Low-viscosity MXene conductive ink suitable for ink-jet printing and preparation method thereof

Abstract

The invention discloses low-viscosity MXene conductive ink suitable for ink-jet printing and a preparation method thereof, and the preparation method comprises the following steps: 1) adding LiF powder into concentrated hydrochloric acid HCl, stirring to completely dissolve LiF, then adding a Ti3AlC2MAX phase to carry out an etching reaction, washing and centrifuging the etched solid precipitate, and collecting the dispersion liquid on the upper layer, thereby obtaining the low-viscosity MXene conductive ink suitable for ink-jet printing; the dispersion liquid is rich in high-quality MXene single-layer / few-layer nanosheets; and 2) centrifuging the dispersion liquid to obtain a water-based MXene precipitate, dispersing the water-based MXene precipitate in an organic composite solvent, then carrying out oscillation, centrifugation and re-dispersion, and then adjusting the concentration through the organic composite solvent to obtain the low-viscosity MXene conductive ink suitable for ink-jet printing, and the ink prepared by the method does not easily block a nozzle.

Description

Technical Field

[0001] The present invention belongs to the field of MXene conductive ink preparation, and relates to a low-viscosity MXene conductive ink suitable for inkjet printing and a preparation method thereof. Background Art

[0002] Printed electronics technology can print integrated circuits, sensors, capacitors, displays, radio frequency identification tags and other flexible wearable electronic devices on flexible materials, which constitute a huge part of current smart wearable products and are of great significance to the innovative development of industry, society and science.

[0003] Due to the rich functional groups on the surface of MXene, additive-free stable inks can be made only under the interaction force between nanosheets, which have excellent electrical, optical and mechanical properties, bringing great hope for the commercialization of large-scale manufacturing of functional films or electronic components using solution processing (screen printing, inkjet printing, slit coating, etc.).

[0004] Since the inkjet printing process has strict requirements on ink viscosity, surface tension, volatility and filler size distribution, the application of water-based MXene nanosheets in inkjet printing is greatly limited. For example, water-based MXene ink has a high surface tension and is not suitable for high-precision inkjet printing of micropatterns. In addition, water-based MXene ink is easily disturbed by dust impurities, ions, residual solvents and other factors in the inkjet printer inlet pipeline, resulting in local deposition of MXene nanosheets in the printer nozzle and clogging the nozzle. This phenomenon is very likely to occur in the process of cleaning the nozzle after the device / pattern is printed. Single organic solvent-based MXene ink (such as N-methylpyrrolidone, NMP, as a dispersing solvent) will also encounter the phenomenon of destroying the dispersion stability of the residual ink in the nozzle during the cleaning process, resulting in MXene sedimentation and clogging the nozzle. Therefore, in order to solve the above problems, it is urgent to prepare a low-viscosity MXene conductive ink suitable for high-precision inkjet printing, which is not easy to clog the equipment nozzle during the entire printing process to achieve a sustainable environmental protection concept. Summary of the invention

[0005] The purpose of the present invention is to overcome the shortcomings of the above-mentioned prior art and provide a low-viscosity MXene conductive ink suitable for inkjet printing and a preparation method thereof. The ink prepared by the method is not easy to clog the nozzle.

[0006] To achieve the above object, the present invention discloses a method for preparing a low-viscosity MXene conductive ink suitable for inkjet printing, comprising the following steps:

[0007] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0008] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0009] Furthermore, the process of washing and centrifuging the etched solid precipitate is as follows:

[0010] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0011] Further, in step 1), Ti 3 AlC 2 The particle size of the MAX phase is 400-150 mesh, and the concentration of concentrated hydrochloric acid HCl is 6M-12M.

[0012] Further, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 1 to 3:1.

[0013] Furthermore, in step 1), the etching reaction time is 24 to 48 hours, and the reaction temperature is 20 to 50°C.

[0014] Furthermore, the shaking and ultrasonic treatment time is 0.5 to 2 hours, the rotation speed of the centrifugal treatment is 2000 to 5000 rpm / min, the centrifugal time is 15 to 60 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 0.1 to 5M.

[0015] Furthermore, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 0.2 to 5 μm.

[0016] Furthermore, during the redispersion in step 2), the vortex oscillation time is 20 to 60 minutes, the centrifugal treatment speed is 8000 to 10000 rpm / min, and the centrifugal time is 60 to 180 minutes.

[0017] Furthermore, the organic composite solvent is a mixture of one or more of N-methylpyrrolidone (NMP), dimethyl sulfoxide (DMSO), N,N-dimethylformamide (DMF), polyethylene glycol (PEG), ethanol and deionized water.

[0018] The present invention discloses a low-viscosity MXene conductive ink suitable for inkjet printing, which is prepared based on the preparation method of the low-viscosity MXene conductive ink suitable for inkjet printing.

[0019] The present invention has the following beneficial effects:

[0020] The low-viscosity MXene conductive ink suitable for inkjet printing and the preparation method thereof according to the present invention are specifically operated, wherein the solvent of the conductive ink is an organic composite solvent, and the conductive material is a two-dimensional Ti 3 C 2 T x MXene, in addition, during the implementation of inkjet printing, the nanosheets are not easy to deposit and wrinkle, have good physical stability, the ink can maintain uniform steady-state colloidal properties, and is not easy to clog the nozzle. At the same time, it achieves the dual goals of printing high-precision and high-conductive electrodes and easy to clean and sustainable development. It is an inkjet printing ink with great commercial prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The accompanying drawings constituting a part of the present invention are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the accompanying drawings:

[0022] Figure 1 Ti prepared in Example 1 3 C 2 T x XRD of thin films;

[0023] Figure 2 Ti prepared in Example 1 3 C 2 T x TEM image of nanosheets;

[0024] Figure 3 This is a real picture of the low-viscosity organic composite MXene ink prepared in Example 1;

[0025] Figure 4 The antenna pattern prepared by inkjet printing in Example 1;

[0026] Figure 5 The lines and micro patterns prepared by inkjet printing in Example 1. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] In the description of the present invention, it should be understood that the terms “include” and “comprises” indicate the presence of described features, wholes, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, wholes, steps, operations, elements, components and / or collections thereof.

[0029] It should also be understood that the terms used in the present specification are only for the purpose of describing specific embodiments and are not intended to limit the present invention. As used in the present specification and the appended claims, unless the context clearly indicates otherwise, the singular forms "a", "an" and "the" are intended to include plural forms.

[0030] It should be further understood that the term "and / or" used in the present specification and the appended claims refers to any combination of one or more of the associated listed items and all possible combinations, and includes these combinations. For example, A and / or B can represent: A exists alone, A and B exist at the same time, and B exists alone. In addition, the character " / " in the present invention generally indicates that the associated objects are in an "or" relationship.

[0031] It should be understood that, although the terms first, second, third, etc. may be used to describe preset ranges, etc. in the embodiments of the present invention, these preset ranges should not be limited to these terms. These terms are only used to distinguish preset ranges from each other. For example, without departing from the scope of the embodiments of the present invention, the first preset range may also be referred to as the second preset range, and similarly, the second preset range may also be referred to as the first preset range.

[0032] The word "if" as used herein may be interpreted as "at the time of" or "when" or "in response to determining" or "in response to detecting", depending on the context. Similarly, the phrases "if it is determined" or "if (stated condition or event) is detected" may be interpreted as "when it is determined" or "in response to determining" or "when detecting (stated condition or event)" or "in response to detecting (stated condition or event)", depending on the context.

[0033] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. The components of the embodiments of the present invention described and shown in the drawings here can usually be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present invention provided in the drawings is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0034] Various structural schematic diagrams of the embodiments disclosed in the present invention are shown in the accompanying drawings. These figures are not drawn to scale, and some details are magnified and some details may be omitted for the purpose of clear expression. The shapes of various regions and layers shown in the figures and the relative sizes and positional relationships therebetween are only exemplary, and may deviate in practice due to manufacturing tolerances or technical limitations, and those skilled in the art may additionally design regions / layers with different shapes, sizes, and relative positions according to actual needs.

[0035] The method for preparing low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0036] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, and the etched solid precipitate is washed with dilute HCl, LiCl and deionized water in sequence until it is neutral, and then subjected to oscillation, ultrasonic stripping and centrifugation, and then the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0037] 2) The dispersion is centrifuged at high speed to obtain a high-concentration aqueous MXene precipitate, the aqueous MXene precipitate is dispersed in an organic composite solvent, and then shaken, centrifuged, and dispersed again to obtain an organic composite steady-state MXene conductive ink.

[0038] 3) The concentration of the organic composite steady-state MXene conductive ink is adjusted to a preset concentration, and then printed on the substrate according to the pattern using an inkjet printer.

[0039] In step 1), Ti 3 AlC 2 The particle size of the MAX phase is 400-150 mesh, the concentration of concentrated hydrochloric acid HCl is 6M-12M, LiF and Ti3 AlC 2 The mass ratio of the MAX phase is 1 to 3:1, the etching reaction time is 24 to 48 hours, the reaction temperature is 20 to 50°C, the oscillation and ultrasonic time is 0.5 to 2 hours, the centrifugal speed is 2000 to 5000 rpm / min, the centrifugal time is 15 to 60 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 0.1 to 5M.

[0040] In step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 0.2 to 5 μm.

[0041] The organic composite solvent is a mixture of one or more of N-methylpyrrolidone (NMP), dimethyl sulfoxide (DMSO), N,N-dimethylformamide (DMF), polyethylene glycol (PEG), ethanol and deionized water, wherein the content of the deionized water does not exceed 10wt%.

[0042] During the redispersion in step 2), the vortex shaking time is 20 to 60 minutes, the centrifugal treatment speed is 8000 to 10000 rpm / min, and the centrifugal time is 60 to 180 minutes.

[0043] The concentration of the organic composite steady-state MXene conductive ink is adjusted by adjusting the amount of the organic composite solvent added.

[0044] In step 3), the substrate includes one or more of A4 paper, photo paper, PET substrate, PI substrate, metal substrate, glass substrate and fiber fabric substrate.

[0045] Embodiment 1

[0046] This embodiment includes the following steps:

[0047] Add 0.8g of LiF powder to 12M concentrated hydrochloric acid and stir until the LiF is completely dissolved to obtain an etching solution; take 0.5g of 200 mesh Ti 3 AlC 2 The MAX phase is added to the etching solution for etching reaction. The etched solid precipitate is washed multiple times with dilute 1M HCl, 1M LiCl, and deionized water in sequence until it is close to neutral (pH≈6). The precipitate is then shaken on a vortex shaker for 60 minutes and ultrasonicated in an argon environment for 90 minutes to achieve the exfoliation of the nanosheets and reduce the lateral size of the nanosheets. The nanosheets are then centrifuged at 3000 rpm / min for 30 minutes to collect the upper dispersion, which is rich in high-quality MXene single-layer / few-layer nanosheets.

[0048] The dispersion was further centrifuged at a speed of 10,000 rpm / min for 90 minutes to obtain a high-concentration aqueous MXene precipitate. The precipitate was dispersed in an NMP+PEG organic composite solvent and vortexed for 30 minutes and centrifuged at 10,000 rpm / min for 120 minutes. The dispersion and centrifugation steps were repeated 2 to 3 times to obtain an organic steady-state MXene conductive ink.

[0049] A certain amount of MXene ink was vacuum filtered, vacuum dried, and weighed to calculate its concentration. The concentration of the organic steady-state MXene conductive ink was adjusted to 10 mg / ml using NMP+PEG composite solvent, and printed on photo paper according to a preset pattern using an inkjet printer.

[0050] After printing is completed, the nozzle is cleaned multiple times using NMP+PEG organic composite solvent.

[0051] Embodiment 2

[0052] This embodiment includes the following steps:

[0053] The process steps for preparing high-quality MXene monolayer / few-layer nanosheets are the same as those in Example 1. The dispersion rich in monolayer / few-layer MXene nanosheets is further centrifuged at 10,000 rpm / min for 90 min to obtain a high-concentration aqueous MXene precipitate. The precipitate is further dispersed in a DMSO+ethanol organic composite solvent, vortexed for 30 min, and centrifuged at 10,000 rpm / min for 70 min. The dispersion and centrifugation steps are repeated 2 to 3 times to obtain an organic steady-state MXene conductive ink.

[0054] A certain amount of MXene ink was vacuum filtered, vacuum dried, and weighed to calculate its concentration. The prepared organic steady-state MXene conductive ink was adjusted to a concentration of 13 mg / ml using a DMSO+ethanol composite solvent and printed on photo paper according to a preset pattern using an inkjet printer.

[0055] After printing is completed, the nozzle is cleaned multiple times using DMSO+ethanol organic composite solvent.

[0056] Embodiment 3

[0057] This embodiment includes the following steps:

[0058] The process steps for preparing high-quality MXene monolayer / few-layer nanosheets are the same as those in Example 1. The dispersion rich in monolayer / few-layer MXene nanosheets is further centrifuged at 10,000 rpm / min for 90 min to obtain a high-concentration aqueous MXene precipitate. The precipitate is further dispersed in an organic composite solvent of DMSO+NMP, vortexed for 30 min, and centrifuged at 10,000 rpm / min for 80 min. The dispersion and centrifugation steps are repeated 2 to 3 times to obtain an organic steady-state MXene conductive ink.

[0059] A certain amount of MXene ink was vacuum filtered, vacuum dried, and weighed to calculate its concentration. The prepared organic steady-state MXene conductive ink was adjusted to a concentration of 8 mg / ml using a DMSO+NMP composite solvent and printed on photo paper according to a preset pattern using an inkjet printer.

[0060] After printing is completed, the nozzle is cleaned multiple times using DMSO+NMP organic composite solvent.

[0061] Embodiment 4

[0062] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0063] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0064] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0065] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0066] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0067] In this embodiment, in step 1), Ti 3 AlC 2 The particle size of the MAX phase was 150 mesh and the concentration of concentrated hydrochloric acid HCl was 6M.

[0068] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 3:1.

[0069] In this embodiment, in step 1), the etching reaction time is 30 hours and the reaction temperature is 40°C.

[0070] In this embodiment, the shaking and ultrasonic time is 2 hours, the rotation speed of the centrifugal treatment is 2000 rpm / min, the centrifugal time is 60 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 0.1M.

[0071] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 0.2 μm.

[0072] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 20 min, the centrifugal treatment speed is 10000 rpm / min, and the centrifugal time is 180 min.

[0073] In this embodiment, the organic composite solvent is N-methylpyrrolidone (NMP).

[0074] Embodiment 5

[0075] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0076] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0077] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0078] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0079] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0080] In this embodiment, in step 1), Ti 3AlC 2 The particle size of the MAX phase was 200 mesh and the concentration of concentrated hydrochloric acid HCl was 10M.

[0081] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 3:1.

[0082] In this embodiment, in step 1), the etching reaction time is 39 hours and the reaction temperature is 30°C.

[0083] In this embodiment, the shaking and ultrasonic time is 1 hour, the rotation speed of the centrifugal treatment is 4000 rpm / min, the centrifugal time is 30 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 2M.

[0084] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 1 μm.

[0085] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 50 min, the centrifugal treatment speed is 8000 rpm / min, and the centrifugal time is 60 min.

[0086] In this embodiment, the organic composite solvent is dimethyl sulfoxide (DMSO).

[0087] Embodiment 6

[0088] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0089] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0090] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0091] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0092] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0093] In this embodiment, in step 1), Ti 3 AlC 2 The particle size of the MAX phase was 400 mesh and the concentration of concentrated hydrochloric acid HCl was 12M.

[0094] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 3:1.

[0095] In this embodiment, in step 1), the etching reaction time is 24 hours and the reaction temperature is 20°C.

[0096] In this embodiment, the shaking and ultrasonic time is 2 hours, the rotation speed of the centrifugal treatment is 2000 rpm / min, the centrifugal time is 60 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 0.1M.

[0097] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 5 μm.

[0098] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 20 min, the centrifugal treatment speed is 10000 rpm / min, and the centrifugal time is 60 min.

[0099] In this embodiment, the organic composite solvent is N,N-dimethylformamide (DMF).

[0100] Embodiment 7

[0101] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0102] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0103] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0104] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0105] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0106] In this embodiment, in step 1), Ti 3 AlC 2 The particle size of the MAX phase is 150 mesh, and the concentration of concentrated hydrochloric acid HCl is 6 MM.

[0107] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 3:1.

[0108] In this embodiment, in step 1), the etching reaction time is 24 hours and the reaction temperature is 50°C.

[0109] In this embodiment, the shaking and ultrasonic time is 0.5h, the rotation speed of the centrifugal treatment is 5000rpm / min, the centrifugal time is 15min, and the concentration of the dilute hydrochloric acid used for cleaning is 5M.

[0110] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 0.2 μm.

[0111] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 60 min, the centrifugal treatment speed is 8000 rpm / min, and the centrifugal time is 180 min.

[0112] In this embodiment, the organic composite solvent is polyethylene glycol (PEG).

[0113] Embodiment 8

[0114] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0115] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0116] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0117] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0118] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0119] In this embodiment, in step 1), Ti 3 AlC 2 The particle size of the MAX phase was 350 mesh and the concentration of concentrated hydrochloric acid HCl was 11M.

[0120] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 2.8:1.

[0121] In this embodiment, in step 1), the etching reaction time is 45 hours and the reaction temperature is 36°C.

[0122] In this embodiment, the shaking and ultrasonic time is 1.8 hours, the rotation speed of the centrifugal treatment is 4500 rpm / min, the centrifugal time is 55 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 4.5M.

[0123] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 4.5 μm.

[0124] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 55 min, the centrifugal treatment speed is 9800 rpm / min, and the centrifugal time is 160 min.

[0125] In this embodiment, the organic composite solvent is ethanol.

[0126] Embodiment 9

[0127] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0128] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0129] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0130] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0131] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0132] In this embodiment, in step 1), Ti 3 AlC 2 The particle size of the MAX phase was 350 mesh and the concentration of concentrated hydrochloric acid HCl was 10M.

[0133] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 2.5:1.

[0134] In this embodiment, in step 1), the etching reaction time is 40 hours and the reaction temperature is 45°C.

[0135] In this embodiment, the shaking and ultrasonic time is 1.5 hours, the rotation speed of the centrifugal treatment is 4000 rpm / min, the centrifugal time is 50 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 4M.

[0136] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 4 μm.

[0137] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 50 min, the centrifugal treatment speed is 9500 rpm / min, and the centrifugal time is 120 min.

[0138] In this embodiment, the organic composite solvent is deionized water.

[0139] Embodiment 10

[0140] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0141] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0142] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0143] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0144] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0145] In this embodiment, in step 1), Ti 3 AlC 2 The particle size of the MAX phase was 200 mesh and the concentration of concentrated hydrochloric acid HCl was 9M.

[0146] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 2:1.

[0147] In this embodiment, in step 1), the etching reaction time is 35 hours and the reaction temperature is 35°C.

[0148] In this embodiment, the shaking and ultrasonic time is 1.5 hours, the rotation speed of the centrifugal treatment is 3000 rpm / min, the centrifugal time is 30 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 3M.

[0149] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 3 μm.

[0150] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 45 min, the centrifugal treatment speed is 9000 rpm / min, and the centrifugal time is 120 min.

[0151] In this embodiment, the organic composite solvent is a mixture of ethanol and deionized water.

[0152] Embodiment 11

[0153] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0154] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0155] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0156] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0157] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0158] In this embodiment, in step 1), Ti 3 AlC 2 The particle size of the MAX phase was 150 mesh and the concentration of concentrated hydrochloric acid HCl was 8M.

[0159] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 2:1.

[0160] In this embodiment, in step 1), the etching reaction time is 30 hours and the reaction temperature is 30°C.

[0161] In this embodiment, the shaking and ultrasonic time is 1 hour, the rotation speed of the centrifugal treatment is 3000 rpm / min, the centrifugal time is 25 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 1M.

[0162] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 1 μm.

[0163] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 35 min, the centrifugal treatment speed is 9000 rpm / min, and the centrifugal time is 100 min.

[0164] In this embodiment, the organic composite solvent is a mixture of polyethylene glycol (PEG), ethanol and deionized water.

[0165] Embodiment 12

[0166] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0167] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0168] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0169] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0170] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0171] In this embodiment, in step 1), Ti 3 AlC 2 The particle size of the MAX phase was 400 mesh and the concentration of concentrated hydrochloric acid HCl was 7M.

[0172] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 1.2:1.

[0173] In this embodiment, in step 1), the etching reaction time is 26 hours and the reaction temperature is 25°C.

[0174] In this embodiment, the shaking and ultrasonic time is 0.8h, the rotation speed of the centrifugal treatment is 2500rpm / min, the centrifugal time is 20min, and the concentration of the dilute hydrochloric acid used for cleaning is 0.3M.

[0175] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 0.5 μm.

[0176] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 20 to 60 minutes, the centrifugal treatment speed is 8500 rpm / min, and the centrifugal time is 70 minutes.

[0177] In this embodiment, the organic composite solvent is a mixture of N,N-dimethylformamide (DMF), polyethylene glycol (PEG), ethanol and deionized water.

[0178] Embodiment 13

[0179] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0180] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0181] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0182] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0183] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0184] In this embodiment, in step 1), Ti 3 AlC 2 The particle size of the MAX phase was 150 mesh and the concentration of concentrated hydrochloric acid HCl was 12M.

[0185] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 3:1.

[0186] In this embodiment, in step 1), the etching reaction time is 48 hours and the reaction temperature is 50°C.

[0187] In this embodiment, the shaking and ultrasonic time is 2 hours, the rotation speed of the centrifugal treatment is 5000 rpm / min, the centrifugal time is 60 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 5M.

[0188] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 5 μm.

[0189] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 60 min, the centrifugal treatment speed is 10000 rpm / min, and the centrifugal time is 180 min.

[0190] In this embodiment, the organic composite solvent is a mixture of dimethyl sulfoxide (DMSO), N,N-dimethylformamide (DMF), polyethylene glycol (PEG), ethanol and deionized water.

[0191] Embodiment 14

[0192] The method for preparing the low-viscosity MXene conductive ink suitable for inkjet printing of the present invention comprises the following steps:

[0193] 1) Add LiF powder to concentrated hydrochloric acid HCl, stir until LiF is completely dissolved, then add Ti 3 AlC 2 The MAX phase is subjected to an etching reaction, the etched solid precipitate is washed and centrifuged, and the upper dispersion is collected, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets;

[0194] 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

[0195] In this embodiment, the process of washing and centrifuging the etched solid precipitate is as follows:

[0196] The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

[0197] In this embodiment, in step 1), Ti 3 AlC 2 The particle size of the MAX phase was 400 mesh and the concentration of concentrated hydrochloric acid HCl was 6M.

[0198] In this embodiment, in step 1), LiF and Ti 3 AlC 2 The mass ratio of the MAX phase is 1:1.

[0199] In this embodiment, in step 1), the etching reaction time is 24 hours and the reaction temperature is 20°C.

[0200] In this embodiment, the shaking and ultrasonic time is 0.5h, the rotation speed of the centrifugal treatment is 5000rpm / min, the centrifugal time is 15min, and the concentration of the dilute hydrochloric acid used for cleaning is 0.1M.

[0201] In this embodiment, in step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 0.2 μm.

[0202] In this embodiment, during the redispersion in step 2), the vortex oscillation time is 20 min, the centrifugal treatment speed is 8000 rpm / min, and the centrifugal time is 60 min.

[0203] In this embodiment, the organic composite solvent is a mixture of N-methylpyrrolidone (NMP), dimethyl sulfoxide (DMSO), N,N-dimethylformamide (DMF), polyethylene glycol (PEG), ethanol and deionized water.

[0204] Those skilled in the art will readily appreciate other embodiments of the present invention after considering the specification and disclosure of the invention. This application is intended to cover any variations, uses or adaptations of the present invention that follow the general principles of the present invention and include common knowledge or customary techniques in the art that are not disclosed by the present invention. The specification and examples are to be considered exemplary only, and the true scope and spirit of the present invention are indicated by the following claims.

[0205] It should be understood that the present invention is not limited to the exact construction that has been described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The scope of the present invention is limited only by the appended claims.

[0206] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent structural change made to the above embodiment based on the technical essence of the present invention still falls within the protection scope of the technical solution of the present invention.

Claims

1. A method for preparing a low-viscosity MXene conductive ink suitable for inkjet printing, characterized in that: The following steps are involved: 1) adding LiF powder to concentrated hydrochloric acid HCl, stirring to completely dissolve LiF, then adding Ti3AlC2 MAX phase for etching reaction, washing and centrifuging the etched solid precipitate, and collecting the upper dispersion, wherein the dispersion is rich in high-quality MXene single-layer / few-layer nanosheets; 2) Centrifuging the dispersion to obtain an aqueous MXene precipitate, dispersing the aqueous MXene precipitate in an organic composite solvent, then shaking, centrifuging and re-dispersing, and then adjusting the concentration with the organic composite solvent to obtain a low-viscosity MXene conductive ink suitable for inkjet printing.

2. The method for preparing a low-viscosity MXene conductive ink suitable for inkjet printing according to claim 1, characterized in that: The process of washing and centrifuging the etched solid precipitate is as follows: The etched solid precipitate was washed with dilute HCl, LiCl and deionized water in sequence until it was neutral, and then subjected to shaking, ultrasonic stripping and centrifugation.

3. The method for preparing a low-viscosity MXene conductive ink suitable for inkjet printing according to claim 1, characterized in that: In step 1), the particle size of the Ti3AlC2 MAX phase is 400-150 mesh, and the concentration of concentrated hydrochloric acid HCl is 6M-12M.

4. The method for preparing a low-viscosity MXene conductive ink suitable for inkjet printing according to claim 1, characterized in that: In step 1), the mass ratio of LiF to Ti3AlC2 MAX phase is 1 to 3:

1.

5. The method for preparing a low-viscosity MXene conductive ink suitable for inkjet printing according to claim 1, characterized in that: In step 1), the etching reaction time is 24 to 48 hours, and the reaction temperature is 20 to 50°C.

6. The method for preparing a low-viscosity MXene conductive ink suitable for inkjet printing according to claim 2, characterized in that: The shaking and ultrasonic time is 0.5 to 2 hours, the rotation speed of the centrifugal treatment is 2000 to 5000 rpm / min, the centrifugal time is 15 to 60 minutes, and the concentration of the dilute hydrochloric acid used for cleaning is 0.1 to 5M.

7. The method for preparing a low-viscosity MXene conductive ink suitable for inkjet printing according to claim 1, characterized in that: In step 1), the thickness of the MXene single-layer / few-layer nanosheets is less than 5 nm, and the average lateral size of the MXene single-layer / few-layer nanosheets is 0.2 to 5 μm.

8. The method for preparing a low-viscosity MXene conductive ink suitable for inkjet printing according to claim 2, characterized in that: During the redispersion in step 2), the vortex shaking time is 20 to 60 minutes, the centrifugal treatment speed is 8000 to 10000 rpm / min, and the centrifugal time is 60 to 180 minutes.

9. The method for preparing a low-viscosity MXene conductive ink suitable for inkjet printing according to claim 2, characterized in that: The organic composite solvent is a mixture of one or more of N-methylpyrrolidone (NMP), dimethyl sulfoxide (DMSO), N,N-dimethylformamide (DMF), polyethylene glycol (PEG), ethanol and deionized water.

10. A low-viscosity MXene conductive ink suitable for inkjet printing, characterized in that: It is prepared according to the method for preparing low-viscosity MXene conductive ink suitable for inkjet printing as described in any one of claims 1 to 9.

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