FLUID VALVE WITH GOLD-CONTAINING AND / OR PLATINUM-CONTAINING COATING

DE502018015384D1Active Publication Date: 2024-12-19AGILENT TECHNOLOGIES INC
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Patent Information

Application Number
DE502018015384
Authority / Receiving Office
DE · DE
Patent Type
Patents
Current Assignee / Owner
Priority Date
2017-01-27
Filing Date
2018-01-23
Publication Date
2024-12-19
Estimated Expiration
2038-01-23

AI Technical Summary

Technical Problem

High-pressure HPLC systems face challenges in maintaining reliable fluidic seals and reducing wear on fluid valves due to the high stress and compressibility of liquids, which affects the precision and longevity of the components.

Method used

A fluid valve design featuring gold-containing or platinum-containing coatings on the contact surfaces of movable valve components, providing lubrication, balancing, and biocompatibility, thereby reducing wear and ensuring high tightness and long service life.

Benefits of technology

The gold or platinum coatings significantly reduce abrasion and ensure low-wear operation, enhance biocompatibility, and maintain fluidic tightness even under high pressures, extending the service life of the fluid valve and preventing undesirable interactions with biological samples or solvents.

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Description

TECHNICAL BACKGROUND

[0001] The present invention relates to a fluid valve, a sample separation device and a method for manufacturing a fluid valve.

[0002] In an HPLC, a liquid (mobile phase) is typically moved through a so-called stationary phase (e.g., in a chromatographic column) at a very precisely controlled flow rate (e.g., in the range of microliters to milliliters per minute) and at a high pressure (typically 20 to 1000 bar and beyond, currently up to 2000 bar), at which the compressibility of the liquid is noticeable, in order to separate individual components of a sample liquid introduced into the mobile phase. Such an HPLC system is known, for example, from EP 0,309,596 B1 by the same applicant, Agilent Technologies, Inc.

[0003] Such an HPLC system often has one or more fluid valves. Reliable fluid sealing is challenging, especially at high pressures, and the stress on the fluid valve components is high.

[0004] US 8,876,081 B2 shows a valve for an HPLC application where a diamond-like carbon (DLC) coating is used to reduce friction. REVELATION

[0005] It is an object of the invention to enable switching of a fluid valve in a sample separation device with high tightness and low wear. This object is achieved by means of the independent claims. Further embodiments are shown in the dependent claims.

[0006] According to the present invention, a fluid valve (i.e., a valve for controlling fluid, wherein a fluid may be a gas and / or a liquid, optionally comprising solid particles) is provided for a sample separation device (for example, a liquid chromatography device), wherein the fluid valve comprises a first valve component (with a contact surface, furthermore, in particular, a contact surface with a second valve component, wherein the first valve component may, for example, be designed as a rotor device) and a second valve component (with a contact surface, furthermore, in particular, a contact surface with the first valve component, wherein the second valve component may, for example, be designed as a stator device), wherein the first valve component and the second valve component are adjacent to one another (in particular at the contact surfaces), are movable relative to one another (for example, rotatable or longitudinally displaceable), and are configured such thatthat in at least one switching state, at least one switchable fluid channel (in particular switchable by a relative movement of the valve components to one another) is formed between them, and wherein at least a part of a (in particular outer and / or inner) surface (in particular the contact surface) of at least one of the first valve component and the second valve component is provided with a gold-containing and / or platinum-containing coating.

[0007] According to another exemplary embodiment, a sample separation device for separating a fluidic sample (in particular into different fractions which may differ with respect to at least one separation property) is provided, wherein the sample separation device has a fluid valve with the features described above.

[0008] According to the invention, a method for producing a fluid valve for a sample separation device according to claim 14 is provided, wherein in the method a first valve component and a second valve component are provided such that they adjoin one another and are movable relative to one another, the first valve component and the second valve component are designed such that at least one switchable fluid channel is formed between them in at least one switching state, and at least part of a surface of at least one of the first valve component and the second valve component is provided with a gold-containing and / or platinum-containing coating.

[0009] According to the invention, a fluid valve is provided in which at least part of a surface of at least one of two relatively movable valve components is provided with a gold-containing or gold-containing coating. Surprisingly, it has been found that such a gold-containing surface at a contact surface between the valve components creates lubrication between the opposing valve components that slide against each other during a switching operation, so that when a gold-containing coating is provided, only very little abrasion can be expected between the valve components, even during long-term operation. Such a fluid valve therefore has a long service life. In synergy with the described lubricating effect, a gold-containing coating on the contact surface(s) also ensures that a certain level of compensation is provided between the valve components during a switching operation.Depending on its hardness, the gold coating is capable of compensating for locally high forces, for example, in the case of tolerance-related or otherwise generated minor misalignment between the valve components, by the gold material clearly avoiding the load. This additional function of the gold-containing coating on the contact surface further increases the service life of the fluid valve. Advantageously, the gold coating is also biocompatible, meaning it interacts very little or not in an undesirable way with a fluid (especially a liquid such as a solvent or a biological sample) that may flow through the at least one fluid channel formed between the valve components during switching of the fluid valve.In this way, a gold-containing coating on the surface of fluid structures / microstructures prevents undesirable effects such as corrosion, increased sample adhesion, the formation of undesirable chemical reaction products, or undesirable changes in the fluid processed by the fluid valve, etc. When coating a multi-component valve component composed of several bonded elements or bodies (for example, a rotor device composed of several bonded rotor elements), the gold-containing coating on one or both opposing bond surfaces promotes the strength of the one-piece bond. This reliably ensures the intrinsic cohesion of the corresponding valve component.

[0010] As an alternative or complement to gold, platinum is also a high-performance material for coating the respective surface. In particular, platinum exhibits pronounced biocompatibility and can also provide the advantages described above for gold in a similar or equivalent manner.

[0011] According to exemplary embodiments of the invention, the gold-containing layer or the gold layer, in particular a hard gold layer, can be applied to many materials. For example, this is also possible on a copper substrate. This allows the ductile properties (in particular, formability) and the excellent thermal conductivity of this material to be utilized.

[0012] Another biocompatible embodiment of a valve component (i.e., a rotor or a stator) is a platinum coating. This can also be deposited galvanically (i.e., non-selectively). Due to the acidic platinum bath, the substrate (e.g., a valve component) should be configured to withstand this acid attack. In this regard, pre-gold plating before applying the platinum-containing coating or platinum coating is advantageous for many substrates. Alternatively, such a platinum layer can be applied to the surfaces of a substrate (e.g., a rotor substrate or another valve component) using a (particularly selective) sputtering process. Suitable substrates include, for example, metals such as copper, steel, palladium, or tungsten, glasses (particularly with an adhesion promoter), higher-melting plastics such as PEEK, or one or more ceramics.

[0013] A platinum coating has the particular advantage that unwanted adhesion of biomolecules (e.g. proteins) to it practically does not occur.

[0014] In the context of this application, the term "gold-containing" refers in particular to a coating material on a surface that contains more than insignificant traces of gold. For example, the gold component of the coating can contain at least 1 percent gold by weight, in particular at least 10 percent gold by weight, more particularly at least 50 percent gold by weight, preferably at least 90 percent gold by weight, and most preferably at least 99 percent gold by weight (to achieve particularly high biocompatibility).

[0015] In the context of the present application, the term "platinum-containing" refers in particular to a coating material on a surface that contains more than insignificant traces of platinum. For example, the platinum component of the coating can contain at least 1 percent platinum by weight, in particular at least 10 percent platinum by weight, more particularly at least 50 percent platinum by weight, preferably at least 90 percent platinum by weight, and most preferably at least 99 percent platinum by weight (to achieve particularly high biocompatibility).

[0016] In the context of the present invention, the term "valve component" refers to a valve body that can be moved relative to another valve component during a switching operation of the fluid valve. According to a preferred embodiment, the two valve components are a rotor device and a stator device of a fluid valve. Alternatively, however, it is also possible, for example, to accomplish the switching of the fluid valve through a longitudinal movement between two interacting valve components.

[0017] In the context of the present application, the term "surface" of a valve component refers in particular to an inner and / or outer boundary or contact surface of the valve component. Parts of such a surface can be, in particular, a contact surface between the valve components interacting in a fluid-tight manner and / or an inner bonding surface between bonded individual bodies of a valve component and / or a surface in fluid contact for delimiting a fluid channel or a fluid structure of the valve component(s).

[0018] In the following, additional designs of the fluid valve, the method and the sample separation device are described.

[0019] According to the invention, the first valve component has a contact surface as part of its surface, and the second valve component has a contact surface as part of its surface, wherein the first valve component and the second valve component adjoin one another (in particular, touch one another) at the contact surfaces. Within the context of the present application, the term "contact surface" of a valve component is understood to mean, in particular, a boundary or contact surface of the valve component with another valve component interacting with this valve component, at which boundary or contact surface a fluid-tight interface is formed between the valve components. Simultaneously, the at least one fluid channel formed between the valve components in at least one switching state of the fluid valve can pass through said boundary or contact surface.

[0020] According to the invention, at least a portion of the contact surface of at least one of the first valve component and the second valve component is provided with the gold-containing coating. A gold-containing and / or platinum-containing coating of at least one such contact surface promotes lubrication and balancing of the valve components and ensures low-wear operation (tribologically optimized).

[0021] According to one embodiment, the coating can be formed on at least one of the two contact surfaces between the first valve component and the second valve component. By providing an entire contact surface between the two valve components of the fluid valve with a gold-containing and / or platinum-containing coating, which can be provided entirely by one of the two valve components or throughout by both valve components, it is ensured that no tribological material constellation that promotes abrasion or wear can occur at any point in the contact area between the valve components.

[0022] According to one embodiment, the coating can be formed on the contact surface of the first valve component and on the contact surface of the second valve component. If both opposing and tribologically interacting contact surfaces of the two valve components are fully or partially coated with a gold-containing and / or platinum-containing coating, the described effects with regard to lubrication, compensability, and biocompatibility are particularly pronounced.

[0023] According to one exemplary embodiment, a counter-surface having at least one fluid structure with a further part of the surface can be located opposite the contact surface of at least one of the first valve component and the second valve component as another part of the surface. The contact surface and counter-surface can be parallel to one another. The structured surface or structural surface can be located inside a two- or multi-component valve component, for example at the interface between two rotor elements of a rotor device that are bonded to one another or possibly simply lie on top of one another. The fluid structures can be part of the at least one fluid line that can be formed between the valve components. For example, the fluid structures can be grooves and / or fluid connections whose delimiting walls form the aforementioned surface part.

[0024] According to one embodiment, at least a portion of at least one of the fluid structures and / or the counter surface can be provided with the gold-containing and / or platinum-containing coating. In the fluid structures, this coating can lead to biocompatibility and thus significantly reduced damage during operation of the fluid valve, regardless of the fluid used. In the counter surface, the coating can promote the connectability (e.g., by bonding) of one valve component to another valve component.

[0025] According to one embodiment, the mating surface can be bonded to the coating with a cover body. Bonding (or other joining) of the cover body (e.g., a rotor element) with another body of the valve component (e.g., another rotor element) can be facilitated by the gold or platinum content of the coating. The resulting bond can be chemically particularly stable due to the gold and / or platinum-containing coating. Re-gold plating of the outer surfaces and the connecting structures is also possible, if necessary. Subsequent application of platinum is also possible.

[0026] According to one embodiment, at least a portion (e.g., a partial layer of a multi-layer coating) of the coating may comprise or consist of hard gold. In this context, hard gold may be understood to mean an alloy with a main component of gold (in particular, greater than 99 percent by weight), traces of carbon (e.g., up to 0.7 percent by weight), and an additive (e.g., nickel and / or cobalt, e.g., 0.2 to 0.3 percent by weight), which results in greater hardness than gold. It has been found that a coating of hard gold has particularly advantageous properties with regard to lubrication, compensability, hardness, and biocompatibility. Fluid valves coated in this way on the contact surface between the valve components exhibit excellent service lives and are particularly low-wear.

[0027] According to one embodiment, at least a portion (for example, a partial layer of a multi-layer coating) of the coating can comprise cobalt in a range between 0.05 weight percent and 1 weight percent, in particular in a range between 0.2 weight percent and 0.3 weight percent, and otherwise gold. The gold component particularly promotes compensability and biocompatibility, while the cobalt component provides good lubricity and special hardening of the coating. However, it is particularly advantageous if the cobalt component lies within the described value ranges for the cobalt component, most advantageously within the narrower of the two described value ranges for the cobalt component. If the value ranges for the cobalt component are significantly undercut, the lubricity of the coating is reduced.If the cobalt component's values ​​are significantly exceeded, the coating may no longer meet the highest biocompatibility requirements. The biocompatibility of the coating is promoted by the properties of gold, which is inert even to aggressive chemicals and biofluids.

[0028] According to one embodiment, the platinum-containing coating can be particularly advantageously formed by first pre-gold-plating a respective surface (i.e., in particular, providing it with a gold-containing layer, for example, pure gold) and subsequently applying a layer comprising platinum or consisting of platinum (in particular by sputtering, PVD). When implementing the coating using platinum, it is therefore advantageous to form a double layer, i.e., a layer of a first material directly on a surface and the subsequent application of platinum to this layer. However, it is also possible to apply platinum directly to a substrate (for example, based on an acidic bath).

[0029] According to one embodiment, exactly one of the first valve component and the second valve component can be provided with the gold-containing and / or platinum-containing coating, and the other of the first valve component and the second valve component can be provided with a different coating made of a different material. The material of the other coating can have a higher hardness than the material of the gold-containing and / or platinum-containing coating. According to a particularly preferred embodiment, the opposing valve components are coated with different materials on their contact surfaces. It is very advantageous to coat one of the two valve components, in particular a rotor device, with the gold-containing and / or platinum-containing coating.The opposing contact surface of a valve component, preferably designed as a stator device, can, however, be coated with a different material specifically tailored to its requirements in order to improve the interacting properties between the opposing contact surfaces. For example, the other material of the other coating can have a higher hardness (and a different roughness) than the material of the gold- and / or platinum-containing coating. The adaptation of these properties can relate to the tribological system (i.e., the running properties related to opposing friction surfaces), the hardness, the (bio)compatibility, the lubricity, the compensating ability of the coating material, or, more generally, to improving the wear resistance of the fluid valve.

[0030] According to one embodiment, a coating made of the other material can comprise or consist of diamond or diamond-like carbon (DLC). It has proven particularly advantageous to form the first coating of hard gold with a cobalt component and the second coating, which differs from the described first coating, of diamond or DLC. The latter materials are particularly hard and reliably reduce abrasion or wear of the valve component coated therewith. A metallic coating (particularly made of hard gold) can achieve high biocompatibility, and a DLC coating can even achieve bioinertness.

[0031] According to one embodiment, the coating may comprise multiple layers. Such a multi-layer coating is an effective measure for adjusting the desired properties of the coating between the valve components. In particular, a double coating, i.e., a coating with exactly two layers of different materials, has proven to be a reasonable balance between the manufacturing effort and the achievable properties.

[0032] According to one embodiment, a first layer can be pure gold directly on a base body of the respective valve component, and a second layer can be hard gold on the first coating. A pure gold component is understood here, in particular, to be a component that consists essentially or entirely of gold. The external hard gold component arranged above it forms the actual contact surface with the opposing valve component.

[0033] According to one exemplary embodiment, a base body of the respective valve component on which the coating is arranged can comprise metal, in particular steel. The base body of the valve components can be selected almost freely due to the advantageous properties of the coatings. A metallic component, in particular a steel component, furthermore in particular stainless steel, is a good choice of material with regard to the hardness and manufacturability of the valve component. It is also possible to form one of the valve components from bare steel. However, other materials, such as ceramic or the like, are possible. A metallic valve component, in particular one made of steel, has the advantage of being particularly easy and good to coat with the gold-containing and / or platinum-containing layer.Layer delamination or undesirable chemical phenomena at an interface between the metallic valve component and the gold-containing and / or platinum-containing coating are advantageously suppressed.

[0034] According to one embodiment, the first valve component and the second valve component can be movable relative to one another in such a way as to establish at least two different fluid coupling states (e.g., fluidly coupled and fluidly decoupled) of the at least one fluid channel. For example, in a first fluid coupling state, a fluidic connection through the fluid valve can be enabled. In contrast, in a second fluid coupling state, such a fluidic coupling can be prevented. It is also possible for different fluidic paths through the valve component to be enabled in different fluid coupling states. The individual fluid coupling states can be established by the relative movement of the valve components to one another.

[0035] According to one embodiment, the at least one fluid channel can be formed from at least one groove in the first valve component (for example, a rotor device) and at least two fluid connections (for example, ports) on the second valve component (for example, a stator device), wherein in different switching states of the fluid valve, the fluid connections can be brought into different fluidic coupling states with the at least one groove. Advantageously, two or more fluid connections can be provided on a stator component of a fluid valve, which can be fluidically coupled to other fluidic components (for example, via capillaries or hose connections). The actual fluidic connections are then achieved by one or more switchable grooves, which are preferably provided on a contact surface or axially offset from the contact surface of a valve component designed as a rotor device.In the corresponding fluid coupling states, the grooves can be either fluidically connected to certain fluid connections or fluidically decoupled from them.

[0036] According to one embodiment, the first valve component can be designed as a rotor device that is rotatable relative to a laboratory system, and the second valve component can be designed as a stator device that is at rest relative to a laboratory system and that is rotatable relative to one another. The design as a rotor valve ensures a particularly compact configuration in which many different fluid coupling states can be set with little effort. Alternatively, a design as a displacement valve is also possible, in which a longitudinal displacement between the two valve components enables different fluid coupling states through the one or more fluid channels formed between the valve components.

[0037] According to one embodiment, the first valve component, when configured as a rotor device, can have a first rotor element and a second rotor element, which can in particular be bonded to one another. The first rotor element can define at least part of the at least one fluid line (for example, have at least one groove and / or at least one fluid passage). In contrast, the second rotor element can form a cover for the first rotor element (in particular, be free of elements of the fluid line and, for example, form a circumferentially closed capillary-like line section by covering a groove of the first rotor element). The formation of a rotor component (and / or a stator component) from two (or more) individual bodies that are connected to one another has proven particularly advantageous.This allows fluidic channels to be formed inside a rotor assembly with minimal effort in one of the two rotor elements before the two rotor elements are bonded together to form a one-piece rotor assembly. Such bonding joins the rotor elements together in such a way that they are subsequently fused together at the interface (e.g., by ultrasonic and / or thermocompression bonding). This allows even complex fluidic structures to be formed inside a rotor component without the associated fluidic complexity becoming excessive.

[0038] According to one embodiment, the first rotor element can have, as at least part of a first fluid line, a groove (extending, for example, in a plane perpendicular to a rotation axis) on one of the two opposite main surfaces, and, as at least part of a second fluid line, at least one passage (extending, for example, parallel to a rotation axis) through the first rotor element and a groove fluidically coupled thereto (extending, for example, in a plane perpendicular to a rotation axis) on the other of the two opposite main surfaces. Two grooves formed in mutually opposite main surfaces, which are connected to one another by one or more passages extending perpendicular thereto (alternatively, the passages can also be drilled obliquely), result in high fluidic performance of a rotor device designed in this way.In particular, this can prevent unwanted fluidic overlaps when switching a fluid valve, for example, if a groove extending in the radial direction is not to be brought into undesired fluid communication with grooves extending, for example, in the tangential direction. One of the two grooves can then be relocated to a different plane using the described configuration of the rotor device and can thus fluidically tunnel under the other groove, which is not to be brought into fluid communication with it. In this way, even complex fluidic structures (for example, in two or more planes) can be integrated into a compact fluid valve.

[0039] According to another embodiment, the first valve component, as at least part of a first fluid line, can have a groove on a main surface facing the second valve component, and as at least part of a second fluid line, can have at least one passage through at least part of the first valve component and a line section fluidly coupled thereto. In particular, the groove, on the one hand, and the line section, on the other hand, can extend over different radial regions of the first valve component.

[0040] According to one embodiment, the fluid valve can have a leak sealing element arranged between the first valve component and the second valve component for fluidic low-pressure sealing and controlled leak removal. In particular, the sealing element can be a sealing ring. Such a sealing element can further strengthen the fluidic tightness between the two valve components. Although the gold-containing and / or platinum-containing coating already contributes to the tightness of the at least one fluid channel between the two valve components due to its intrinsic properties, the leak-freeness can also be further improved for high-pressure applications (such as in HPLC) by an additional sealing element.Such a sealing element can, for example, be a sealing ring which can be arranged in a groove of one of the two valve components and, after connecting (for example pressing) the two valve components, presses fluid-tight against the opposite contact surface of the other valve component.

[0041] According to one embodiment, the sealing element can comprise or consist of polytetrafluoroethylene (PTFE, Teflon®) or a PTFE-EPDM (ethylene-propylene-diene) composite. However, sealing elements made of other materials (e.g., perfluoroelastomers, especially nanoactivated) are possible.

[0042] According to one embodiment, at least one of the first valve component and the second valve component can comprise at least one material from a group consisting of a metal, a plastic (in particular with or without filler particles), and a ceramic. By selecting the appropriate material, additional properties of the fluid valve, for example, mechanical and / or thermal properties, can be adjusted.

[0043] According to one embodiment, different fluidic structures can be provided in different diameter ranges of the first valve component. This allows even complex fluidic coupling tasks to be enabled in a compact fluid valve.

[0044] According to one embodiment, at least one function from a group consisting of a fluidic restriction, a fluidic delay device for delaying a fluid flow, an intermediate storage volume for temporarily storing a predefined fluid quantity (for example, in the nanoliter to microliter sample range), and a fluidic mixing device can be provided by means of the at least one fluid channel. A fluidic restriction can, for example, be provided as a constriction between two fluid connections by forming a groove with a defined width and depth than the fluid connections. A fluidic delay device can, for example, represent an extended fluid channel (for example, a non-linear connection) between fluid connections, for example, a meandering or spiral channel configuration.For example, a sample section can be temporarily imprisoned in an intermediate storage volume or subjected to a fluidic reactor reaction there. For this purpose, a measure can be provided in the respective fluid channel that predestines the fluid channel as a reactor and / or enables a temporary shutoff of the temporarily stored or buffered fluid volume. A fluidic mixing device can, for example, be configured with several channels of different lengths and / or diameters branching off from a fluid connection, so that fluid components flowing through the different channels have different flow velocities, thereby resulting in a mixing of a fluidically coupled fluid therein. However, additional or other functions are possible.

[0045] According to one embodiment, the coating can be formed on the respective valve component by means of a non-selective or non-specific deposition process. In other words, according to the described embodiment, it is not necessary to ensure that the coating of the respective valve component is formed exclusively on the contact surface. This considerably simplifies the manufacturing process of the fluid valve because masking processes and the like (which would be necessary for selectively forming the coating only at selected locations) are not required. In addition, coating other surface areas of the respective valve component (for example, fluid structures such as grooves, fluid connections and / or passages that contribute to the formation of the at least one fluid channel) has the advantage that these surfaces are then also provided with bioinert or biocompatible protection.When forming the coating on the surface, it has proven particularly simple from a manufacturing perspective to coat the entire exposed surface of the respective valve component (or a subcomponent thereof). This is due to the fact that such coatings (e.g., DLC) can be formed using deposition processes (e.g., chemical vapor deposition (CVD), PACVD), in which the coating is deposited non-specifically over the entire surface. In the case of gold, this is often a galvanic process of the entire exposed surface of a respective valve component. This coating, which is particularly simple from a manufacturing perspective, simultaneously ensures that all of the technical advantages of the coating (lubrication, compensability, bioinertness / biocompatibility, bondability, etc.) are achieved.) in different surface areas of a particular valve component. Additional effort (masking, etc.) required to limit the coating to individual surface areas can also be eliminated.

[0046] According to one exemplary embodiment, at least a part of at least one fluid structure of the first valve component (in particular a rotor device) can be offset in the axial direction relative to the contact surfaces, so that in at least one switching state of the fluid valve, this part and at least one other part of at least one fluid structure of the first valve component and / or the second valve component (in particular a stator device) at least partially overlap when viewed along the axial direction. According to such an exemplary embodiment, different parts of fluid structures of a rotor device or a stator device of a fluid valve can be formed overlapping one another in the axial viewing direction or projection and axially in different planes, without necessarily being fluidically coupled to one another or being undesirably temporarily coupled to one another during a switching operation.This can be achieved by arranging the different parts of the fluid structures in different axial planes of the fluid valve, but still at least partially aligned with each other in the viewing direction. This makes it possible to provide a compact fluid valve that can flexibly handle even complex fluidic structures.Due to the displacement of different parts of the fluid structures into different planes, these can intersect or cross each other when viewed in or projected onto the direction of rotation statically (for example, when the parts are all integrated in the rotor device) and / or dynamically (for example, during rotation of the rotating device relative to a stationary stator device, when the parts are partly integrated in the rotor device and partly in the stator device) without fluid flowing undesirably from one part of the fluid structure(s) into the other part of the fluid structure(s).

[0047] According to one embodiment, in the at least one rotational state in which the at least partial overlap occurs, the at least one part and the at least one other part can be fluidically decoupled from one another. Different fluids can thus flow independently of one another through the part and through the other part in at least one said rotational state without undesirably interacting with one another. According to another embodiment, in the rotational state in which the at least partial overlap occurs and / or in another rotational state, the at least one part and the at least one other part can be fluidically coupled to one another in a targeted manner.

[0048] According to one embodiment, the at least one other part may be formed by at least one fluid connection of the stator device (see for example Figure 12). A spatially static fluid connection of the stator device can thus be provided at any position, in particular even with multiple orbital radii of the said structures, without running the risk of temporarily coming into undesirable interaction with a groove, channel system or the like located inside the rotor device during the switching of the fluid valve.

[0049] According to one embodiment, the at least one other part can be formed by a plurality of fluid connections of the stator device, which are arranged at at least two different radii of the stator device relative to the rotation axis. Due to the possibility of providing a plurality of fluid connections at different radii, even complex fluidic tasks can be fulfilled by a compact fluid valve.

[0050] According to one embodiment, the at least one part can extend from a first radius to a second radius of the rotor device (in particular in the radial direction), and the at least one other part can be arranged on a third radius that is greater than the first radius and smaller than the second radius. The arrangement of the structures on the corresponding radii can be related to the axis of rotation. When the fluid valve is switched, for example, the other part designed as a fluid connection can then slide over the fluid structure between the first radius and the second radius without entering into fluidic interaction with it.

[0051] According to another embodiment, the at least one other part of the at least one fluid structure can also be associated with the rotor device and can be offset relative to the at least one part of the at least one fluid structure of the rotor device in the axial direction relative to the axis of rotation (see, for example, Figure 13 ). According to this design, it is possible to provide different fluid structures at different levels in the rotor device, which can be operated independently of one another. These can, for example, intersect in plan view.

[0052] According to one exemplary embodiment, the at least one other part of the at least one fluid structure can be arranged on the contact surface of the rotor device, thus directly at the interface between the rotor device and the stator device. In particular, the at least one other part of the at least one fluid structure can be a surface groove of the rotor device at its contact surface. The other part of the corresponding fluid structure can be manufactured on the contact surface with particularly low manufacturing effort, for example by removing material (for example by milling) from the surface to form the groove.

[0053] According to one exemplary embodiment, the at least one fluid structure of the rotor device can have at least one passage (for example, designed as a vertical blind hole or through-hole) through the rotor device from the contact surface of the rotor device to the at least one part (spatially offset from the contact surface). Such a passage can be formed with little effort, for example, by drilling (or by etching or by the PEM process) a vertical bore in or through the rotor device or a rotor element thereof. Inclined drilling is also possible. Through one or more such passages, a fluidic connection can be established with simple means with a fluid structure of the rotor device that is axially offset from the contact surface.

[0054] According to one embodiment, the at least one passage and the at least one part may form a fluidic bypass for the at least one other part (see for example Figure 4 or Figure 5 ). Illustratively, two passages and a groove-like or capillary-like other part can cause a tunneling of a fluid structure at the contact surface or in another plane of the rotor device.

[0055] According to one embodiment, two passages and a part connecting these passages can be provided, which together form a substantially U-shaped structure in cross-section (see for example Figure 4 or Figure 5 ). Such a U-shape can be formed by two vertical passages and a horizontal connecting part between the two vertical passages to tunnel under another fluid structure.

[0056] According to one embodiment, the at least one part may be formed by a groove in a first rotor element of the rotor device, which groove is covered by a second rotor element (see for example Figure 5 ). Milling a groove is possible with minimal manufacturing effort. If a first rotor element with a groove produced in this way is covered by a second rotor element, for example, a continuous one, a capillary-like structure can be formed that is circumferentially closed or limited.

[0057] According to one embodiment, the at least one part may extend in the radial direction of the rotor device (see for example Figure 6 ). This allows a fluidic path to be kept advantageously short without losing the possibility of forming one or more further fluidic structures (in other planes) of the rotor device in a radial intermediate region.

[0058] According to one embodiment, the separation device can be designed as a chromatographic separation device, in particular as a chromatography separation column. In a chromatographic separation, the chromatography separation column can be provided with an adsorption medium. The fluid sample can be held on this adsorption medium and only subsequently removed fractionally with sufficient mobile phase (isocratic) or in the presence of a specific solvent composition (gradient), thus achieving the separation of the sample into its fractions.

[0059] The sample separation device can be a microfluidic instrument, a life science device, a liquid chromatography device, an HPLC (high-performance liquid chromatography), a UHPLC system, an SFC (supercritical fluid chromatography) device, a gas chromatography device, an electrochromatography device, and / or a gel electrophoresis device. However, many other applications are possible.

[0060] The fluid pump can, for example, be designed to pump the mobile phase through the system at a high pressure, for example a few hundred bar up to 1000 bar and more.

[0061] The sample separation device can have a sample injector for introducing the sample into the fluidic separation path. Such a sample injector can have an injection needle that can be coupled to a seat in a corresponding fluid path. The needle can be retracted from this seat to collect the sample. After reinserting the needle into the seat, the sample is located in a fluidic path that can be switched into the separation path of the system, for example, by switching a valve, leading to the introduction of the sample into the fluidic separation path.

[0062] The sample separation device can include a fraction collector for collecting the separated components. Such a fraction collector can, for example, direct the various components into different liquid containers. The analyzed sample can also be directed to a waste container.

[0063] Preferably, the sample separation device may include a detector for detecting the separated components. Such a detector may generate a signal that can be observed and / or recorded and is indicative of the presence and quantity of the sample components in the fluid flowing through the system. SHORT DESCRIPTION OF THE CHARACTERS

[0064] Other objects and many of the attendant advantages of embodiments of the present invention will be readily appreciated and better understood by reference to the following more detailed description of embodiments taken in conjunction with the accompanying drawings. Features that are substantially or functionally the same or similar are designated by the same reference numerals. Figure 1 shows an HPLC system according to an exemplary embodiment of the invention. Figure 2shows a three-dimensional exploded view of a fluid valve according to an exemplary embodiment of the invention. Figure 3 shows a three-dimensional exploded view of a rotor device of the fluid valve according to Figure 2 . Figure 4 shows a cross-sectional view of a stator or rotor of a fluid valve according to an exemplary embodiment of the invention. Figure 5 shows a cross-sectional view of a rotor device of a fluid valve according to an exemplary embodiment of the invention. Figure 6 shows a fluid processing device with a fluid valve according to an exemplary embodiment of the invention. Figure 7 to Figure 10 show grooves designed as functional fluid components of a rotor device of a fluid valve according to an exemplary embodiment of the invention. Figure 11shows a cross-sectional view of a three-layer fluid valve according to an exemplary embodiment of the invention. Figure 12 shows a three-dimensional view of a rotor device and part of a stator device of a fluid valve according to an exemplary embodiment of the invention. Figure 13 shows a three-dimensional view of a rotor device of a fluid valve according to another exemplary embodiment of the invention. Figure 14 shows a plan view of the rotor device according to Figure 13 .

[0065] The representation in the drawings is schematic.

[0066] Before exemplary embodiments are described with reference to the figures, some basic considerations will be summarized on the basis of which exemplary embodiments of the invention have been derived.

[0067] According to a first aspect of an embodiment of the invention, at least a portion of a surface (in particular at a contact surface between interacting valve components, at a bonding surface between individual bodies of a valve component, at a fluid structure of a valve component, etc.) of a valve component (in particular a stator device or a rotor device) is provided with a gold-containing and / or platinum-containing coating. This results in lubrication (in particular Au-Co lubrication in the case of hard gold) and compensating ability at the contact surface, biocompatibility of the fluid structures, mechanical robustness of the fluid valve, and bondability of individual elements of a valve component.

[0068] According to another aspect of an embodiment of the invention, fluid structures of a valve component (in particular a rotor device or a stator device) are guided in multiple planes (in particular at a contact surface and in the interior) of a valve component. This allows the density of fluid structures in a fluid valve to be increased, the complexity and number of functions to be increased, and thus the compactness of the system to be improved. At the same time, this leads to a shortening of the fluid paths and thus to a low dead volume of the fluid valve.

[0069] According to the invention, a fluid valve is provided which is designed as a rotor valve or shear valve. Further preferably, a surface portion, in particular of the rotor component, of such a rotor valve is provided with a gold plating. If the gold-containing coating is formed from hard gold, it can have a Vickers hardness of 160 HV ± 20 HV. Another surface area, in particular of the stator component of such a fluid valve, can be provided with a DLC (diamond-like carbon) coating. Preferably, a fluid valve is created in the following configurations: Teflon® or MoldFlon® on DLC (bioinert); PEEK on DLC (bioinert); gold on DLC or gold on gold (biocompatible).

[0070] Conventional shear valves for HPLC applications are typically constructed from three core components: a hard stator component, a generally softer rotor component, and one or more springs, particularly spring washers (force unit). Particularly at high fluid pressures (i.e., high contact forces), these technologies lead to limitations in terms of reliability and leak-tightness due, among other things, to suboptimal tribological conditions (pairings) either with regard to the soft component or (for example, with carbon fiber-filled PEEK on DLC) also with regard to the harder component, so that these components must be replaced more frequently. These technologies traditionally require frequent replacement of the soft component, in particular, due to heavy wear, as this can result in limitations in terms of reliability and leak-tightness.

[0071] In contrast, according to an exemplary embodiment of the invention, a fluid valve with a long service life and low wear is provided. In particular, a shear valve rotor and a shear valve stator are created in which a coating procedure and a special material selection can be carried out. This makes it possible to provide gold and / or DLC coatings on contact surfaces of such a rotor component or stator component, and to create a fluid valve with a long service life through such a coating. In particular, the coating of a contact surface of one of the valve components with a gold-containing and / or platinum-containing layer is provided in order to provide high reliability with regard to pressure stability. Furthermore, such a coating creates technical advantages with regard to bonding behavior, stability over a long service life and chemical robustness.Bioinertness or biocompatibility, which is particularly advantageous for sample separation applications.

[0072] When the coating is configured as a double layer, an inner layer (e.g., pre-gold) can, for example, have a thickness in a range between 0.1 µm and 5 µm, in particular between 0.15 µm and 0.5 µm. An outer layer (e.g., hard gold) can, for example, have a thickness in a range between 5 µm and 50 µm, in particular between 7 µm and 10 µm. The first layer can be a pure gold layer, whereas the second layer can be a hard gold layer.

[0073] If both opposing contact surfaces of the two valve components have a coating, it is advantageous to provide both contact surfaces with a gold-containing and / or platinum-containing coating. An alternative advantageous configuration is to provide a gold-containing and / or platinum-containing layer on one of the contact surfaces and coat it with a hard coating, for example, made of diamond or DLC, on the other valve component.

[0074] A first valve component, which can be designed in particular as a rotor component, can be configured to reduce wear and provide high fluid tightness, even under high pressure. Such a valve component can also be compatible with solvents such as those used in liquid chromatography. A bioinert or biocompatible property of such a valve component is also advantageous. Such a valve component can also ensure a long service life of a sealing element. In the event of a defect, such a valve component can also enable adequate drainage of escaping fluid.

[0075] With regard to the second valve component, which is preferably designed as a stator component, the described architecture allows the provision of highly flexible fluid connections for capillaries or the like, as well as the provision of check valves, helical windings, etc.

[0076] The formation of a valve component, which is preferably realized as a rotor component, can be achieved by initially manufacturing two (or more) rotor elements as separate bodies. A first rotor element can be formed with a groove on a front main surface and with a groove on a rear main surface. This rotor element can also have one or more holes in the form of passages or through-bores, with which the front main surface is fluidically coupled to the rear main surface. The other rotor element can be designed to cover and seal the rear main surface of the first rotor element by means of bonding. It is possible to coat the surfaces of metallic rotor elements with gold or a gold-containing material.The two rotor elements (e.g., metal parts) of the rotor assembly can then be bonded together to form a one-piece rotor assembly with a buried capillary (formed by the covered groove). Bonding the two rotor elements to each other can be carried out, in particular, by means of ultrasonic and / or thermocompression bonding. In thermobonding, the rotor elements (preferably previously surface-cleaned and / or surface-activated) are pressed together at elevated temperature or elevated pressure (optionally with the application of ultrasonic energy), thereby joining them to form a one-piece structure. In ultrasonic bonding, the formation of a one-piece structure can be promoted by applying ultrasound. It is also possible to attach a sealing element, for example, a PTFE sealing ring, to the rotor component.

[0077] Each of the two rotor elements can be made from one of the materials listed below: steel with gold plating; polyetheretherketone (PEEK) and / or carbon fiber-filled PEEK (thermally bondable); ceramic (bondable on both sides); solid Teflon material; Teflon® or MoldFlon® with perfluoroalkoxy polymer (PFA) (bondable on both sides), optionally filled or unfilled (bondable). The filling can be made with filler particles that increase the wear resistance and / or pressure stability of the respective valve component or rotor element.

[0078] The second valve component, preferably designed as a stator component, can be formed by coating the inner or exposed surfaces with DLC (diamond-like carbon) or another hard material. Alternatively, this surface can also be provided with a gold- and / or platinum-containing coating, like that of the rotor component.

[0079] Such a fluid valve achieves extensive compatibility with a wide range of solvents (e.g., organic solvents such as ethanol or inorganic solvents). Furthermore, unwanted sample carryover between consecutive analyses, measurements, or other fluid processing steps can be avoided with such a valve architecture. A fluid valve with a long service life can be created. Furthermore, the potential risk of loss of fluid sample material is mitigated with the described valve configuration. A further advantage of this architecture is that, due to the provision of a sealing element around a high-pressure sealing area, in the event of a leak, the discharge of escaping fluid can be precisely defined and channeled through a channel in the stator device.

[0080] Providing the rotor assembly with two rotor elements, one of which has grooves on opposing main surfaces and a connecting passage, offers additional advantages. In this way, fluidic functions such as restrictions, delay volumes, fixed volumes for injection, or superimposed functions on different rotor radii can be implemented on a main surface of the corresponding rotor element that is rearward relative to the stator component by means of a bridge-like decoupling of different fluid channels. In this way, complex fluidic structures can be provided with small dimensions. It is possible to work with fluid connections at different rotor diameters without having any restrictions on switching performance. The degree of freedom in the development of rotor seals is high.

[0081] Figure 1shows the basic structure of an HPLC system as an example of a sample separation device 10, such as can be used for liquid chromatography. A fluid pump 20 as a fluid drive device, which is supplied with solvents from a supply unit 25, drives a mobile phase through a separation device 30 (such as a chromatographic column) containing a stationary phase. A degasser 27 can degas the solvents before they are fed to the fluid pump 20. A sample introduction unit 40 with a switching valve or fluid valve 95 is arranged between the fluid pump 20 and the separation device 30 in order to introduce a sample liquid into the fluidic separation path. The stationary phase of the separation device 30 is intended to separate components of the sample.A detector, see flow cell 50, detects separated components of the sample, and an intermediate fractionator can be provided to dispense separated components of the sample into designated containers. Liquids no longer required can be discharged into a waste container 60.

[0082] A control unit 70 controls the individual components 20, 25, 27, 30, 40, 50, 60, 95 of the sample separation device 10. Configurations of the fluid valve 95 according to exemplary embodiments of the invention are described below with reference to the further figures.

[0083] Figure 2 shows a three-dimensional view of a fluid valve 95 according to an exemplary embodiment of the invention in an exploded view. Figure 3 shows a three-dimensional view of a rotor device 102 of the fluid valve 95 according to Figure 2 in an exploded view.

[0084] The fluid valve 95 is suitable, for example, for use in a sample separation device 10, such as the one shown in Figure 1 The fluid valve 95 has a first valve component, which is designed as a rotor device 102 and whose individual parts are Figure 3 are shown in more detail. The fluid valve 95 further comprises a second valve component, which is designed as a stator device 104 and interacts with the rotor device 102. The rotatable rotor device 102 and the stationary stator device 104 are movable relative to each other by a rotational movement of the rotor device 102 and are configured such that one or more switchable fluid channels 106 are formed between them (only partially shown in Figure 2). At least a portion of a contact surface 108 of the rotor device 102 and / or at least a portion of a contact surface 108 of the stator device 104 is or are preferably provided with a gold-containing coating 110. The contact surfaces 108 of the rotor device 102 and the stator device 104 are opposite one another and can contact one another in a high-pressure fluid-tight manner during operation of the fluid valve 95. More specifically, the gold-containing coating 110 can be formed from hard gold, which contains cobalt in a range between 0.2 weight percent and 0.3 weight percent, approximately 0.7 weight percent carbon, and otherwise essentially only gold (approximately 99 weight percent). It is particularly preferred if the coating 110 of the rotor device 102 contains gold and the coating 110 of the stator device 104 contains DLC (diamond-like carbon). This ensures good lubrication at the interface (i.e.the contact surfaces 108) between the valve components 102, 104 as a tribological pair and consequently low-friction operation of the fluid valve 95. In the event of minor misalignments between the two valve components 102, 104, the coating 110 provides a certain compensating ability and thereby further extends the service life of the fluid valve 95. In addition, the hardness of the DLC coating 110 ensures low abrasion and consequently low wear. In the area of ​​the fluid channels 106, the coating 110 creates a surface that is at least biocompatible and can withstand aggressive solvents and biological samples without corrosion or the undesirable generation of significant chemical interaction products. When the two in . Figure 3When the rotor elements 122, 124 shown are joined together by bonding to form a one-piece rotor device 102, the coating 110 between the rotor elements 122, 124 promotes the strength at their interfaces. To make these advantages particularly apparent and for reasons of ease of manufacture of the coatings 110 by non-selective deposition, the coating 110 can advantageously be formed on an entire surface of the rotor device 102 or the stator device 104.

[0085] By moving the rotor device 102 relative to the stator device 104, different fluid coupling states or fluid decoupling states of the at least one fluid channel 106 can be set. For example, fluid structures 166 (such as grooves, passages, closed fluid lines, etc.) of the rotor device 102 and corresponding fluid structures 168 (not shown in Figure 2, for example grooves, closed fluid lines, fluid connections, etc.) of the stator device 104 can be fluidically coupled to one another or fluidically decoupled from one another in different switching states. As shown in Figure 2 As shown, the stator device 104 has fluid connections 120 (also referred to as ports) to which Figure 2 fluid components not shown (for example injector 40, fluid pump 20, separating device 30, cf. Figure 1 ) can be fluidically connected. This can be achieved, for example, using capillary connections and a suitable fitting (not shown). According to Figure 2 Furthermore, an annular sealing element 130 is inserted into a corresponding annular groove 133 of the rotor device 102.

[0086] As in Figure 3As shown, the rotor-side part of the at least one fluid channel 106 can be formed by the fluid structures 166, which are formed in the first rotor element 122 and a part of which is delimited by the second rotor element 124 by covering. For this purpose, the first rotor element 122 can be arranged at its Figure 3 lower main surface are bonded to the second rotor element 124 to form the one-piece rotor device 102 and are thereby covered by it. The fluid structures 166 contain (here tangential) grooves 118 on a Figure 3 upper main surface of the rotor device 102, vertical passages 126 between the two main surfaces and a (here radial) line section 128. The line section 128 is formed by a groove in the Figure 3lower main surface of the first rotor element 122 and a main surface of the second rotor element 124 adjacent thereto in the assembled state. Ends of the passages 126 and ends of the conduit section 128 are fluidically connected to one another or coincide, forming a U-shaped cavity.

[0087] Although in Figure 3 not shown, the stator-side part of the at least one fluid channel 106 can be connected by at least two fluid connections 120 (see Figure 2 ) may be formed on the stator device 104. In different switching states of the fluid valve 95, the fluid connections 120 can be brought into different fluidic coupling states (ie, fluidically coupled or fluidically decoupled) with the grooves 118 or the upper ends of the passages 126.

[0088] As in Figure 3As shown, the rotor device 102 is formed by a disc-shaped first rotor element 122 and a disc-shaped second rotor element 124, which can be joined to form a one-piece body by means of ultrasonic and / or thermocompression bonding to form the rotor device 102. As shown in Figure 3As can be seen, the first rotor element 122, which has the line section 128, the grooves 118, and the passages 126, defines a part of the at least one fluid channel 106, whereas the second rotor element 124, in the exemplary embodiment shown, provides a continuous cover for the first rotor element 122. The grooves 118, on the one hand, and the line section 128, on the other hand, extend over different radial and tangential regions and in planes of the rotor device 102 that are axially offset from one another. Since the grooves 118 and the line section 128 extend in different axial planes of the rotor device 102, they always remain fluidically decoupled, although they can extend over overlapping radial and / or tangential regions. In this way, it is possible to compactly integrate complex fluidic structures into the rotor device 102.In other words, the described architecture of different recesses in different axial planes of the rotor device 102 makes it possible to form different fluidic structures 106 in different diameter ranges of the rotor device 102 in a compact manner and while reliably maintaining fluidic decoupling. In other words, this is achieved by offsetting a portion 170 of the fluid structures 166 of the rotor device 102 relative to the planar contact surface 108 in the axial direction 164 relative to a rotation axis 162. As a result, this portion 170 and another portion 172 of the fluid structures 166 overlap at the contact surface 108 of the rotor device 102 when viewed along the axial direction 164.The first valve component, designed as a rotor device 102, can rotate in a direction of rotation 163 (or in the opposite direction) during switching operation in order to form different fluidic coupling states with the stator device 104. The part 170 of the fluid structures 166 of the rotor device 102 is located at the position shown in FIG. Figure 3 lower main surface of the first rotor element 122, whereas the other part 172 of the fluid structures 166 of the rotor device 102 is located at the Figure 3 upper main surface of the first rotor element 122 and therefore directly adjacent to the contact surface 108 of the stator device 104 of the fluid valve 95.

[0089] How best in Figure 3As can be seen, the fluid valve 95 further comprises a leak sealing element 130, which is arranged for fluidic sealing between the rotor device 102 and the stator device 104. For this purpose, the sealing element 130, designed as a leak sealing ring, can be inserted into the annular groove 133 of the rotor device 102. The sealing element 130 can be made, for example, from polytetrafluoroethylene (PTFE) or a PTFE and EPDM composite or another tribological pair.

[0090] Figure 4 shows a cross-sectional view of a fluid valve 95 according to an exemplary embodiment of the invention.

[0091] As a detail 131 in Figure 4 As can be seen, the coating 110 of the rotor device 102 (alternatively or additionally to the stator device 104) can have several layers 112, 114. According to Figure 4A first layer 112 of pure gold is formed directly on a base body 116 (made of steel) of the rotor device 102. A second layer 114 on the first layer 112 comprises hard gold. In contrast, detail 137 in Figure 4 that the coating 110 of the stator device 104 (alternatively or additionally to the rotor device 102) can be formed as a monolayer on a base body 116 (for example, also made of steel). The monolayer can comprise, for example, hard gold, DLC, or diamond. It is possible for one or both valve components 102, 104 to be coated with exactly one or more layers 112, 114, and for these coatings 110 to be identical or different. The combinations hard gold-hard gold and hard gold-DLC are particularly preferred.

[0092] Figure 4shows that all exposed surfaces of the stator device 104, which forms the second valve component, and of the rotor device 102, which forms the first valve component, are covered with the respective coating 110. In other words, the respective coating 110 is produced using a method (e.g., vapor deposition, chemical vapor deposition, PACVD, etc.) in which the coating 110 is formed on the respective valve component 102, 104 by means of a non-selective deposition process. This is simple in terms of manufacturing technology, since the coating can then be carried out using a simple process. A selective coating of only certain surface areas is then unnecessary. The coating 110 has advantageous effects not only on the contact surfaces 108, but also on the surfaces of the fluid structures 166, 168, as described above.

[0093] Also according to Figure 4In projection onto the vertical axis there are shown overlapping and axially offset fluid structures 166, 168, which are fluidically decoupled from each other. As a result, the fluid valve 95 is Figure 4 compact, flexible design, shows high fluid technology performance and allows short fluid paths.

[0094] Figure 5 shows a cross-sectional view of a first valve component of a fluid valve 95 designed as a rotor device 102 according to an exemplary embodiment of the invention.

[0095] Figure 5 shows how two rotor elements 122, 124 of the first valve component 102 form an integral one-piece body after being attached to each other by ultrasonic and / or thermocompression bonding.

[0096] In the fluid valve 95 according to Figure 5 lies the (with a Figure 5Opposite the contact surface 108 of the rotor device 102 (which cooperates fluid-tight with the second valve component 104 (not shown), as another part of an inner surface of the rotor device 102, is a parallel counter-surface 183 with a fluid structure 166. The counter-surface 183 delimits the rotor element 122 and bears against the rotor element 124. Both the fluid structures 166 and the counter-surface 183 are provided with a gold-containing and / or platinum-containing coating 110.

[0097] The mating surface 183 of the rotor element 122 is thermally bonded and / or ultrasonically bonded to the coating 110 with a cover body in the form of the rotor element 124. The ability of the rotor elements 122, 124 to be securely joined to one another by thermal bonding (i.e., pressing them together at elevated temperature or increased energy input) and / or ultrasonic bonding (i.e., bonding by applying ultrasound) is significantly increased by the gold-containing and / or platinum-containing coating 110. This also increases the pressure stability of the fluid valve 95.

[0098] By covering the walls of the rotor element 122, which define the fluid structures 166 and consequently also a portion of the fluid lines 106, with the gold-containing and / or platinum-containing coating 110, biocompatible fluid lines 106 are created. These allow the transport of even aggressive fluids (e.g., solvents or biological fluids) without damaging the fluid valve 95 or the fluids. Such a coating 110 made of the inert precious metal gold also significantly suppresses corrosion of the fluid valve 95.

[0099] Figure 6 shows a fluid processing device 111 with a fluid valve 95 according to an exemplary embodiment of the invention.

[0100] A needle 141 is arranged in a seat 143 and can be moved out of it (not shown) to draw fluidic sample from a sample container (not shown) and, after retracting into the seat 143, inject it via the fluid valve 95 into a fluidic path with a fluidic reactor 199. When the sample is drawn in by the needle 141, the sample can be temporarily stored in an intermediate storage volume 147, a so-called sample loop. The drawing in of the sample can be accomplished by a metering pump 149. A piston of the same can move back in a piston chamber for drawing in and forward for injection. Furthermore, Figure 6a waste 165, a fluid restriction 167, check valves 169, and a liquid container 171 are shown. To operate the fluid processing device 111, the fluid valve 95 is provided with grooves 118 and fluid connections 120, which are arranged in a rotor device 102 and a stator device 104 in different planes. In particular, a line section 128 as part 170 of fluid lines 106 is arranged opposite a paper plane of Figure 6 downwards, whereas another part 172 of the fluid lines 106 is also in the plane of the paper from Figure 6can extend. In particular, by arranging the radially extending groove corresponding to line section 128 in a different axial plane than the fluid connections 120 according to part 172 (and than the tangential grooves 118 between the fluid connections 120), rotational switching of the fluid valve 95 is enabled without the line section 128 according to part 170 being undesirably fluidically coupled for a time to time with the fluid connections 120 according to the other part 172.

[0101] Figure 7 to Figure 10 show grooves 118 designed as functional fluid components of a rotor device 102 of a fluid valve 95 according to an exemplary embodiment of the invention. Figure 7 to Figure 10show which additional fluidic functions a groove 118 can fulfill, which can be arranged in a main surface of the rotor device 102 facing away from the stator device 104. By means of a corresponding fluid channel 106, for example, at least one function from a group consisting of a fluidic restriction, a fluidic delay device for delaying a fluid flow, an intermediate storage volume for temporarily storing a predefined amount of fluid, and a fluidic mixing device, etc., can be provided.

[0102] According to Figure 7 A fluidic intermediate storage volume is provided. A fluidic restriction by a locally reduced groove diameter is Figure 8 shown. In Figure 9A mixing device is provided which provides several fluidic paths of different diameters and different lengths between two fluid connections 126, so that different fluid portions coupled into the different paths can be mixed by different running times. According to Figure 10 A fluidic delay device is created because the path between the two fluid connections 126 is artificially extended by a spiral groove compared to a linear direct connection.

[0103] Figure 11 shows a cross-sectional view of a fluid valve 95 according to an exemplary embodiment of the invention.

[0104] In Figure 11 It is shown that a rotor device 102 can also be formed by more than two rotor elements 122, 124 (here by three bonded rotor elements 122, 124, 199). In addition, according to Figure 11a third rotor element 199 is provided, which enables the formation of even more complex fluidic structures.

[0105] Figure 12 shows a three-dimensional view of a rotor device 102 and a part of a stator device 104 of a fluid valve 95 according to an exemplary embodiment of the invention.

[0106] The Figure 12 The fluid valve 95 shown is also designed for operation with a sample separation device 10 and has a rotor device 102 shown in detail with fluid structures 166. Only partially and schematically shown is a stator device 104 cooperating with the rotor device 102 with fluid structures 168, of which Figure 12only one fluid connection 120 is shown. As in the previously described embodiments, the rotor device 102 and the stator device 104 are coupled to each other in a fluid-tight manner at corresponding contact surfaces 108 and are rotatable relative to each other about a rotation axis 162 (see rotation arrow 193). Although this is described in detail in Figure 12 Not shown, in certain rotational states, a fluid channel 106 extending through the contact surface 108 can be formed by means of the fluid structures 166, 168. The fluid structures 168 of the stator device 104 used for this purpose, namely further fluid connections 120 aligned with outlet openings 191 (on radius R1 or R2) of the fluid structures 166 of the rotor device 102 on the contact surface 108, are shown in Figure 12 not shown.

[0107] A part 170 of the fluid structures 166 of the rotor device 102 is offset in the axial direction 164 relative to the rotation axis 162 with respect to the contact surface 108, so that in at least one rotational state of the fluid valve 95, this part 170 and another part 172 of the fluid structures 168 of the stator device 104 (namely the part 172 shown in Figure 12 shown fluid connection 120 on radius R3) when viewed along the axial direction 164 overlap or even align. This is the case when, compared to the illustration according to Figure 12 the rotor device 102 and the stator device 104 have been rotated relative to each other by an angle α. In the latter rotational state, the part 170 and the other part 172 overlap or are aligned when viewed along the axial direction 164, without being fluidly coupled to each other.

[0108] Although this is Figure 12Not shown, the passage of the fluid structures 166 of the rotor device 102 along an interior of the rotor device 102 also allows the other part 172 to be formed by a plurality of fluid connections 120 of the stator device 104, which can be arranged on at least two different radii relative to the rotation axis 162. A configuration with fluid connections 120 on different radii is shown, for example, in Figure 6 shown.

[0109] According to Figure 12 Part 170 extends from a first radius R1 to a second radius R2 of the rotor assembly 102. The other part 172 is arranged at a third radius R3, which is greater than the first radius R1 and smaller than the second radius R2. The radii R1, R2, R3 are all relative to the rotation axis 162.

[0110] As in Figure 5 can also be Figure 12One part 170 may be formed by a groove 118 in a first rotor element 122 of the rotor device 102, which groove 118 is covered by a second rotor element 124. In this way, a capillary or fluidic path can be formed in the interior of the rotor device 102, which is completely bounded by the material of the rotor device 102, with little manufacturing effort.

[0111] The axially offset portion 170 of the fluid structures 166 can extend in the radial direction of the rotor device 102 and yet does not limit the design freedom to provide fluid connections 120 of the stator device 104 at any desired radii. Thus, regardless of the extension of the portion 170 over a large radial area, the rotor device 102 can be provided and freely moved along any attachable fluid connections 120 of the stator device 104 without temporarily causing an undesirable fluidic coupling between the illustrated fluid structures 166 and 168 during switching.

[0112] At least a part of the contact surface 108 of at least one of the rotor device 102 and the stator device 104 can also be formed according to Figure 12 be provided with a coating 110, as described with reference to Figure 2 to Figure 5 described.

[0113] Figure 13shows a three-dimensional view of a rotor device 102 of a fluid valve 95 according to another exemplary embodiment of the invention. Figure 14 shows a plan view of the rotor device 102 according to Figure 13 .

[0114] In the fluid valve 95 according to Figure 13 and Figure 14 The other part 172 also belongs to the fluid structures 166 of the rotor device 102. The other part 172 is further offset from the part 170 of the fluid structures 166 of the rotor device 102 in the axial direction 164 relative to the rotation axis 162 relative to the contact surface 108. More precisely, the other part 172 of the fluid structures 166 is arranged at the contact surface 108 and in the plane of the paper according to Figure 14 The part 170 is designed as a radially extending section of one of the fluid structures 166, which is below the paper plane according to Figure 14The other part 172 is formed as a circular ring segment of another of the fluid structures 166. More precisely, according to Figure 13 and Figure 14 the other part 172 of the fluid structures 166 a groove 118 of the rotor device 102 at the contact surface 108. The fluid structures 166 of the rotor device 102 also have two passages 126 that are parallel to one another and extend in the axial direction 164 through the rotor device 102 from the contact surface 108 to the part 170. The passages 126 and the part 170 thus form a substantially U-shaped bypass for the at least one other part 172, which is fluidically decoupled from the part 170. This makes it possible for a first fluid to flow through the part 170, while independently a second fluid flows through the other part 172. The associated fluidic channels are accommodated in a very small space and allow a compact design.

[0115] The axially offset portion 170 of the fluid structures 166 can extend in the radial direction of the rotor device 102 and yet does not limit the design freedom to provide the other portion 172 of the fluid structures 166 at any desired radii. Thus, regardless of the extension of the portion 170 over a large radial area, the other portion 172 of the rotor device 102 can be provided along essentially any desired spatial region without creating an undesirable fluidic coupling between the illustrated fluid structures 166 and 168.

[0116] At least a part of the contact surface 108 of at least one of the rotor device 102 and the stator device 104 can also be formed according to Figure 13 and Figure 14 be provided with a coating 110, as described with reference to Figure 2 to Figure 5 described.

Claims

1. A fluid valve (95) for a sample separation device (10), wherein the fluid valve (95) comprises: a first valve component (102); a second valve component (104); wherein the first valve component (102) and the second valve component (104) adjoin each other, are rotatable or longitudinally displaceable relative to each other, and are configured such that in at least one switching state at least one switchable fluid channel (106) is formed between them; wherein the at least one fluid channel (106) is formed of at least one groove (118) in the first valve component (102) and at least two fluid ports (120) at the second valve component (104), and wherein in different switching states of the fluid valve (95) the fluid ports (120) can be brought into different fluidic coupling states with respect to the at least one groove (118); wherein at least a part of a surface of at least one of the first valve component (102) and the second valve component (104) is provided with a gold-containing and / or platinum-containing coating (110); wherein the fluid valve (95) is a shear valve, wherein the first valve component (102) comprises a contact surface (108) as part of its surface and the second valve component (104) comprises a contact surface (108) as part of its surface, wherein the first valve component (102) and the second valve component (104) adjoin each other at the contact surfaces (108), and wherein at least a part of the contact surface (108) of at least one of the first valve component (102) and the second valve component (104) is provided with the gold-containing and / or platinum-containing coating (110), so that a lubrication between the first valve component (102) and the second valve component (104), a balance of the valve components and a low-wear operation are promoted.

2. The fluid valve (95) according to claim 1, wherein the coating (110) is formed at at least an entire one of the contact surfaces (108) between the first valve component (102) and the second valve component (104).

3. The fluid valve (95) according to claim 1 or 2, wherein the coating (110) is formed at the contact surface (108) of the first valve component (102) and at the contact surface (108) of the second valve component (104).

4. The fluid valve (95) according to one of the claims 1 to 3, wherein the contact surface (108) of at least one of the first valve component (102) and the second valve component (104) as another part of the surface is opposed by a counter surface (183) with at least one fluid structure (166, 168) with another part of the surface.

5. The fluid valve (95) according to claim 4, wherein at least a part of at least one of the fluid structures (166, 168) and / or the counter surface (183) is provided with the gold-containing and / or platinum-containing coating (110).

6. The fluid valve (95) according to claim 5, wherein the counter surface (183) is bonded to the coating (110) with a cover body (124).

7. The fluid valve (95) according to one of the claims 1 to 6, wherein at least a part of the coating (110) comprises or consists of hard gold; and / or wherein at least a part of the coating (110) comprises cobalt in a range between 0.05 weight percent and 1 weight percent, in particular in a range between 0.2 weight percent and 0.3 weight percent, up to 0.7 weight percent carbon, and otherwise gold.

8. The fluid valve (95) according to one of the claims 1 to 7, comprising at least one of the following features: wherein the first valve component (102) and the second valve component (104) are provided with different coatings (110); wherein the coating (110) comprises a plurality of layers (112, 114), wherein in particular a first layer (112) of the coating (110) is formed directly on a base body (116) of the respective valve component (102, 104), and further in particular comprises pure gold, and a second layer (114) is formed on the first layer (112), and further in particular comprises hard gold; wherein a base body (116) of at least one of the valve components (102, 104), on which the coating (110) is arranged, comprises metal, in particular steel; wherein the first valve component (102) and the second valve component (104) are movable relative to each other such that thereby at least two different fluid coupling states of the at least one fluid channel (106) are adjustable; wherein the first valve component (102) is formed as a rotor unit and the second valve component (104) is formed as a stator unit, wherein the rotor unit and the stator unit are rotatable relative to each other.

9. The fluid valve (95) according to one of the claims 1 to 8, wherein the first valve component (102) comprises a first rotor element (122) and a second rotor element (124), in particular bonded to each other, wherein the first rotor element (122) defines at least one part (170, 172) of the at least one fluid channel (106) and wherein the second rotor element (124) forms a cover of the first rotor element (122), in particular wherein the first rotor element (122) comprises as at least one part (172) of a first fluid channel (106) a groove (118) on one of the two opposing main surfaces of the first rotor element (122) and as at least one part (170) of a second fluid channel (106) at least one passage (126) through the first rotor element (122) and another groove (118) fluidically coupled therewith on the other one of the two opposing main surfaces of the first rotor element (122).

10. The fluid valve (95) according to one of the claims 1 to 9, comprising at least one of the following features: wherein the first valve component (102) comprises as at least one part (172) of a first fluid channel (106) a groove (118) on a main surface of the first valve component (102) facing the second valve component (104) and as at least one part (170) of a second fluid channel (106) at least one passage (126) through at least one part of the first valve component (102) and a conduit section (128) fluidically coupled therewith, wherein in particular the groove (118) on the one hand and the conduit section (128) on the other hand extend over different, in particular overlapping, regions, in particular radial regions, of the first valve component (102); comprising a sealing element (130), which is arranged for sealing between the first valve component (102) and the second valve component (104), wherein the sealing element (130) is in particular a sealing ring and / or comprises or consists of polytetrafluoroethylene, a polytetrafluoroethylene-ethylene-propylene-diene composite or a perfluoroelastomer, in particular nanoactivated; wherein at least one of the first valve component (102) and the second valve component (104) comprises at least one material from a group consisting of a metal, a plastic, in particular with filler particles or without filler particles, and a ceramic; wherein in different diameter regions of the first valve component (102) different fluidic structures (106) are formed; wherein by means of the at least one fluid channel (106) at least one fluidic function from a group consisting of a fluidic restriction, a fluidic delay unit for delaying a fluid flow, an intermediate storage volume for intermediate storing of a predefined fluid quantity, and a fluidic mixing device is provided.

11. The fluid valve (95) according to one of the claims 1 to 10, wherein at least one part (170) of at least one fluid structure (166) of the first valve component (102) is offset in an axial direction (164) with respect to the contact surfaces (108), so that in at least one switching state of the fluid valve (95) this part (170) and at least another part (172) of at least one fluid structure (166, 168) of the first valve component (102) and / or the second valve component (104) at least partially overlap when viewed along the axial direction (164), in particular comprising at least one of the following features: wherein in the at least one switching state, in which the at least partial overlap occurs, the at least one part (170) and the at least another part (172) are fluidically decoupled from each other; wherein the at least one another part (172) is formed by at least one fluid port (120) of the second valve component (104) formed as a stator unit; wherein the at least one another part (172) of the at least one fluid structure (166) is associated to the first valve component (102) formed as a rotor unit and is offset in the axial direction (164) with respect to the at least one part (170) of the at least one fluid structure (166) of the rotor unit.

12. A sample separation device (10) for separating a fluidic sample, wherein the sample separation device (10) comprises: a fluid drive (20) for driving the fluidic sample located in a mobile phase; a fluid valve (95) according to one of the claims 1 to 11 for introducing the fluidic sample into the mobile phase; a sample separation unit (30) for separating the fluidic sample located in the mobile phase.

13. The sample separation device (10) according to claim 12, further comprising at least one of the following features: the sample separation unit (30) is formed as a chromatographic separation unit, in particular as a chromatographic separation column; the sample separation device (10) is configured for analyzing at least one physical, chemical and / or biological parameter of at least one fraction of the fluidic sample; the sample separation device (10) comprises at least one from the group consisting of a detector device, a device for chemical, biological and / or pharmaceutical analysis, a liquid chromatography device and an HPLC device; the fluid drive (20) is configured for driving the mobile phase at a high pressure; the fluid drive (20) is configured for driving the mobile phase at a pressure of at least 100 bar, in particular of at least 500 bar, further in particular of at least 1000 bar; the sample separation device (10) is configured as a microfluidic device; the sample separation device (10) is configured as a nanofluidic device; the sample separation device (10) is configured as a preparative device; the sample separation device (10) comprises an injector unit (40) with the fluid valve (95) for introducing the fluidic sample into a fluidic path between the fluid drive (20) and the sample separation unit (30); the sample separation device (10) comprises a detector (50), in particular a fluorescence detector or UV absorption detector, for detecting the separated fluidic sample; the sample separation device (10) comprises a sample fractionator or a drain container (60) for fractionating the separated fluidic sample.

14. A method for manufacturing a fluid valve (95) for a sample separation device (10), wherein the method comprises: providing a first valve component (102) and a second valve component (104) such that they adjoin each other and are rotatable or longitudinally displaceable relative to each other; forming the first valve component (102) and the second valve component (104) such that between them in at least one switching state at least one switchable fluid channel (106) is formed, wherein the at least one fluid channel (106) is formed of at least one groove (118) in the first valve component (102) and at least two fluid ports (120) at the second valve component (104), and wherein in different switching states of the fluid valve (95) the fluid ports (120) can be brought into different fluidic coupling states with respect to the at least one groove (118); providing at least a part of a surface of at least one of the first valve component (102) and the second valve component (104) with a gold-containing and / or platinum-containing coating (110); wherein the fluid valve (95) is a shear valve, wherein the first valve component (102) comprises a contact surface (108) as part of its surface and the second valve component (104) comprises a contact surface (108) as part of its surface, wherein the first valve component (102) and the second valve component (104) adjoin each other at the contact surfaces (108), and wherein at least a part of the contact surface (108) of at least one of the first valve component (102) and the second valve component (104) is provided with the gold-containing and / or platinum-containing coating (110), so that a lubrication between the first valve component (102) and the second valve component (104), a balance of the valve components and a low-wear operation are promoted.

15. The method according to claim 14, wherein the coating (110) is formed by a non-selective deposition process on the respective valve component (102, 104).