Obtaining conductive reduced graphene oxide nanoparticles with probiotic bacteria-containing material

The interaction of probiotic bacteria with graphene oxide allows for the production of conductive reduced graphene oxide nanoparticles, addressing the scalability and cost issues in graphene production, enabling advanced applications in biosensors and diagnostic devices.

WO2025170551A1PCT designated stage Publication Date: 2025-08-14BİOPROBİF SAĞLIK GIDA ARGE SANAYİ & TİCARET LİMİTED ŞİRKETİ
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Patent Information

Application Number
PCT/TR2024/050168
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Filing Date
2024-02-28
Publication Date
2025-08-14

AI Technical Summary

Technical Problem

The lack of a reliable, clean, and cost-effective method for producing graphene on a large scale hinders its widespread use in various applications, particularly in high-tech products and industrial applications.

Method used

The interaction of probiotic bacteria-containing material, specifically Bifidobacterium infantis, with graphene oxide in both sonographic and non-sonographic environments, facilitates the production of conductive reduced graphene oxide nanoparticles through a sustainable and scalable process.

Benefits of technology

This method enables the production of more sustainable, clean, and scalable nanomaterials, expanding their use in applications such as full-cell biosensors and field-deployable diagnostic devices, while offering an environmentally friendly approach.

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Abstract

The invention is the obtaining of conductive reduced graphene oxide nanoparticles with probiotic bacteria-containing material which involes the synthesis of conductive reduced graphene oxide nanoparticles with material containing probiotic bacteria, and which can synthesize graphene oxide in certain acidic conditions and reduce it at room conditions using ultrasonic, magnetic stirrer mixed with probif.
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Description

[0001] OBTAINING CONDUCTIVE REDUCED GRAPHENE OXIDE NANOPARTICLES WITH PROBIOTIC BACTERIA-CONTAINING MATERIAL

[0002] Technical Field

[0003] The invention relates to obtaining conductive reduced graphene oxide nanoparticles with probiotic bacteria-containing material in which probif interacts with graphene oxide in both sonographic (imaging using sound waves) and non-sonographic aerobic environments, resulting in more efficient, more effective and less toxic graphene oxide.

[0004] Background of the Invention

[0005] The "tips" of today's pencils are not made of lead, but of chemical called graphite. Graphite is a material formed when carbon atoms come together in a hexagonal arrangement. Graphite has the most stable arrangement of carbon known. Normally graphite exists in the form of 3-dimensional layers. When only one of these layers is considered, we come across graphene.

[0006] Graphene is a single layer of graphite. It has a hexagonal carbon arrangement, but its three-dimensional structure has a height of only 1 atom.

[0007] It is quite possible to find graphite in nature, but it is not possible to find graphene in a single layer. Scientists have been envisioning a single-layer hexagonal arrangement of carbon for many years. Even during the production of pencils, graphene was unknowingly produced. In 1962, it was examined under an electron microscope for the first time, which was not possible until then. Until this time, graphene had always been observed as part of other metals. But everything changed in 2004 when Andre Geim and Konstantin Novoselov from the University of Manchester "rediscovered" graphene. Geim and Novoselov not only isolated graphene, but also managed to identify all its characteristic properties. The term graphene is perceived as if it refers to a single material, but even though it sounds like a singular material, graphene is actually a large group of materials. Graphene is one of the thinnest materials. This is because, although it contains many atoms in two dimensions, it contains only a layer of carbon in the third dimension. In this way, it can have the highest surface to weight ratio known. In other words, it has a high surface area per unit weight. Graphene is also one of the strongest, hardest and most stretchable materials known.

[0008] More than 200 research centers around the world are trying to produce new products using graphene. Tens of thousands of academic articles on graphene have been published until today.

[0009] There are major technology companies working on graphene. One of these companies conducts a graphene utilization project consisting of about 50 steps. We will soon be able to see graphene used in mobile applications. In particular, graphene is the most important material that makes flexible touch screens possible.

[0010] Another company conducting work with graphene has succeeded in pushing the limits of transistors smaller than 7 nanometers by using graphene. Thanks to the graphene through which electricity is passed, they are able to place the nanomaterials used in transistor construction with 97% accuracy.

[0011] Graphene has been used in many different areas, enabling different sectors to advance rapidly. Since graphene is 3-4 times stronger than carbon fiber, it has started to be used in the automotive and aviation sectors. As a result of some studies, graphene may become the main material of wings in aviation and replace carbon fiber. Carbon fiber is widely used in airplanes because safety and resistance are extremely important; however, the reason why we do not see it widely in automotive is that carbon fiber cannot be produced by cheap injection method. However, although graphene paves the way for production by cheap injection, the methods and techniques are not fully established.

[0012] Easy ways to produce graphene are, however, not yet fully established. Researchers have now realized the advantages of using nanomaterials to create more efficient computers, medical devices and high-tech products. At this point, graphene has emerged as a revolutionary material in nanotechnology due to its electrical conductivity, mechanical strength and flexibility. However, the challenges of producing graphene on a large scale for use in daily applications prevent the full exploitation of this potential.

[0013] Graphene is a material derived from graphite, the material found in an ordinary pencil, and has a structure as thick as a single carbon atom. The thin structure of single-layer graphene provides the highest possible surface-to-volume ratio, increasing its usability in various industrial applications. Moreover, graphene's exceptional properties enable a variety of applications in a range of fields, from bioanalytical applications to drug carriers, composite materials to advanced transistors.

[0014] One obstacle to the widespread use of graphene is the lack of a reliable, clean, cost- effective and scalable production method. At this point, chemical vapor deposition (CVD) and graphite exfoliation methods are widely used for graphene production. However, chemical vapor deposition (CVD) has disadvantages such as the limited surface area of the substrate and the need for special atmosphere.

[0015] The invention highlights the interaction of Probif with graphene oxide as a solution to these challenges in graphene production. This innovative method allows graphene oxide to be produced more sustainably and cost-effectively with the help of bacteria. These capabilities of microorganisms can further expand the use of nanomaterials in applications such as full-cell biosensors and field-deployable diagnostic devices, bringing rapid detection and complex computational capabilities.

[0016] The combination of graphene and Probif represents an important step forward in the production of nanomaterial. This approach will enable the production of more sustainable, clean and scalable nanomaterials in the future. Probif's interaction with graphene oxide could be a breakthrough in the production of high-tech products such as computers, medical devices and plays an important role in industrial applications by offering an environmentally friendly approach. This innovation will contribute to a broader role for nanomaterials in future applications.

[0017] Detailed Description of the Invention

[0018] In this detailed description, it relates to the obtaining of conductive reduced graphene oxide nanoparticles with probiotic bacteria-containing material and is described only for a better understanding of the subject and without any limiting effect.

[0019] The components used during the production of conductive reduced graphene oxide nanoparticles with probiotic bacteria-containing material are as follows:

[0020] • probif (probiotic bifidobacterium infantis, xylooligosaccharide, sodium alginate composite)

[0021] • graphene oxide (100mg)

[0022] Bifidobacterium infantis is a lactic acid (butyric acid, propionic acid) producing bacterium, which indicates the presence of a high negative redox potential. This feature is evidence of the bacteria's fast electron transfer and strong carbon decomposing ability.

[0023] In the invention in question, in the graphene oxide (100 g) material, there are materials containing:

[0024] • %1 - 90 mg graphene oxide nanoparticles

[0025] • %1-10 gr probiotic product with probif brand and ingredients (alginate I xylooligosaccharide I bidobakterium infantis).

[0026] The process steps of making the invention are as follows;

[0027] • graphene oxide synthesis, 300-400 ml sulfuric acid (H2SO4) and 30-50 ml phosphoric acid (H3PO4) are placed in a beaker, the beaker is placed in an oil bed, making sure that the level of the oil is above the level of the liquid mixture, the temperature of the oil is set to 50-60°C, which allows to stabilize the temperature of the reaction between 40-45°C, the beaker is put into the mixer together with the oil bed and mixed at 150-250 rpm, • 2-4 g graphite is slowly added to the acid solution. 13-20 g potassium permanganate (KMnO4) is slowly added to the solution, the reaction is stirred at 35-45 °C for 16 hours, with the solution temperature measured at frequent intervals with a thermometer,

[0028] • after stirring for 16 hours, the suspension is transferred to a beaker containing 300-400g of ice and stirred, (while transferring the suspension, it should be ensured that no graphene oxide remains in the beaker), 2-5 ml of hydrogen peroxide (H2O2) (30 wt%) is added dropwise while the suspension is mixing with the ice,

[0029] • this mixture is centrifuged at 2500-3500 rpm for 40-55 minutes,

[0030] • after centrifugation, the supernatant (acid) is decanted into the waste bin, centrifuge tubes are filled with up to 350-450 ml of pure water to wash the pellets and centrifuged at 4500-5500 rpm for 45 min,

[0031] • then it is centrifuged for 3 times with HCL and 3 times with pure ethanol at 4500-5500 rpm for 45 min each, in this step, non-conductive graphene oxide nanoparticles are obtained and the reduction reaction is initiated by mixing with probif at room conditions and ultrasonic environment I magnetic stirrer,

[0032] • the obtained 90 mg graphene oxide nanoparticles and 5-10 g probif powder are measured and added to pure water,

[0033] • 30-100 ml of pure water is placed in an ultrasonic / frequency bath (Isolab LB. IS.621.05.003) under 50 Hz-5 Gigaherz in an aerobic 23 Celsius (room conditions),

[0034] • it is observed that graphene oxide and Probif branded probiotic material, which are mixed for about 19 hours, turn into black color,

[0035] • the resulting mixture is nanoparticulated in a centrifuge device (CAPP CRP - 432X, serial no: QF042286),

[0036] • when the bacteria remove the oxygen groups, the graphene oxide becomes conductive (rGO) and the bifidobacterium binds hydrogen and oxygen, releasing hydrogen peroxide (H2O2), which makes the environment acidic with a measured Ph :4,6 in pH value (Hanna Model HI-2202 Edge Meter),

[0037] • measurements are taken to determine the crystal structure and molecular structure of the solution obtained by FTIR and Raman Spectroscopy, • Graphene Oxide reduction (rGO) in accordance with the literature is determined by characterization measurements,

[0038] • the same processes are repeated in aerobic media in a magnetic stirrer without ultrasonic media,

[0039] • 90 mg graphene oxide nanoparticles and 5 - 10 g Probif obtained are measured in powder form and added to pure water, this mixture is mixed in a beaker in aerobic, room conditions at 20-25 degrees Celsius in a magnetic stirrer at 475-550 rpm (Elektromag M 221 Magnetic Stirrer)

[0040] • At the end of the 7th day, the pH measurement value is 5.2, the resulting mixture is centrifuged to produce nanoparticles (rGO).

[0041] The technical features mentioned in each claim are followed by a reference number and these reference numbers are used only to facilitate understanding of the claims and should not be considered as limiting the scope of any of the elements indicated by these reference numbers for illustrative purposes.

[0042] It is clear that a person skilled in the art can also demonstrate the novelty set forth in the invention by using similar embodiments and / or apply this embodiment to other areas with similar purposes used in the relevant art. Therefore, it is also obvious that such embodiments will lack the criterion of novelty and especially the criterion of exceeding the state of the art.

Claims

CLAIMS1. The obtaining of conductive reduced graphene oxide nanoparticles with probiotic bacteria-containing material, wherein the components used during obtaining the invention comprise probif (probiotic bifidobacterium infantis, xylooligosaccharide, sodium alginate composite), graphene oxide (100mg)2. The obtaining of conductive reduced graphene oxide nanoparticles with probiotic bacteria-containing material according to claim 1 , wherein in the graphene oxide (100 g) material, there are materials containing %1 - 90 mg graphene oxide nanoparticles %1-10 g probiotic product with probif brand and ingredients (alginate I xylooligosaccharide I bidobakterium infantis).

3. The obtaining of conductive reduced graphene oxide nanoparticles with probiotic bacteria-containing material wherein it is characterized that it comprises the following steps• graphene oxide synthesis, 300-400 ml sulfuric acid (H2SO4) and 30-50 ml phosphoric acid (H3PO4) are placed in a beaker, the beaker is placed in an oil bed, making sure that the level of the oil is above the level of the liquid mixture, the temperature of the oil is set to 50-60°C, which allows to stabilize the temperature of the reaction between 40-45°C, the beaker is put into the mixer together with the oil bed and mixed at 150-250 rpm,• 2-4 g graphite is slowly added to the acid solution. 13-20 g potassium permanganate (KMnO4) is slowly added to the solution, the reaction is stirred at 35-45 °C for 16 hours, with the solution temperature measured at frequent intervals with a thermometer,• after stirring for 16 hours, the suspension is transferred to a beaker containing 300-400g of ice and stirred, (while transferring the suspension, it should be ensured that no graphene oxide remains in the beaker), 2-5 ml of hydrogen peroxide (H2O2) (30 wt%) is added dropwise while the suspension is mixing with the ice,• this mixture is centrifuged at 2500-3500 rpm for 40-55 minutes,• after centrifugation, the supernatant (acid) is decanted into the waste bin, centrifuge tubes are filled with up to 350-450 ml of pure water to wash the pellets and centrifuged at 4500-5500 rpm for 45 min,• then it is centrifuged for 3 times with HCL and 3 times with pure ethanol at 4500-5500 rpm for 45 min each, in this step, non-conductive graphene oxide nanoparticles are obtained and the reduction reaction is initiated by mixing with probif at room conditions and ultrasonic environment I magnetic stirrer,• the obtained 90 mg graphene oxide nanoparticles and 5-10 g probif are measured in powder form and added to pure water,• 30-100 ml of pure water is placed in an ultrasonic / frequency bath (Isolab LB. IS.621.05.003) under 50 Hz-5 Gigaherz in an aerobic 23 Celsius (room conditions),• it is observed that graphene oxide and Probif branded probiotic material, which are mixed for about 19 hours, turn into black color,• the resulting mixture is nanoparticulated in a centrifuge device (CAPP CRP - 432X, serial no: QF042286),• when the bacteria remove the oxygen groups, the graphene oxide becomes conductive (rGO) and the bifidobacterium binds hydrogen and oxygen, releasing hydrogen peroxide (H2O2), which makes the environment acidic with a measured Ph :4,6 in pH value (Hanna Model HI-2202 Edge Meter),• measurements are taken to determine the crystal structure and molecular structure of the solution obtained by FTIR and Raman Spectroscopy,• Graphene Oxide reduction (rGO) in accordance with the literature is determined by characterization measurements,• the same processes are repeated in aerobic media in a magnetic stirrer without ultrasonic media,• 90 mg graphene oxide nanoparticles and 5 - 10 g Probif obtained are measured in powder form and added to pure water, this mixture is mixed in a beaker in aerobic, room conditions at 20-25 degrees Celsius in a magnetic stirrer at 475-550 rpm (Elektromag M 221 Magnetic Stirrer)• At the end of the 7th day, the pH measurement value is 5.2, the resulting mixture is characterized by the fact that it contains steps to produce the nanoparticles (rGO) by centrifugation.

Citation Information

Patent Citations

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