Precursor material production apparatus and method for producing precursor materials for high-purity, large-volume and homogeneously or heterogeneously doped optical fiber preforms

A continuous fluidic system with a micromixer addresses the challenges of producing high-purity, large-volume optical fiber preforms by ensuring homogeneous or heterogeneous doping, achieving consistent quality and reproducibility in industrial-scale fiber production.

WO2026041188A1PCT designated stage Publication Date: 2026-02-26LEIBNIZ INST FUR PHOTONISCHE TECHN E V ENGL LEIBNIZ INST OF PHOTONIC TECH
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Patent Information

Application Number
PCT/DE2025/100746
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-08-23
Filing Date
2025-08-06
Publication Date
2026-02-26

AI Technical Summary

Technical Problem

Existing methods for producing optical fiber preforms face challenges in achieving high-purity, large-volume, and homogeneous or heterogeneous doping, leading to material inhomogeneities, reproducibility issues, and quality problems in industrial-scale fiber production, particularly due to batch-based precipitation processes and complex, costly sol-gel processes.

Method used

A continuous fluidic system using a fluidic micromixer combines reactants and dopants in a controlled manner, enabling homogeneous or heterogeneous doping of precursor materials for optical fiber preforms, ensuring reproducibility and automation, with precise control over synthesis conditions.

Benefits of technology

The solution allows for the production of high-purity, large-volume precursor materials with consistent quality, facilitating the production of high-quality optical fibers with high throughput and flexibility in material composition, suitable for industrial-scale automation.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to a precursor material production apparatus and to a method using same for producing precursor materials for high-purity, large-volume and homogeneously doped optical fiber preforms. The invention relates to a precursor material production apparatus and to a method using same for producing precursor materials for high-purity, large-volume and homogeneously or deliberately heterogeneously doped optical fiber preforms, which enable homogeneous doping in optical fiber preforms when the constituents of the precursor material are being mixed, such that no quality problems arise in the optical fibers drawn from the preforms. The invention is characterized in that a reactant (211) in the form of a first constituent and a suspension (221) in the form of a second constituent of the precursor material (6) are mixed in the precursor material production apparatus so that the first constituent can be fed via a first inlet opening (3a) and the second constituent can be fed via at least one further inlet opening (3b) to a mixing system (3) in a manner that allows metering, with the result that the first constituent and the second constituent are mixed in the mixing system (3) into a mixed material that is homogeneously or deliberately heterogeneously enriched with the dopant and that can be fed for further processing as precursor material (6), wherein the apparatus (1) is a microfluidic system which comprises at least two reservoirs (21) for the reactant (211) and the suspension (221), and at least two fluid channels (2), wherein each fluid channel (2) runs out of a reservoir (21) and, via the inlet openings (3a, 3b), into the mixing system (3), where the reactant (211) and the suspension (221), each of which is in a fluid, are intimately mixed in the form of the mixed material (6), wherein the mixer (3) is a fluidic micromixer.
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Description

[0001]

[0002] Precursor material manufacturing device and method for producing precursor materials for high-purity, large-volume and homogeneously or heterogeneously doped optical fiber preforms

[0003] The invention relates to a precursor material manufacturing device and a method for producing precursor materials for high-purity, large-volume and homogeneously or heterogeneously doped optical fiber preforms according to the preamble of the claims.

[0004] Currently, various established methods exist for producing mostly small-volume, high-purity fiber core materials; the most established of these is, for example, modified chemical vapor deposition (MCVD, including the variants solution doping and gas phase doping).

[0005] This process produces material quantities typically < 9 mm in diameter and approximately 30 cm in length, corresponding to volumes < 20 cm or masses < 50 g.

[0006] Such materials typically exhibit significant material inhomogeneities, particularly concentration fluctuations both radially and longitudinally. Furthermore, the layer-by-layer material build-up during the deposition of larger quantities of material leads to radial periodic fluctuations in refractive index and dopant concentration along the cross-section. Specific refractive index profiles of certain fiber types, such as large-mode-area (LMA) fibers and multi-chain fibers, are generally produced via a process called stacking, a predefined stacking / arrangement of many appropriately doped rods to form a preform. Obtaining the required material quantities for manufacturing such stacks necessitates numerous individually produced MCVD preforms, each of which must be individually evaluated and selected for compatibility – a significant drawback of this technical solution.

[0007] Particle-based processes for the production of doped preforms, such as the process according to EP 2 215 025 Bl, utilize a chemical precipitation step in a discontinuous, open system. Typically, an acidic, aqueous nanoparticle suspension mixed with water-soluble substances is dropwise added to an ammoniacal precursor. Due to the volumes involved, a continuous change in pH conditions (similar to a titration) occurs during the precipitation step; that is, the first drop experiences a different pH environment than the last.

[0008] In addition, there are mixing states that vary depending on the container shapes used, filling levels, stirrers, etc., and the suspensions used (viscosities, densities, solids and salt contents), and are not reproducible.

[0009] In particular, the volume differences of the droplet and the receiving medium, on the order of 1:1000, are a disadvantage of this technical solution, as local concentration gradients form in the time between initial contact and complete mixing in the receiving medium. These gradients temporarily promote sometimes pronounced increases in concentration compared to the targeted concentration, which can subsequently lead to undesirable accumulations (so-called clustering) that cannot be resolved by subsequent processing steps of the precursor materials.

[0010] Furthermore, this process requires precipitation to be carried out at a much higher pH value than would be necessary for efficient precipitation.

[0011] In contrast, a reduction of the NH3 content in the feedstock leads to a reduction in the homogeneity of the precipitated, doped suspension and an increase in the radial and longitudinal inhomogeneities in the processed end product in the conventional process according to EP 2 215 025 Bl.

[0012] Sol-gel-based processes, due to their costly raw materials, often very long drying times (for solid / monolith production), or multi-step processing to achieve solid material (for powder-based routes), are only feasible for single preforms. A major disadvantage is the uncontrollable risks that can arise during the required, lengthy drying phase of monolith production, such as cracking in the green body or incomplete removal of organic matter from the resulting pores.

[0013] Although infiltration of phase-separated, melt-derived glasses is in principle suitable for the production of large-volume fiber preforms, it is only conditionally scalable and automatable for such materials due to the unavoidable impurities (e.g. from the crucible materials), interfering ions (from glass melt, necessary for phase separation) and the elaborate, complex production process, and is not fully controllable with regard to purity and homogeneity.

[0014] The aforementioned problems of the particle-based liquid doping process lead to poor quality of the precipitation process with a lack of reproducibility, resulting in precursor materials that often exhibit insufficient doping homogeneity for high-purity and large-volume optical fiber preforms, which consequently causes problems when warping the fiber preform into an optical fiber, especially on an industrial scale.

[0015] Based on this prior art, the object of the present invention is to provide a precursor material production device and a method for producing precursor materials for high-purity, large-volume and homogeneously or heterogeneously doped optical fiber preforms, which does not have the aforementioned disadvantages of the prior art, in particular when mixing components of the precursor material, and thus enables homogeneous or targeted heterogeneous doping in optical fiber preforms, so that no quality problems arise in the optical fibers drawn from the preforms, in particular not in industrial production and with large quantities of material (>150 g batches).Furthermore, the process is intended to produce large quantities of material (>150 g batches) in a continuous, efficient synthesis process, independent of batch size, with high reproducibility, automation, and pinpoint accuracy with regard to synthesis conditions and resulting material properties. This allows for automated integration into the manufacturing processes of drawn, high-quality optical glass fibers. Highly pure (nano-) particles and / or particle agglomerates in large quantities are functionalized with dopants and additives in a particularly homogeneous or specifically heterogeneous manner. These can then be used as precursor materials for the production of glass fiber preforms. From these preforms, high-quality optical fibers can then be efficiently produced with high production throughput using known drawing processes. Simultaneously, this enables the cost-effective, continuous production of fiber preform materials within the overall manufacturing process.

[0016] According to the invention, this problem is solved by the features of claims 1 and 14.

[0017] Further advantageous embodiments of the invention are specified in the dependent claims. These can be combined with one another in a technologically meaningful manner.

[0018] The essence of the invention lies in the fact that, in the precursor material production device and in the process using this device, a targeted combination of the intended starting reactants with a desired high mass fraction (dissolved species and / or nanoparticles) on a small volume takes place in a continuous reaction process in a fluidic system in the form of a flow cell with a mixer under defined, composition-specific conditions (such as pH value, temperature, viscosity).

[0019] This precursor material production device is used in particular for carrying out the mixing of several process fluids containing dissolved or suspended reactants, dopants, additives, or precursor materials in continuous processes, such as in manufacturing processes for drawn optical glass fibers of the highest quality. Highly pure (nano-)particles and / or particle agglomerates in large quantities and in a particularly homogeneous or specifically heterogeneous manner are functionalized with dopants and additives and can thus be used as precursor materials for the production of glass fiber preforms. From these, optical fibers of the highest quality can then be efficiently produced with high production throughput using known drawing processes, and at the same time, cost-effective production of fiber preform materials can be continuously enabled within the overall manufacturing process.for adjusting pH, complexation or viscosity during ongoing manufacturing processes.

[0020] According to the invention, a precursor material manufacturing device for producing a precursor material for a high-purity, large-volume, and homogeneously or selectively heterogeneously doped optical fiber preform is provided, wherein a fluid-carried solid in nanoparticle form, with or without dopants or additives dissolved in the fluid, is introduced as the first component (hereinafter referred to as "suspension") via a first fluidic inlet channel of a fluidic system, and one or more fluid-carried dopants and / or additives are introduced as the second component (hereinafter referred to as "reactant") via at least one further fluidic inlet channel of a fluidic system, each in a metered manner, into a mixing system, such that the first component and all further components mix homogeneously or selectively heterogeneously in the mixing system to form a particle mixture variably enriched with the dopants and reactants.which can be supplied as a starting material in the form of a precursor material for further processing, wherein the mixing system is advantageously a fluidic micromixer and particularly advantageously a fluidic micromixer in the form of a flow-through mixing cell. Both the suspension and the reactant are advantageously held in separate reservoirs to continuously enter the respective fluid channels.

[0021] In this process, solid-carrying fluids such as SiO2 particle mixtures are used, which are designed as a liquid suspension.

[0022] The doping of the SiO2 particle mixtures can be carried out by adding fluorides and fluorine-containing compounds or one or more nitrides or oxides (or, in further processing, oxide-forming additives) of the following group of elements as dopants: Li, Be, B, Na, Mg, Al, Si, P, K, Ca, Sc, Ti, V, Cr, Mn, Co, Ni, Zn, Ga, Ge, As, Se, Rb, Sr, Y, Zr, Nb, Mo, Tc, Ru, Rh, Cd, In, Sn, Sb, Te, Cs, Ba, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, Re, Os, Ir, TI, Pb, Bi, Ac, Cu, Pt, Au, Ag, Pd.

[0023] The device according to the invention produces the mixture as a precursor material for further processing, so that it is either homogeneously mixed or specifically heterogeneously mixed depending on the objective, but can also be variably enriched with respect to the dopants.

[0024] In this way, it is possible to achieve a desired composition of the mixture due to the dosing capability when feeding it into the mixing system via the inlet channels.

[0025] In addition to homogeneous enrichment with the dopant, variable enrichment with the dopant is also possible in the continuous process, whereby in addition to homogeneous admixture of the dopant, a temporarily variable admixture of the dopant can also take place.

[0026] A change in the dopant mixture can generally be achieved by a targeted, volume-defined supply of the required amount of reactant, so that a defined adjustment of the material properties of the precursor material is possible within continuous overall manufacturing processes from the precursor material through fiber preforms to optical fibers with a wide variety of optical properties.

[0027] Due to the metering capability of the fluidic supply of components into a fluidic micromixer, reproducible precursor material is created for further processing.

[0028] In general, the precursor material production device according to the invention is suitable for all dopants (dissolved species, solids, and nanoparticles) and solids (undissolved nanoparticles) that can be introduced into fluids. However, the targeted manipulation of the physical or chemical properties of the precursor material via the reactant additives proves particularly advantageous in the continuous production of fiber preform material.

[0029] It is particularly advantageous to use the precursor material production device according to the invention in the production of homogeneously doped or selectively heterogeneously doped optical fiber preform material, wherein the device enables a continuous production process compared to previously known production methods with chemical precipitation by dropping into an ammoniacal reservoir, as disclosed, for example, in EP 2 215 025 Bl.

[0030] According to one embodiment of the invention, the first and / or the further components can be fed into the mixing system in a controlled manner via a dosing unit. The dosing units can be controlled by a control unit during the feeding process into the mixing system.

[0031] As previously explained, the metering capability during the addition of the first and subsequent components is a crucial aspect for the reproducible production of the mixture as a precursor material for further processing. According to this embodiment, one or more metering units can be used for adding the components, the dispensing of which can be controlled in a suitable manner. One possible implementation of the metering capability is the control of the flow rates of the respective fluids. Coupling the metering unit(s) with the control unit enables a correspondingly controlled dispensing of the components.

[0032] According to one embodiment of the invention, the dosing unit is provided with a measuring unit for monitoring the quantity supplied.

[0033] The measuring unit can be coupled with the control unit. For this purpose, the controlled feeding concept described above is extended to include monitoring of the actual quantity fed by a measuring unit.

[0034] Thus, it is possible, for example, to detect any deviations in the density or flow behavior of the respective fluid, such as those caused by inhomogeneities, agglomerates or uneven distribution in the reservoir, during the ongoing process and to dynamically compensate for them by adjusting the dosing power via the control unit.

[0035] According to one embodiment of the invention, a T-mixer, for example, is used as a fluidic micromixer for mixing two fluids, which is located between the respective fluid channels.

[0036] Such devices enable an improvement in mixing quality and can be used in the device according to the invention as needed.

[0037] According to one embodiment of the invention, the entire fluidic system, or parts thereof, can be temperature controlled.

[0038] Depending on the objective, temperature control of the entire or parts of the fluidic system counteracts the unwanted formation of agglomerates in the fluidic mixture and ensures a uniform density of the mixture after it leaves the mixing system, or promotes (partial) agglomeration and enables targeted heterogeneity of the mixture exiting the mixing system.

[0039] According to one embodiment of the invention, the mixture can be fed to a flow meter after leaving the mixing system. In addition to the input-side verification of the actual addition of components using the measuring unit described above, it is also possible to optically measure the mixture at the output side as it leaves the mixing system, for example, using a flow meter, in order to achieve a comparison with the process time. Thus, the flow meter can detect any variations in the metered quantities introduced during the time-delayed passage through the mixing system and transmit this information to the control unit.

[0040] Furthermore, according to the invention, a method for mixing components of a precursor material for homogeneously or selectively heterogeneously doped optical fiber preforms is specified using a precursor material manufacturing device described above, in which the following steps are carried out:

[0041] • Providing a mixing system in the form of a fluidic micromixer,

[0042] • metered addition of a first component as a dopant or reactant in a fluid (solution or solid) and a second component as a solid in a fluid in the form of nanoparticles (suspension),

[0043] • Mixing the first component and the second component in the mixing system so that the first component and the second component mix homogeneously in the mixing system to form a mixture variably enriched with the reactant,

[0044] • and further processing of the mixture as precursor material for homogeneously or specifically heterogeneously doped (e.g. with a gradient) optical fibers.

[0045] According to a further embodiment of the method according to the invention, the metered feeding is carried out by means of metering units, wherein the metering units are dynamically controlled with respect to a flow rate of the first component or the second component during filling. According to a further embodiment of the method according to the invention, the metering units are provided at the outlet with measuring units that monitor the quantity actually fed by the metering units.

[0046] According to a further embodiment of the method according to the invention, the mixture is fed to a mixing system, advantageously a fluidic micromixer and particularly advantageously a fluidic micromixer in the form of a flow measuring cell, after leaving the metering units.

[0047] According to a further embodiment of the method according to the invention, a control unit controls the dosing units based on the values ​​of the flow measuring cells.

[0048] According to a further embodiment of the method according to the invention, a control unit controls the dosing units based on the values ​​of the flow measurement cells and the measuring units.

[0049] This technical solution aims to produce the synthesis of highly pure, doped nanoparticles and doped particle agglomerates of variable composition and size (distribution) in a continuous, efficient process that is highly reproducible, automatable and precise with regard to the synthesis conditions and resulting material properties in large quantities of material (>150 g approach).

[0050] In particular, this provides a process that, regardless of batch sizes, composition, or doping, yields material of consistent quality for optical fiber preforms. This material can be used, for example, in the production of optical fiber preforms with high homogeneity or precisely adjustable chemical-structural heterogeneity. Large quantities of high-purity doped SiO2 are required, for instance, for fibers with large mode areas or multi-chain fibers. The developed technical solution enables controlled, continuous mixing of the reactant and potential precipitation of the dopants in the suspension under predefined conditions at any point during the mixing / precipitation step. It also avoids the monotonous changes in environmental, reaction, and mixing conditions that would otherwise occur with conventional (batch-based) precipitation.

[0051] By using an adequately dimensioned flow mixing cell, various fluids (particle-, ion-, reactant- and additive-carrying liquids) can be combined in a continuous flow in the smallest volume and mixed homogeneously, continuously and reproducibly in the shortest possible time (mixing times <10 ms) and thus optimally brought to the (precipitation) reaction.

[0052] By selectively combining nanoparticles or their particle agglomerates of variable composition and size (distribution) with any dopant solutions for co-precipitation in suspension, a continuous, efficient process is possible which is highly reproducible, automatable and precise with regard to the synthesis conditions and resulting material properties, enabling the production of large quantities of material (>150 g / batch with mass loadings of >lg / L, typically >100 g / L doped SiO2).

[0053] This technical solution thus enables consistent reaction conditions and results in the production of precursor materials for high-purity, large-volume and homogeneously doped optical fiber reforming, regardless of the quantities of starting materials used and the planned quantities of product, while aiming for chemical structural homogeneity.

[0054] This also allows for variation / targeted modification of the synthesis parameters during the continuous process, which is useful for selectively increasing heterogeneity. Due to its continuous nature, flexibility regarding material composition, and the ease of temporary in-line adjustments, the method enables flexible scaling of the synthesis of large quantities (>150 g / batch) in an automated process, with precisely adjustable reaction and mixing conditions and high reproducibility.

[0055] Thus, the provided technical solution allows both the production of very small quantities of material (<1 g) and upscaling to large quantities (>1 kg), with identical material properties.

[0056] Continuous production enables resource-efficient integration into an automated production line.

[0057] The invention is explained in more detail below with reference to the figure and the exemplary embodiments, without being limited to these, and wherein identical or identically acting elements are provided with the same reference numerals.

[0058] This shows

[0059] Fig. 1 : a schematic representation of a precursor material manufacturing device according to the invention for mixing components of a precursor material for a fiber preform.

[0060] Fig. 1 shows a schematic representation of an embodiment of the precursor material manufacturing device, in which only the components relevant to the invention are shown.

[0061] However, it goes without saying that the invention can be extended to include the further addition of additional additives as admixtures.

[0062] Fig. 1 shows that the precursor material production device (1) has a reservoir (21, 22) for the reactant (211) and for the suspension (221), which is provided with a corresponding fluidic microchannel (2) for adding the reactant as the first component and the suspension as the second component.

[0063] Fluidic reactant (211) is added via the first inlet channel (2).

[0064] The second inlet channel (2) serves to supply the suspension (221).

[0065] The reactant (211) is used to selectively influence the physical or chemical properties of the mixture and the resulting precursor material.

[0066] Each of the two reservoirs (21, 22) is connected to a metering unit (51, 52), which in the illustrated embodiment can be designed as a fluidic metering unit.

[0067] The dosing units (51, 52) each enable the controlled addition of a predetermined amount of the respective substance in the form of reactant (211) and suspension (221).

[0068] For example, the amount dispensed can be determined based on the intrinsic parameters of the fluidic dosing units (51, 52) using the activation time of the fluidic dosing units (51, 52).

[0069] Optionally, as shown in Fig. 1, one or both dosing units (51, 52) can be equipped with a measuring unit (41, 42). The measuring units (41, 42) allow for verification of the actual quantity dispensed by the dosing units (51, 52).

[0070] Both the dosing units (51, 52) and the measuring units (41, 42), if present, are connected to a control unit (5) which controls the dispensing of the substances via the dosing units (51, 52) and, if applicable, incorporates the values ​​of the measuring units (41, 42) into the control.

[0071] The reactant (211) and suspension (221) dispensed by the dosing units (51, 52) now enter the mixer (3), which is designed as a fluidic micromixer (3), and can particularly advantageously be a flow-through mixing cell. The composition of the mixture (6) can be continuously controlled over a wide range by means of the controlled addition of reactant (211) and suspension (221), so that a reproducible precursor material is created for further processing into doped optical fiber preforms and fibers. The precursor material production device and the process using it can be integrated into existing, continuous industrial production lines at the appropriate point of precursor material feed.

[0072] First, a first component, the reactant (211), and a second component, the suspension (221), are added in a metered manner. By mixing the first component and the second component in the fluidic micromixer (3), the first component and the second component mix in the fluidic micromixer (3) in a defined manner to form an enriched mixture (6) with homogeneous or specifically heterogeneously enriched dopants.

[0073] The mixture (6) is then further processed as a precursor material. Metered feeding can be carried out using metering units (51, 52), whereby the metering units (51, 52) are continuously, homogeneously, or dynamically controlled with respect to the flow rate of the first component or the second component during the filling of the fluid channels (2).

[0074] Furthermore, the dosing units (51, 52) can be equipped at the output with the measuring units (41, 42) which monitor the quantity actually supplied by the dosing units (51, 52).

[0075] The mixture (6) can be fed to the flow measuring cell (31) before entering the fluidic micromixer (3) and to the flow measuring cell (32) after leaving the fluidic micromixer (3).

[0076] Here, the control unit (5) is designed to control the dosing units (51, 52) based on the values ​​from the flow measurement cells (31, 32) and the measuring units (41, 42). 1. Exemplary embodiment (a to f)

[0077] An aqueous SiO2 suspension mixed with dissolved Al 3+ and RE 3+ and a density = 1.1 g / ml, and with a solids content of 14.6%, is mixed with a series of further solutions 2: NH3 in water, density = 0.99 g / ml at 12 mL / min each in a T-mixer, wherein variants (a to f) exist.

[0078] 2. Example of implementation

[0079] An aqueous SiO2 suspension mixed with dissolved Al 3+ A solution with a density of 1.1 g / ml, an initial pH of ~0.5 and a solids content of -14% is mixed with another solution 2: NH3 in water pH of -11, density = 0.99 g / ml at 13 and 11 mL / min in a T-mixer.

[0080] 3. Example of implementation

[0081] An aqueous SiO2 suspension mixed with dissolved Al 3+ and RE 3+ and a density of 1.1 g / ml, an initial pH of -0.5 and a solids content of -14% is mixed with another solution 2: NH3 in water pH of -10.5, density = 0.99 g / ml at 13 and 11 mL / min in a T-mixer.

[0082] 4. Example of implementation

[0083] An aqueous SiO2 suspension mixed with dissolved Al 3+ , RE 3+and boric acid with a density of 1.1 g / ml, an initial pH of -1.3, and a solids content of -14%, is mixed with another solution 2: NH3 in water, pH of -11.5, density = 0.99 g / ml, at flow rates of 14 and 10 mL / min in a T-mixer. 5. Example of implementation

[0084] An aqueous SiO2 suspension mixed with dissolved Al 3+ and RE 3+ and a density of 1.1 g / ml, an initial pH of -1.3 and a solids content of -14% is mixed with another solution 2: NH3 in water pH of -11, density = 0.99 g / ml at 14 and 10 mL / min in a T-mixer.

[0085] 6. Example of implementation

[0086] An aqueous SiO2 suspension with a density of 1.1 g / ml, an initial pH of -11 and water-soluble organic additives with a solids content of -14% is treated with a solution of Al 3+ and RE 3+ mixed in water with a pH of -1 and a density of 1 g / ml at a rate of 12 mL / min in a T-mixer.

[0087] 7. Example of implementation

[0088] An aqueous SiO2 suspension mixed with dissolved Al 3+ , RE 3+ and phosphoric acid with a density of 1.1 g / ml, an initial pH of ~1.5 and a solids content of -14% is mixed with another solution 2: NH3 in water pH of -11.5, density = 0.99 g / ml at 13.5 and 11.5 mL / min in a T-mixer.

[0089] All features shown in the description, the drawing and the exemplary embodiments as well as in the following claims can be essential to the invention both individually and in any combination with one another.

[0090]

[0091] 1 - Precursor material manufacturing device

[0092] 2 - Fluid channels

[0093] 21 - Reservoir

[0094] 211 - Reactant in the form of one or more dopants and / or additives carried by a fluid)

[0095] 22 - Reservoir

[0096] 221 - Suspension in the form of a fluid-borne solid in nanoparticle form, with or without dopants or additives dissolved in the fluid)

[0097] 3 - Mixer (in the form of a fluidic micromixer, in particular a flow-through mixing cell)

[0098] 3a - Entrance 1

[0099] 3b - Entrance 2

[0100] 31 - Sensor 1 / Flow measuring cell 1

[0101] 32 - Sensor 2 / Flow measuring cell 2

[0102] 41 - Unit of measurement 1

[0103] 42 - Measuring unit 2

[0104] 5 - Control unit

[0105] 51 - Dosing unit 1

[0106] 52 - Dosing unit 2

[0107] 6 - Mixture material / Precursor material

Claims

Patent claims 1. Precursor material production device (1) for high-purity, large-volume, and homogeneously or heterogeneously doped optical fiber preforms, in which a reactant (211) as the first component and a suspension (221) as the second component of the precursor material (6) are mixed, wherein the first component can be metered into a mixing system (3) via a first inlet opening (3a) and the second component can be metered into a mixing system (3) via at least one further inlet opening (3b), such that the first component and the second component mix in the mixing system (3) to form a mixture homogeneously or in a controlled heterogeneous manner enriched with the reactant (211), which can be supplied as precursor material (6) for further processing, characterized in that the precursor material production device (1) is a microfluidic system comprising at least two reservoirs (21) for the reactant (211) and the suspension (221) as well as at least two fluid channels (2).wherein each fluid channel (2) leads from a reservoir (21) via the inlet openings (3a, 3b) into the mixing system (3), where reactant (211) and suspension (221) are obtained as precursor material (6) in the fluid in the form of a mixture, wherein the mixing system (3) is a fluidic micromixer.

2. Precursor material manufacturing device according to claim 1, characterized in that the fluidic micromixer is a flow-through mixing cell.

3. Precursor material production device according to claim 1 or 2, characterized in that the reactant (211) is one or more dopants and / or additives carried by a fluid and that the suspension (221) is a fluid-carried solid in nanoparticle form, with or without dopants or additives dissolved in the fluid.

4. Precursor material production apparatus according to claim 3, characterized in that the reactant (211) is present as a component in the form of fluorides and fluorine-containing compounds in a fluid or one or more nitrides or oxides or, in further processing, oxide-forming additives of the group consisting of the elements Li, Be, B, Na, Mg, Al, Si, P, K, Ca, Sc, Ti, V, Cr, Mn, Co, Ni, Zn, Ga, Ge, As, Se, Rb, Sr, Y, Zr, Nb, Mo, Tc, Ru, Rh, Cd, In, Sn, Sb, Te, Cs, Ba, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, Re, Os, Ir, TI, Pb, Bi, Ac, Cu, Pt, Au, Ag, Pt 5. Precursor material production apparatus according to claim 4, characterized in that the suspension (221) is in the form of SiO2 nanoparticles in a fluid as a slurry, which is treated with fluorides and fluorine-containing compounds or one or more nitrides or oxides or, in further processing, oxide-forming additives of the following group of elements: Li, Be, B, Na, Mg, Al, Si, P, K, Ca, Sc, Ti, V, Cr, Mn, Co, Ni, Zn, Ga, Ge, As, Se, Rb, Sr, Y, Zr, Nb, Mo, Tc, Ru, Rh, Cd, In, Sn, Sb, Te, Cs, Ba, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, Re, Os, Ir, TI, Pb, Bi, Ac, Cu, Pt, Au, Ag, Pt is included as a component.

6. Precursor material manufacturing device according to one of claims 1 to 5, characterized in that the first and / or the further components can be supplied to the mixing system (3) in a controlled manner via a metering unit (51, 52).

7. Precursor material manufacturing device according to claim 6, characterized in that the dosing units (51, 52) are controllable via a control unit (5) during feeding to the mixing system (3).

8. Precursor material manufacturing device according to one of the Claims 1 to 7, characterized in that the Dosing unit (51, 52) with a measuring unit (41, 42) for is equipped with monitoring of the supplied quantity of reactant (211) and suspension (221).

9. Precursor material manufacturing device according to claim 8, characterized in that the measuring unit (41, 42) is equipped with the The control unit (5) is coupled.

10. Precursor material manufacturing device according to one of claims 1 to 9, characterized in that the mixing system (3) is temperature-controlled.

11. Precursor material manufacturing device according to one of claims 1 to 10, characterized in that the mixture in the form of the precursor material (6) can be supplied to a processing line for homogeneously or specifically heterogeneously doped optical fiber preforms after leaving the mixing system (3).

14. Method for mixing components of a precursor material using a precursor material manufacturing device according to any one of claims 1 to 13, wherein the following steps are performed: - Providing a precursor material manufacturing device (1), - Metered addition of a first component as a reactant contained in a liquid (211) and a second component as a suspension (221), - Mixing the first component and the second component in the mixing system (3), which is designed as a fluidic micromixer, such that the first component and the second component mix homogeneously or in a targeted heterogeneous manner in the mixing system (3) to form a mixture (6) homogeneously or variably enriched with the reactant (211), and - Further processing of the mixture (6) into doped optical fiber preforms.

15. Method according to claim 14, characterized in that the metered supply is carried out by means of metering units (51, 52), wherein the dosing units (51, 52) are controlled continuously or dynamically with respect to a flow rate of the first component or the second component during the flow through the fluidic micromixer (3).

16. Method according to claim 14 or 15, characterized in that the metering units (51, 52) are provided at the outlet with measuring units (41, 42) which monitor the quantity actually supplied by the metering units (51, 52) and / or the flow within the fluid channels (2) before and after the fluidic micromixer (3) is measured and monitored with sensors in the form of flow measuring cells (31, 32).

17. Method according to claim 16, characterized in that the control unit (5) controls the dosing units (51, 52) on the basis of the values ​​of the flow measuring cells (31, 32) and / or the measuring units (41, 42).

18. Method according to one of claims 14 to 17, characterized in that the control unit (5) controls the dosing units (51, 52) on the basis of the measured values ​​of the flow measuring cells (31, 32) and / or the measuring units (41, 42).

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