Method and apparatus for forming a low-grain layer on a substrate - Patents.com

Abstract

To provide an improved method and an improved apparatus for covering a substrate.SOLUTION: The invention relates to a method and an apparatus for forming one or more layers of few particles on a substrate in vacuum. The layer is deposited on the substrate from a cylindrical raw material by magnetron sputtering in some cases with a component of a reactive gas. The layer is deposited upward against gravity by a sputtering-up method. While performing the method or in the apparatus, structure of the layer or a stoichiometry atomic composition of the layer can be arbitrarily adjusted using a plasma source 12. Multiple sputtering supply sources having different raw materials 5, 6 and 7 can be provided in the apparatus, so that multiple layers composed of different compositions can be adhered on the substrate in one process at a high speed.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present invention relates to a method and an apparatus for forming one or more small-grain layers on a substrate in a vacuum. The layers are deposited on the substrate by magnetron sputtering from a cylindrical source material, optionally together with a reactive gas component. Deposition of the layers occurs against gravity in a so-called "sputter-up" process. The layers can optionally be adjusted in their structure or their stoichiometric atomic composition by means of a plasma source in the process or in the apparatus. Several sputter sources with different source materials can be provided in the apparatus, so that several layers of different compositions can be deposited on the substrate at high rates in one process. [Background technology]

[0002] Optical precision filters are important components of many industrial products in optical technology. Their applications range from laser engineering to medical and biomedical engineering, as well as the display and automotive industries and even the solar industry. Due to ever-increasing technological demands and due to increasing competition from low-wage countries, the demand for better, more flexible and at the same time economical manufacturing processes for optical precision coatings is growing. Current processes are increasingly being pushed against their technical limits, especially when high demands are made. Increasing waste, poor long-term stability and infeasibility of technical specifications reduce cost-effectiveness and hinder the introduction of new products.

[0003] In this respect, optical thin film systems utilizing the principles of interference, for example for laser engineering, medical and biomedical engineering, display engineering and automotive engineering as well as the solar industry, require that specific filter properties be measured as precisely as possible with low absorption and losses in the optical filters. In particular, in order to comply with the required minimum losses, it is absolutely necessary to minimize the contamination of the surfaces with particles, since these particles can cause scattering, absorption and low breakdown thresholds (e.g. in the area of ​​laser application).

[0004] The layer properties to be achieved in this regard may require mutually exclusive processing conditions: for example, a stable coating with high layer hardness (without edge temperature dependence) and a very smooth surface is generally associated with a compressive stress in the layer, whereas a stress-free layer is usually rough and shows a high dependence on temperature and humidity (spectral changes).

[0005] The great importance of the interaction of active particles (ions, neutrals, radicals) with the layer growth process and thus with the layer properties was recognized early on. The morphology and layer properties in plasma coating processes are essentially determined by the type and energy distribution of both ions and neutral particles, the particle energies of which can vary greatly depending on the plasma conditions.

[0006] The optical properties are also affected by particle bombardment of the growing layer (e.g. by sputtering gas particles): for example, the introduction of argon into an oxide or fluoride layer leads to an increase in absorption.

[0007] The possible influence of the energy of ions and neutral particles and their density is of considerable importance for the fabrication and optimization of optical layers. For example, energetic neutral particles bombarding the growing layer can induce Frenkel defects (Hisashi Arakaki, Kazutoshi Ohashi and Tomoko Sudou, "Sputter-Induced Defects in Zn-Doped GaAs Schottky Diodes," Semicond. Sci. Technol. 19, No.1 (January 2004), p. 127-132). Nanodefects play an even greater role in high-performance optical elements for ultrashort pulse laser applications or UV laser applications.

[0008] U.S. Patent No. 5,525,199 (Corning OCA; "Reactive Magnetron Sputtering Apparatus") and "Methods") is 5 x 10 -5 ~1.5×10-4 Torr (=6.7×10 -5 ~2.0×10 -4 The sputtering method and apparatus are described in a vacuum with a process pressure of 1000 psig (millibar). The substrate to target spacing is 16 inches (=40 cm).

[0009] The same is true of U.S. Patent No. 5,851,356 (Corning OCA; "Low Pressure Reactive Magnetron Spa"). The same apparatus and method are described in the "Applied Chromatography and Methodology" ("Applied Chromatography and Methodology"). The processing pressure range of this apparatus is 5×10 -5 ~4.2×10 -4 Torr (=6.7×10 -5 ~5.6×10 -4 The distance from the target is also 16 inches.

[0010] By tuning the process according to the prior art, a time constant of approximately 20-30 milliseconds can be achieved. One disadvantage of this dynamic stabilization is that even with ideal adjustment, small variations in the remaining process conditions and thus in the stoichiometry of the layers are inevitable, which can lead to small inhomogeneities and thus to loss mechanisms. For example, these inhomogeneities can lead to light losses (e.g., intensity losses), dispersion biases, and / or absorption biases. In particular, such inhomogeneities pose significant problems when using very high quality optical layers.

[0011] Therefore, the prior art has provided a solution to sputter extremely thin substoichiometric or metal layers and then oxidize them exclusively in oxygen plasma. The advantage of this method is again mainly on the metal surface of the target. This manufacturing process requires equipment technology with a separate plasma source and the movement of the substrate in the process (Scherer M., J. Pistner et al. (2004), "Innovative Manufacturing of High-Quality Optical Coatings for Applications in Optical and Optoelectronic Devices", 47th (Annual Technical Conference Proceedings of the Society of Vacuum Coaters, 179, 2004). In this process, in each case an extremely thin layer (1-2 Å) is oxidized.

[0012] In particular, a rotating table arrangement, as described in DE 103 47 521 A1, is suitable for this process, since in it a position for coating and a position for post-oxidation can be alternately moved. An apparatus and a method according to DE 103 47 521 A1 are provided for "sputtering down". In this configuration, the source material is deposited on the substrate from top to bottom by means of gravity. The particle flow is essentially characterized by a starting pulse, an impingement and a diffusion of particles from the source material. The heavier the particle, the greater the effect of gravity on the particle. In this "sputter down" process, the heavier particles are accelerated by gravity onto the substrate more. One disadvantage of the "sputter down" process is therefore that the particles are accelerated by gravity towards the substrate, but not away from it. The particles in the "sputter down" process can reach the substrate unhindered. In this respect, the effect of the particles on the quality of the product is neglected.

[0013] However, the particle issue has considerable practical importance in coating processes: particles along with defects on the substrate generally degrade the coating and generally result in its unacceptability. This issue is becoming more and more important as part of the growing demand and increasing miniaturization. [Prior art documents] [Patent documents]

[0014] [Patent Document 1] U.S. Patent No. 5,525,199 [Patent Document 2] U.S. Patent No. 5,851,356 [Patent Document 3] German Patent Publication No. 10347521 (A1) [Non-patent literature]

[0015] [Non-Patent Document 1] Hisashi Arakaki, Kazutoshi Ohashi and Tomoko Sudou, "Sputter-Induced Defects in Zn-Doped GaAs Schottky Diodes," Semicond. Sci. Technol. 19, No. 1 (January 2004), pp. 127-132. [Non-Patent Document 2] Scherer M., J. Pistner et al. (2004), "Innovative Manufacturing of High Quality Optical Coatings for Applications in Optical and Optoelectronic Devices", 47th Annual Technical Conference Proceedings of the Society of Vacuum Coaters, 179, 2004. Summary of the Invention [Problem to be solved by the invention]

[0016] It was therefore an object of the present invention to provide an improved method and an improved apparatus for coating a substrate. [Means for solving the problem]

[0017] This object is met by a method having the features of claim 1 and by a device having the features of claim 10. The further dependent claims show further advantageous developments. According to the invention, there is provided a method for forming a small particle layer by means of at least one magnetron sputtering device on a substrate moved in a vacuum chamber, said layer being formed from a cylindrical source material, optionally together with a reactive gas component, in which the method comprises the following steps: - fixing the substrate by a substrate holder on a rotating table; - depositing at least one layer of source material, optionally together with reactive gas components, on the substrate using a sputtering gas in at least one magnetron sputtering device; is performed, where the magnetron sputtering device is controlled to rotate the turntable so that the cylindrical source material is deposited against gravity (i.e., upwards) onto the substrate.

[0018] In the method according to the invention, at least one plasma source can be used, which can pretreat the surface of the substrate (for example clean the surface) by the action of a plasma, optionally together with a reactive gas, and can optionally be used to adjust the structure and / or stoichiometry of the layer by the action of the plasma of the plasma source, optionally together with a reactive gas.

[0019] In a preferred embodiment of the method, at least one plasma source is used, which can be controlled using a rotation stage. In the past few years, magnetron sputtering sources have proven to be a highly efficient coating tool for producing thin film systems on an industrial scale.

[0020] In the method according to the invention, a magnetron sputtering source is used with a cylindrical source material (i.e. a cylindrical target), preferably in the form of a cylindrical electrode, which is particularly advantageous for optical coatings and when layer homogeneity without bound particles is required.

[0021] With a cylindrical feedstock, the problem of flat targets, i.e. the formation of erosion grooves on the target surface, which results in a change in the layer thickness distribution, does not exist. In principle, a cylindrical feedstock allows an ideal layer thickness distribution to be maintained over the entire service life of the target. Furthermore, the throughput with a cylindrical feedstock is increased compared to a flat feedstock, and the process shows high long-term stability.

[0022] Magnetron sputtering sources are used in the so-called "sputter-up" configuration, which means that a cylindrical source material is deposited on the substrate against gravity, i.e., facing upwards. The advantage of this method is that gravity has a greater effect on heavy particles than on light particles. Thus, the heavy particles are accelerated more in the direction of gravity, i.e., downwards. Thus, they are accelerated away from the substrate and prevented from depositing as a disturbance on the target (substrate).

[0023] The "sputter-up" configuration increases the productivity of the coating process and therefore in particular the quality of the coated element. Further important reasons for the "sputter-up" configuration with cylindrical magnetron electrodes (targets) are the long-term stability of the sputtering process and the arc-free environment due to the lack of charge on the target surface. With flat targets, only areas of the target are removed by sputtering and further redeposition occurs. Charges can build up on the deposited dielectric layer until a breakdown (arcing) occurs. A cylindrical source material (target) has no areas to redeposit. This is an additional advantage of using reactive processes, which results in higher process cleanliness. Furthermore, due to the uniform removal of cylindrical targets, this sputtering off characteristic of the target does not change. This allows for a simpler use of shields, which can be used throughout the entire service life of the target (higher long-term stability).

[0024] In the "sputter-up" configuration, flat targets have even more disadvantages than cylindrical targets. Particles generated by flat source material (targets) can induce short circuits, which are prone to dark spaces in the target. This would destroy the entire batch, especially with coating concepts based on the turntable configuration. Since cylindrical sources do not have dark spaces, they are inherently preferred over flat sources in the "sputter-up" configuration with the turntable configuration.

[0025] In the method according to the invention and in the device according to the invention, at least one plasma source is selectively used to treat the substrate. An important purpose of this plasma treatment is to pretreat the substrate before the actual coating by direct deposition of organic compounds on the substrate. The purpose is to pretreat the substrate so that it is as free as possible from foreign particles. The quality of the sputtered layer can thus be substantially improved in terms of scattering, absorption and damage threshold. As a result, the method according to the invention can provide substantially improved properties to flat substrates (e.g. lenses). The method according to the invention is particularly advantageous for laser devices, edge filters, fluorescence filters, bandpass filters, reflectors for various wavelengths, anti-reflection coatings, mirror coatings, cavity filters and / or UV-IR cut.

[0026] An interface layer can be formed between the coating layers of a substrate having several layers. In the method according to the invention, the interface layer can be supersaturated with O2 and / or the layer can be fully reacted and deposited. This treatment can prevent the interface layer from rising between the two layers. Furthermore, it is intended to reduce the size of the interface layer between the two layers by selectively treating with plasma, the mixture of the two substances having an influence on the interface layer formation in the two layers. The expansion of the interface can be achieved by the action of the plasma source. This not only reduces light loss but also ensures better "design accuracy."

[0027] In the method according to the invention and / or the device according to the invention, the vacuum chamber in the magnetron sputtering device has a capacity of 3×10 -4 Millibar to 5 x 10 -2 Processing pressures can range up to millibar.

[0028] The partial pressure of the sputtering gas and / or reactive gas can be adjusted or stabilized by a generator in the magnetron sputtering apparatus, preferably This is done by adjusting the generator power, the generator voltage and / or the generator current.

[0029] The advantage of this regulation is that in the method according to the invention no dielectric layer is removed from the target, but rather the target is not covered by a dielectric layer at any time. This can be achieved, for example, by operating a metallic target in the so-called "transition mode". By appropriately adjusting the generator, the cylindrical source material (target) here is always metallic and oxygen-free, while there is sufficient oxygen in the processing space to oxidize the growing layer. The control variables listed above are generally obtained for the partial pressure of oxygen or the generator or target voltage. Thus, the deposition of stoichiometric layers can be achieved in this process at high deposition rates, while the effects of particle disturbances are minimized, i.e. the number of particles is very low.

[0030] In this process, the rotation table of the device is 1~500rpm -1 Speed, preferably 150-300 rpm -1 It can rotate at a speed of 150~300rpm. -1 Fast rotation of the turntable in the range of 1000 s (microseconds) can be advantageous for high throughput and high accuracy. With high rotation speeds, time constants of about 500 μs (microseconds) down to several milliseconds can be achieved.

[0031] In a further aspect of this method, the plasma source serves to reduce layer stress in layers on the substrate, preferably by minimizing boundary layer thicknesses and / or boundary layer sizes between individual layers on the substrate.

[0032] The layer stress or layer tension can be explained by the bombardment of the layer by active particles within the theory of the "atomic peening model" (Windischmann, H., (1992), "Intrinsic Stress in Sputter-Deposited Thin Films", Critical Reviews in Solid State and Materials Sciences, 17(6), p.547-596). Negatively charged oxygen ions, especially as they arise in reactive processes, can also have a significant effect on the layer growth. The importance of negative ions in the layer growth has been increasingly discussed in recent years (R. Dodd, S. You, P. Bryant, JW Bradley, "Negative Ion Density Measurements in Reactive Magnetron Sputtering", Plasma Process. Polym. 2009, 6, p.615-619).

[0033] Reflective argon particles were recognized as the source of layer stress by Windischmann, H., (1992), “Intrinsic Stress in Sputter-Deposited Thin Films”, Critical Reviews in Solid State and Materials Sciences, 17(6), p.547-596 in AlN layers, and by Jacobsohn (LG Jacobsohn, RD Averitt, M. Nastasi, “The role of trapped Ar atoms in the mechanical properties of boron carbide films deposited by dc-magnetron Sputtering”, J. Vac. Sci. Technol. A 21(5) (2003), p.1639) in BC layers. Other gases (e.g. the lighter krypton instead of argon) result in significantly lower stresses but also in reduced hardness.

[0034] In a further preferred embodiment, the plasma source fulfills one of the following functions: - Setting the temperature of the substrate; - setting the microstructure of a layer on a substrate; - cleaning the substrate, preferably by reducing organic contaminants on the substrate; Activating the surface of the substrate and / or the surface of a layer on the substrate.

[0035] In the method according to the invention, the thickness of the layer on the substrate can be monitored by monitoring the light transmittance, optionally by measuring the polarized transmittance, monitoring the light reflectance, optionally by measuring the polarized reflectance, monitoring the light absorption and / or by single wavelength ellipsometry or spectral ellipsometry.

[0036] To deposit a particular layer, a high deposition temperature or substrate temperature is required. For this purpose, in a preferred embodiment, a heatable element is attached to the cover of the device. Here, the temperature of the heatable element in the cover of the device is preferably set according to the layer to be produced. The temperature at this point may be varied during the coating process depending on the requirements of the particular layer, and the temperature of the heatable element in the cover may be set at a value between 50°C and 450°C. The temperature of the substrate can thus be set in the range from room temperature (about 20°C) to 300°C. The cover is thermally insulated from the rest of the device.

[0037] The device according to the invention for forming a small particle layer by magnetron spraying on at least one substrate moved in a vacuum has the following characteristics: - at least one magnetron sputtering device having a cylindrical source material, a generator, a sputtering gas, and optionally a reactive gas; - a cover, preferably a cover having a heatable element; and - a turntable having at least one substrate holder.

[0038] The apparatus is characterized by a cover hermetically enclosing the apparatus and a rotating stage hermetically enclosing at least one magnetron sputtering device further arranged such that the apparatus deposits source material (optionally together with a reactive gas component) against gravity toward a substrate.

[0039] In a preferred embodiment, the apparatus includes at least one plasma source, optionally with a reactive gas, where the at least one plasma source can be hermetically enclosed by a turntable of the apparatus with an effective gas to gas compartment separation of 1:25, preferably 1:100. In a preferred embodiment of the apparatus, the turntable is disposed above the plasma source.

[0040] The turntable is preferably positioned above a magnetron sputtering apparatus, and in a preferred embodiment, the turntable is positioned above a plasma source for depositing the source material against the force of gravity towards the substrate.

[0041] The apparatus according to the present invention is further characterized in that the magnetron sputtering apparatus has at least one magnetron electrode (i.e., target) made of source material. The magnetron electrode may have or consist of a target comprising or consisting of a material selected from the group comprising: a ceramic material or a mixture of ceramic materials, a thermal spray material or a mixture of such materials, a crystalline material, a metallic material or a mixture of metallic materials, and / or an oxide-containing material or a mixture thereof.

[0042] Preferably, the magnetron electrodes have targets which contain or consist of ceramic material. The compressive stresses in the optical layers already mentioned are of considerable importance. They can cause refractions in the optical element or even separation of layers or destruction of the substrate. A measure for reducing the tension of layers in the optical element is provided by the ceramic target. In pure water reactive processes using metallic targets, high layer stresses are found to occur due to the influence of negatively charged oxygen ions (JM Ngaruiya, “Fundamental Processes in Growth of Reactive DC Magnetron Sputtered Thin Films” Dissertation, RWTH Aachen (2004)), while enhanced molecular sputtering is found in ceramic targets (e.g. AZO, zinc oxide doped with aluminum) (F. Richter, T. Welzel, R. Kleinhempel, T. Dunger, T. Knoth, M. Dimer. F. Milde, “Ion energy distributions in AZO magnetron sputtering from planer and rotatable magnetrons” Surface & Coatings Technology 204 (2009), p.845-849), thus optimizing the energy input and reducing layer stresses can be expected.

[0043] The magnetron electrodes may contain or consist of targets containing or made of oxide-containing materials. Oxide-containing materials have the advantage that they provide a source of oxygen. In the sputtering region, extra oxygen is often necessary, for example because the oxygen of the plasma source is not sufficient for oxidation or because higher coating rates are to be achieved. In this case, it is advantageous to receive the oxygen directly from the target (i.e. from the magnetron electrodes), since this provides a higher stability compared to metal targets and oxygen as reactive gas. Usually, if the partial pressure of oxygen is not kept exactly constant, the reactive coating of metal (or silicon) targets with reactive gases is accompanied by rate instabilities, since the rate of the metal target may be significantly different from that of the corresponding oxide. If reactive gases (oxygen, nitrogen) are present in the target, their rate is independent of (not dependent on) the coating with an oxide layer.

[0044] A preferred oxide-containing material is TiO x , TaO x , NbO x , ZrO x , ZrO x :Y, HfO x , AlO x , SiO x , ZnO x , InSnO x and / or SnO x where x is particularly preferably selected so that the target itself is conductive, but at the same time x is close to stoichiometric.

[0045] The distance from the substrate to the magnetron electrode can be 2-10 cm, preferably 6-8 cm, particularly preferably 7 cm. The advantage of this distance is that it allows to form a uniform coating of few components with high density and high accuracy. The accuracy of the coating process decreases with the increasing distance from the magnetron electrode to the substrate.

[0046] According to the invention, a gap of 0.1 to 5 mm, preferably 1 to 3 mm, particularly preferably 2 mm is provided between the boundary wall of the magnetron sputtering apparatus and the turntable. This gap is necessary in order to design an airtight magnetron sputtering apparatus, i.e. to prevent the effective internal pressure of the apparatus from increasing. This has proven to be particularly advantageous for ensuring efficient compartmental separation of gases.

[0047] The magnetron sputtering apparatus may have a single magnetron arrangement. The magnetron sputtering apparatus preferably has a dual magnetron arrangement. The advantage of this arrangement is that more source material can be deposited per time the substrate is placed in the magnetron sputtering apparatus compared to a single magnetron arrangement. As a result, the efficiency of the sputtering process is substantially higher. Furthermore, by using a dual magnetron arrangement with bipolar excitation, a better long-term stability is ensured due to the "non-dissipative anode" and also a high plasma density in combination with a dense layer (but a more highly stressed layer) can be ensured.

[0048] In some cases it may also be advantageous to use other discharges. For example, to coat temperature-sensitive substrates such as polymers, direct current power supplies with unipolar pulsing (DC pulsed) are particularly suitable. In this case, the frequency of the pulses is also in the medium frequency range. The reason is that, compared to MF plasmas, pulsed DC plasmas have a lower ion energy and ion current density.

[0049] On the other hand, it is known that it is also possible to operate with RF (radio frequency) discharges. A frequency of 13.56 MHz is customary. Due to the high cost of this type of generator, they are usually not preferred. However, it is advantageous to be able to use RF sputtering to insulate the target material. This can be done, for example, with SiO x , AlO xThis is the case for , but also for other oxide, nitride or fluoride targets. Thus, for example, MgF2 or other fluorides can be sputtered. Thus, it is possible to operate with stoichiometric targets, which increases the process stability. In this respect, backside coating areas (insulating areas) that do not pose any problems due to discharges (arcing) are advantageous, allowing the deposition of layers with very few particles.

[0050] It may therefore be advantageous for the device to have a direct current power supply (DC, a pulsed direct current power supply (DC pulsed)), or a device for generating a HIPIMS, medium frequency or high frequency discharge.

[0051] In a further preferred embodiment, the apparatus preferably comprises two, possibly three, magnetron sputtering devices. The advantage of such an embodiment is that a multilayer coating can be obtained, i.e. a coating on a substrate with a plurality of different layers. In this case, a two-layer type stack consisting of different substances (source materials) can be formed using two magnetron sputtering devices. Thus, in the case of three magnetron sputtering devices, the possibility of a sputtering stack consisting of three different layers on a substrate consisting of different substances is given. Furthermore, a mixture of substances consisting of the respective source materials can also be formed, i.e. a mixed layer can be deposited. The use of two magnetron sputtering devices for optimizing the properties of the layers is particularly advantageous in the region of highly complex optical multilayer filters with more than 100 single layers. Depending on the requirements (e.g. special design), three or more magnetron sputtering devices can also prove advantageous.

[0052] The magnetron sputtering device may have an effective gas compartment separation of 1:25 for gas in vacuum, 1:100 is better. An effective gas compartment separation of 1:100 between the coating positions allows the production of well-defined co-sputtered materials, because the noble and / or reactive gas of the magnetron sputtering device is prevented from migrating further into the magnetron sputtering device. Furthermore, the amount of noble and / or reactive gas can be set more precisely to a specific determined value and / or can be kept constant by the effective gas compartment separation.

[0053] Plasmas based on magnetron discharges generally contain more than 99% non-ionized particles. They can have high energy and therefore contribute highly to the stress of the layer. They can be influenced indirectly, for example, by changing the configuration of the electric field or by using alternative sputtering gases. According to the invention, the sputtering gas may comprise or consist of a noble gas. Preferred noble gases are argon, neon, xenon and krypton. Mixtures of noble gases are also possible.

[0054] According to the invention, the reactive gas may comprise or consist of an oxidizing gas. Oxygen, nitrogen, tetrafluoromethane, octafluorocyclobutane, carbon dioxide and hydrogen fluoride are preferred reactive gases. Mixtures of these gases may also be used.

[0055] The device preferably has a flange for photometer and / or polarimetry. It allows photometric monitoring of the thickness of the layer on the substrate during the sputtering process. For this purpose, rapid broadband measurements (e.g. 300-1000 nm) of transmittance or reflectance can be carried out. The thickness of the layer can be determined and monitored by comparison with the theoretically expected spectrum. In some cases, even quartz crystals can be used, for example using cavity filters, where only small signal changes in transmittance are expected with a particular layer.

[0056] Alternatively, ellipsometry can be performed. It should be performed at an angle of incidence between approximately 55° and 75°, preferably 65°, relative to the normal. In situ ellipsometry can also be used to measure the dispersion of the refractive index (and sometimes the absorptivity). This is always advantageous, since it is necessary to know this precisely for broadband monitoring using transmittance or reflectance measurements. It may also be sufficient to use it stationary (e.g. with a stationary rotation stage) in an in situ polarimetry to measure each of the final deposited layers. This method is therefore suitable for calibration.

[0057] Elements that use the effect of polarization must often be used. In this regard, initial settings are made, for example, for reflectance or transmittance for polarized light. In this regard, Tp and Ts are the elements of transmitted light polarized parallel or perpendicular to the plane of incidence, and Rp and Rs are the elements of reflected light polarized parallel or perpendicular to the plane of incidence. These elements can therefore be used with any inclined angle of incidence (e.g. 45°, 60°, etc.) on the device according to the invention.

[0058] If layer monitoring is performed at tilt angles, it is advantageous to produce a coating that also works at tilt angles. Ellipsometry is often too slow to perform fast measurements, especially at the high rotational speeds of interest here. Measurements of the Rp and Rs (or Tp and Ts) elements can therefore be used very advantageously here. The measurements here are performed at an incidence angle of 45° with stationary polarizers. Two beam paths can be used for the two polarizations.

[0059] Alternatively, the polarization component can be selected and the spectrum combined with the transmittance measured at normal incidence, thus achieving similarly short measurement times (in the millisecond range) as for the transmittance measurements.

[0060] The combination of measurements with polarized light is also particularly suitable for monitoring thin metal layers (eg silver or aluminum), such a combination being used, for example, together with a polarizing beam splitter.

[0061] In a further preferred embodiment of the apparatus, the substrate holder of the rotation stage comprises or consists of polyetheretherketone. The use of polyetheretherketone has the advantage that particle formation is reduced.

[0062] The present invention will now be described in more detail with reference to the following figures and examples, but it is not intended that the present invention be limited to the specific embodiments shown therein. [1] A method for forming a small particle layer by means of at least one magnetron sputtering device (2, 3, 4) on a substrate moved in a vacuum chamber (1), comprising: The layer is formed from a cylindrical source material consisting of at least one magnetron electrode (5, 6, 7) and is subjected to the following steps: - fixing the substrate by a substrate holder (9) on a rotating table (10); - depositing at least one layer of source material (5, 6, 7) on the substrate using a sputtering gas (11) in at least one magnetron sputtering device (2, 3, 4); Here, the magnetron sputtering device (2, 3, 4) can be controlled by rotating the rotating table (10), and a cylindrical source material consisting of magnetron electrodes (5, 6, 7) is deposited on the substrate upward against gravity; The processing pressure in the magnetron sputtering equipment (2, 3, 4) is 3×10 -4 millibars ~ 5 × 10 -2 The method as described above, wherein the partial pressure of the sputtering gas (11) and / or the reactive gas (8) in the magnetron sputtering device (2, 3, 4) is adjusted and / or stabilized by a generator, in the range up to millibar, and the layer thickness on the substrate is monitored to control the process. [2] The method according to [1], characterized in that at least one plasma source (12) is used. [3] The method according to [2], further comprising pretreating the surface of the substrate by the effect of plasma from at least one plasma source (12). [4] The method according to either [2] or [3], comprising adjusting the structure and / or stoichiometry of the layer under the effect of a plasma from at least one plasma source (12). [5] The method according to any one of [2] to [4], wherein at least one plasma source (12) is controlled by a rotating table (10). [6] The method according to any one of [1] to [5], characterized in that the partial pressure of the sputtering gas (11) and / or the reactive gas (8) in the magnetron sputtering apparatus (2, 3, 4) is adjusted by adjusting the generator output, the generator voltage and / or the generator current. [7] The method according to any of [1] to [6], characterized in that the magnetron sputtering device is operated using a direct current power supply (DC), a pulsed direct current power supply (DC pulsed), a HIPIMS, a medium frequency or a high frequency discharge. [8] To control the process: a) Light transmittance monitoring; b) Light reflectance monitoring; c) monitoring of light absorption; d) Single-wavelength ellipsometry or spectral ellipsometry; and / or e) crystalline quartz measurement; The method according to any one of [1] to [7], wherein the thickness of a layer on a substrate is monitored by [9] The method according to any of [1] to [8], wherein the temperature of the heatable element in the cover (13) is set depending on the layer to be produced and / or the temperature is adjusted during the coating process.

[10] An apparatus for forming a small particle layer by magnetron spraying on at least one substrate moved in a vacuum, the apparatus comprising: (a) at least one magnetron sputtering device (2, 3, 4) having at least one magnetron electrode (5, 6, 7) made of cylindrical source material, a generator, and sputtering gas (11); (b) cover (13); and (c) a rotating stage (10) having at least one substrate holder (9); the cover (13) hermetically encloses the apparatus, and the rotating table (10) hermetically encloses the magnetron sputtering apparatus (2, 3, 4); The distance between the magnetron electrodes (5, 6, 7) and the substrate is 2 to 10 cm, and the magnetron sputtering devices (2, 3, 4) are arranged to deposit the material of the magnetron electrodes (5, 6, 7) toward the substrate against gravity; The processing pressure in the magnetron sputtering equipment (2, 3, 4) is 3×10 -4 millibars ~ 5 x 10 -2 The above apparatus in the range up to millibar.

[11] The apparatus described in

[10] , wherein the apparatus includes at least one plasma source (12).

[12] The apparatus according to

[10] or

[11] , characterized in that the rotating table (10) is disposed above the magnetron sputtering apparatus (2, 3, 4).

[13] The magnetron electrodes (5, 6, 7) a) a ceramic material or a mixture of ceramic materials; b) Spray material or mixture of spray materials; c) crystalline materials; d) metallic materials or mixtures of metallic materials; and / or e) oxide-containing materials; or mixtures of these; The apparatus according to any one of

[10] to

[12] , characterized in that it has a target comprising or consisting of the above, or consists of such a target.

[14] The apparatus according to any one of

[10] to

[13] , wherein the distance between the turntable (10) and the boundary walls (14, 15) of the magnetron sputtering apparatus (2, 3, 4) is 0.1 to 5 mm.

[15] The apparatus according to any one of

[10] to

[14] , characterized in that the magnetron sputtering apparatus (2, 3, 4) is configured with a single magnetron arrangement (2) or a dual magnetron arrangement (3, 4).

[16] The apparatus according to any one of

[10] to

[15] , characterized in that it comprises a direct current power supply (DC), a pulsed direct current power supply (DC pulsed) or a HIPIMS, a device for generating a medium frequency or high frequency discharge.

[17] The apparatus according to any one of

[10] to

[16] , characterized in having two or three magnetron sputtering devices (2, 3, 4).

[18] The apparatus according to any one of

[10] to

[17] , characterized in that the magnetron sputtering apparatus (2, 3, 4) has an effective gas compartment separation of 1:25 gas in vacuum.

[19] The apparatus according to any one of

[10] to

[18] , wherein the sputtering gas (11) contains and / or consists of a rare gas.

[20] The apparatus described in any one of

[10] to

[18] , characterized in that the reactive gas (8) contains or consists of a gas from the group consisting of oxygen, nitrogen, tetrafluoromethane, octafluorocyclobutane, carbon dioxide and hydrogen fluoride.

[21] Photometer (16), flange for measuring polarization (17) and / or The device according to any one of

[10] to

[20] , comprising an element comprising:

[22] The apparatus described in any one of

[10] to

[21] , characterized in that the substrate holder (9) of the rotating table (10) contains or is made of polyetheretherketone. [Brief description of the drawings]

[0063] [Figure 1] FIG. 1 shows a schematic plan view of a preferred apparatus according to the present invention, excluding the turntable. [Diagram 2] FIG. 2 shows a schematic plan view of a preferred apparatus according to the invention with a rotating table. [Diagram 3] FIG. 3 shows a schematic side view of a preferred apparatus according to the invention with a rotating table. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0064] 1 shows a schematic diagram of a preferred apparatus according to the invention in plan view, excluding the rotation stage. The apparatus comprises three magnetron sputtering devices 2, 3, 4, one of which is configured as a single magnetron arrangement 2 and two of which are configured as dual magnetron arrangements 3, 4. The magnetron sputtering device 2 comprises a magnetron electrode 5, a sputtering gas 11, and optionally a reactive gas 8, and the apparatus is in a vacuum 1. The magnetron sputtering devices 3, 4 each comprise two magnetron electrodes 6, 7, a sputtering gas 11, and optionally a reactive gas 8, and the apparatus is in a vacuum 1. A plasma source 12 and a photometer 16 and / or a flange 17 for polarimetry are arranged adjacent to the magnetron sputtering devices 2, 3, 4.

[0065] A preferred embodiment of the turntable is shown diagrammatically in plan view in figure 2. A turntable 10 is arranged in the apparatus and comprises, in this example, ten identical substrate holders 9. Figure 3 shows a schematic side view of a preferred embodiment of the apparatus with a rotating table 10. The cross section of the magnetron sputtering apparatus is visible, which has two cylindrical source materials 6, 7 (dual magnetron arrangement). The magnetron sputtering apparatus is hermetically delimited from the rest of the apparatus at the sides by boundary walls 14, 15 and at the top by the rotating table 10, which contains a sputtering gas 11 and optionally a reactive gas 8, which is in a vacuum 1. The two substrate holders 9 of the rotating table 10 are shown in cross section (i.e. visible). A cover 13 is arranged on the rotating table 10, which has boundary walls arranged on the sides of the rotating table 10. The rotating table closes the apparatus in a hermetically sealed manner. [Explanation of symbols]

[0066] 1 Vacuum chamber, 2, 3, 4 Magnetron sputtering device, 5, 6, 7 Magnetron electrode (source material), 8 reactive gas, 9 substrate holder, 10 rotation stage, 11 sputtering gas, 12 plasma source, 13 cover, 14, 15 boundary wall, 16 photometer, 17 flange for polarimetry.

Claims

1. A method for forming a small particle layer by means of at least one magnetron sputtering device (2, 3, 4) on a substrate moved in a vacuum chamber (1), comprising the steps of: In this method, an apparatus is used for forming a small particle layer by magnetron spraying on at least one substrate moved in a vacuum, the apparatus comprising: (a) at least one magnetron sputtering device (2, 3, 4) having at least one magnetron electrode (5, 6, 7), a generator, and a sputtering gas (11); (b) a cover (13); and (c) a rotating stage (10) having at least one substrate holder (9); Including, wherein at least one magnetron electrode is made of a cylindrical source material, the cylindrical source material including or made of a ceramic material, a cover (13) is disposed on the rotating table (10), the cover (13) hermetically encloses the apparatus, and the rotating table (10) hermetically encloses the magnetron sputtering apparatus (2, 3, 4), wherein the magnetron sputtering apparatus (2, 3, 4) is disposed to deposit the source material of the magnetron electrodes (5, 6, 7) against gravity toward a substrate, The method includes the following steps: (ii) fixing the substrate on the rotating table (10) by the substrate holder (9); ■ depositing at least one layer of source material on a substrate using a sputtering gas (11) in at least one magnetron sputtering device (2, 3, 4); in which the source material of the magnetron electrodes (5, 6, 7) is deposited on the substrate upwards against gravity; The processing pressure in the magnetron sputtering apparatus (2, 3, 4) is 3×10 －４ ~5×10 －２ the pressure is in the millibar range, the layer thickness on the substrate is monitored, there is a distance of 0.1-5 mm between the boundary wall of the magnetron sputtering device and the turntable, and the distance from the magnetron electrode to the substrate is 6-10 cm; A method as described above, wherein the temperature of the heatable element in the cover (13) is set depending on the layer to be produced and / or the temperature is adjusted during the coating process.

2. 2. The method according to claim 1, wherein there is a distance of 0.1 to 3 mm between the boundary walls (14, 15) of the magnetron sputtering device (2, 3, 4) and the rotating table (10).

3. 3. The method according to claim 1 or 2, wherein the partial pressure of the sputtering gas (11) in the magnetron sputtering device (2, 3, 4) is adjusted by adjusting the generator power, the generator voltage and / or the generator current.

4. The method according to any of claims 1 to 3, wherein the magnetron sputtering device is operated with a direct current power supply (DC), a pulsed direct current power supply (DC pulsed), a HIPIMS, a medium frequency or a high frequency discharge.

5. To control the process, (a) Light transmission monitoring; (b) monitoring of optical reflectance; (c) monitoring the amount of light absorption; (d) single wavelength ellipsometry or spectral ellipsometry; and / or (e) Crystalline quartz measurement; The method according to any one of claims 1 to 4, wherein the thickness of the layer on the substrate is monitored by

6. 1. An apparatus for forming a small particle layer by magnetron spraying on at least one substrate moved in a vacuum, the apparatus comprising: (a) at least one magnetron sputtering device (2, 3, 4) having at least one magnetron electrode (5, 6, 7), a generator, and a sputtering gas (11); (b) a cover (13); and (c) a rotating stage (10) having at least one substrate holder (9); Including, wherein at least one magnetron electrode is made of a cylindrical source material, the cylindrical source material including or made of a ceramic material, a cover (13) is disposed on the rotating table (10), the cover (13) hermetically encloses the apparatus, and the rotating table (10) hermetically encloses the magnetron sputtering apparatus (2, 3, 4), wherein the magnetron sputtering apparatus (2, 3, 4) is disposed to deposit the source material of the magnetron electrodes (5, 6, 7) against gravity toward a substrate, The processing pressure in the magnetron sputtering apparatus (2, 3, 4) is 3×10 －４ Millibar to 5 x 10 －２ in the millibar range, The gap between the boundary wall and the turntable of the magnetron sputtering device is 0.1 to 5 mm, and the gap between the magnetron electrode and the substrate is 6 to 10 cm; An apparatus as described above, wherein the temperature of the heatable element in the cover (13) is suitable for being set depending on the layer to be produced and / or the temperature is suitable for being adjusted during the coating process.

7. 7. Apparatus according to claim 6, wherein the turntable (10) is arranged above the magnetron sputtering device (2, 3, 4).

8. An apparatus according to claim 6 or 7, wherein the distance between the turntable (10) and the boundary walls (14, 15) of the magnetron sputtering device (2, 3, 4) is between 0.1 and 5 mm.

9. Apparatus according to any of claims 6 to 8, wherein the magnetron sputtering device (2, 3, 4) consists of a single magnetron arrangement (2) or a double magnetron arrangement (3, 4).

10. An apparatus according to any of claims 6 to 9, comprising a direct current power supply (DC), a pulsed direct current power supply (DC pulsed) or a device for generating a HIPIMS, medium frequency or high frequency discharge.

11. Apparatus according to any of claims 6 to 10, comprising two or three magnetron sputtering devices (2, 3, 4).

12. Apparatus according to any of claims 6 to 11, wherein the magnetron sputtering apparatus (2, 3, 4) has an effective gas compartment separation between coating positions within the apparatus of 1:25 gas in vacuum.

13. Apparatus according to any of claims 6 to 12, wherein the sputtering gas (11) comprises or consists of a noble gas.

14. The device according to any one of claims 6 to 13, further comprising a photometer (16), a polarimetry unit provided in the flange (17) and / or an element using the effects of polarized light.

15. An apparatus according to any one of claims 6 to 14, wherein the substrate holder (9) of the turntable (10) comprises or consists of polyetheretherketone.

16. 16. Apparatus according to claim 6, wherein the partial pressure of the sputtering gas (11) in the magnetron sputtering device (2, 3, 4) is regulated and / or stabilized by a generator.

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