06-04|2013-06-03|Device and method for coating with an evaporation material|
    JP2013116612A| JP6267442B2|2012-06-04|2013-06-03|Apparatus and method for coating with evaporating material|
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