Preparation device and preparation method of silver conductive ink material for conformal circuit

Abstract

The invention provides a device and method for preparing a silver conductive ink material for a conformal circuit, and relates to the technical field of conductive ink material.The device comprises an upper airtight glove box and a lower airtight glove box, and a solid-liquid separator is arranged between the upper airtight glove box and the lower airtight glove box in a penetrating mode; the solid-liquid separator comprises an inner cylinder, a funnel arranged on the upper airtight glove box and an outer cylinder arranged on the lower airtight glove box, the bottom of the outer cylinder is sealed and locked by a plug through Morse taper, and a filter membrane is fixed at the bottom of the inner cylinder through a sealing ring; a magnetic stirrer, a powder injector, a liquid injector and a sealing bottle are arranged in the upper airtight glove box, and the upper airtight glove box is provided with a ventilation filtering system. The silver conductive ink material is prepared in the upper airtight glove box and the lower airtight glove box of the silver conductive ink material preparation device, so that the safety of testers is effectively guaranteed, volatile harmful gas generated by inhaling ammonia water and precipitated nano-silver particles are avoided, and meanwhile, the environment in the silver conductive ink material preparation process is kept clean; and dust particles entering the silver conductive ink material are reduced.

Description

Technical Field

[0001] The present application relates to the technical field of conductive ink material preparation, and more specifically, to a device and method for preparing silver conductive ink material for conformal circuits. Background Art

[0002] Silver conductive ink can be printed on curved surface components by inkjet printing to form conformal circuits. Conformal circuits have a wide range of applications and significant advantages. For example, conformal antennas on the surface of drones can greatly reduce their own weight, reduce radar reflection area, and improve maneuverability, aerodynamics, and stealth.

[0003] The technical solutions for preparing silver conductive ink materials in the prior art include:

[0004] (1) A Chinese invention patent with publication number CN111269616A discloses a nanosilver conductive ink and a low-temperature sintering method thereof, wherein the method uses a double protective agent to prepare nanosilver particles, treats the prepared nanosilver particles with a polyaluminium chloride solution, and performs auxiliary sintering treatment on the nanosilver ink using ultraviolet light and HCl solutions of different concentrations. Using the method disclosed in the invention patent, the nanosilver conductive ink has a low sintering temperature, the conductive ink has a uniform and complete morphology after sintering, and the sintered silver layer has excellent conductivity.

[0005] (2) Chinese invention patent with publication number CN104817891A, a direct-write nano-silver conductive ink and its preparation method, the mass percentage composition of which includes: 5-60% silver nanoparticles coated with anionic surfactants, 40-95% ink solvent, the ink solvent is composed of Class A liquid and Class B solid in a mass ratio of 1: (0.01-0.001), Class A liquid is selected from at least one of 1,2-propylene glycol, triethanolamine, oleic acid and deionized water; Class B solid is selected from at least one of benzotriazole, 2,2-dibromo-2-cyanoacetamide and hydroxyethyl cellulose. The preparation method of the direct-write nano-silver conductive ink of the invention is simple and easy to operate; the viscosity of the direct-write nano-silver conductive ink at 20°C is 100-500mPa·s, and the surface tension at 20°C is 30-50mN·m -1 .

[0006] In the production process of silver conductive ink materials, nano-silver particles are used as necessary production raw materials. The toxicity characteristics of silver particles are related to their particle size. The smaller the particle size, the stronger the toxicity. Studies have shown that nano-silver particles of about 20nm are the most toxic, and their toxicity mainly manifests as cytotoxicity and reproductive toxicity. In order to achieve the safe production of silver conductive ink materials, a device for preparing silver conductive ink materials for conformal circuits is needed. Summary of the invention

[0007] To solve the above problems, the technical solution adopted in the present application is a device for preparing silver conductive ink material for conformal circuits and a preparation method thereof, comprising an upper airtight glove box and a lower airtight glove box stacked up and down, a solid-liquid separator is arranged between the upper airtight glove box and the lower airtight glove box, the solid-liquid separator comprises an inner cylinder, a funnel arranged in the upper airtight glove box and an outer cylinder arranged in the lower airtight glove box, the bottom of the outer cylinder is locked by a stopper through a Morse taper seal, and a filter membrane is fixed to the bottom of the inner cylinder through a sealing ring; a magnetic stirrer, a silver acetate powder injector, a formic acid liquid injector, an ammonia water sealed bottle and a silver conductive ink sealed bottle are arranged inside the upper airtight glove box, the upper airtight glove box is provided with a ventilation and filtration system, and both the upper airtight glove box and the lower airtight glove box are provided with operating holes, operating gloves and airtight doors.

[0008] Optionally, there are m×n magnetic stirrers, wherein m is the number of rows, n is the number of columns, m≥2, n≥2.

[0009] Optionally, the ventilation and filtering system is arranged on the top of the upper airtight glove box.

[0010] Optionally, an air curtain device is provided on the top of the airtight door.

[0011] Optionally, the pore size of the filter membrane is 0.2 microns.

[0012] Optionally, the sealing ring is made of fluororubber, and the filter membrane is made of polytetrafluoroethylene or polypropylene.

[0013] The present application also provides a method for preparing a silver conductive ink material for a conformal circuit, which is manufactured using any of the aforementioned devices for preparing a silver conductive ink material for a conformal circuit.

[0014] Optionally, the following steps are included:

[0015] S1: Place a sealed quartz bottle containing ammonia water, a sealed quartz bottle containing formic acid, an empty sealed quartz bottle, and vacuum-packed silver acetate powder into an upper airtight glove box, place the empty sealed quartz bottle into a lower airtight glove box, complete the sealing of the upper and lower airtight glove boxes, and start the ventilation and filtration system;

[0016] S2: Stirring ammonia water and adding to the silver acetate powder injector and formic acid liquid injector;

[0017] S3: adding silver acetate to the ammonia water through a silver acetate powder injector, stirring until the silver acetate is completely dissolved to form a silver acetate ammonia complex;

[0018] S4: adding formic acid to the ammonia water containing the silver acetate ammonia complex through a formic acid injector to generate ammonia formate, sealing a quartz sealed bottle loaded with ammonia water, ammonia formate and the silver acetate ammonia complex, and letting it stand for 24 hours to obtain a silver conductive ink material containing precipitated silver particles;

[0019] S5: separating the precipitated silver particles and the silver conductive ink material by a solid-liquid separation device;

[0020] S6: Performing harmless recovery treatment on the separated silver;

[0021] S7: Silver conductive ink is printed on a curved surface component by inkjet printing to form a conformal circuit, and the conformal circuit is subjected to material and electrical tests.

[0022] Optionally, step S5 includes: placing the silver conductive ink material containing the precipitated silver particles into the funnel of the solid-liquid separator, placing the inner cylinder into the funnel from top to bottom, so that the silver conductive ink material enters the inner cylinder through the sieve holes of the filter membrane, and the silver particles are intercepted by the filter membrane in the area between the inner cylinder and the funnel.

[0023] Optionally, step S6 includes collecting the silver particles, drying them in a drying oven, and sealing and storing them in a quartz sealed bottle, and cleaning the inner cylinder and the sealing cone surface.

[0024] The beneficial effects of the silver conductive ink material preparation device and preparation method for conformal circuit provided by the present application are:

[0025] The silver conductive ink material is prepared in the upper airtight glove box and the lower airtight glove box of the silver conductive ink material preparation device, which effectively ensures the safety of the test personnel and avoids the inhalation of volatile harmful gases produced by ammonia water and precipitated nano-silver particles. At the same time, the environment of the silver conductive ink material preparation process is kept relatively clean to reduce the entry of dust particles into the silver conductive ink material. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for use in the embodiments or descriptions of the prior art.

[0027] Figure 1 A schematic diagram of a device for preparing a silver conductive ink material for a conformal circuit provided in an embodiment of the present application;

[0028] Figure 2 A schematic diagram of a solid-liquid separation device for silver conductive ink material provided in an embodiment of the present application;

[0029] Figure 3 for Figure 2 A magnified view of the local area A;

[0030] Figure 4 for Figure 2 Enlarged view of local B.

[0031] Explanation of the reference numerals: 1-upper airtight glove box; 101-upper operating hole; 102-upper rubber gloves; 103-upper airtight door; 2-magnetic stirrer; 3-quartz sealed bottle; 4-silver acetate powder injector; 5-formic acid liquid injector; 6-upper tool box; 7-silver acetate powder bag; 8-solid-liquid separator; 801-funnel; 802-outer cylinder; 803-stopper; 804-sealing cone; 805-inner cylinder; 806-filter membrane; 807-sealing ring; 808-liquid level; 9. Lower airtight glove box; 901-lower operating hole; 902-lower rubber gloves; 903-lower airtight door; 10-lower tool box; 11-drying box. DETAILED DESCRIPTION

[0032] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present application more clearly understood, the present application is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and are not used to limit the present application.

[0033] like Figures 1 to 4 As shown, a device for preparing silver conductive ink material for conformal circuit and a preparation method thereof, comprising an upper airtight glove box 1 and a lower airtight glove box 9 stacked up and down, a solid-liquid separator 8 is arranged between the upper airtight glove box 1 and the lower airtight glove box 9, the solid-liquid separator 8 comprises an inner cylinder 805, a funnel 801 arranged on the upper airtight glove box 1 and an outer cylinder 802 arranged on the lower airtight glove box 9, the bottom of the outer cylinder 802 is locked by a plug 803 through a Morse taper seal, and a filter membrane 806 is fixed to the bottom of the inner cylinder 805 through a sealing ring 807; a magnetic stirrer 2, a silver acetate powder injector 4, a formic acid injector 5, an ammonia water sealed bottle and a silver conductive ink sealed bottle are arranged inside the upper airtight glove box 1, the ammonia water sealed bottle and the silver conductive ink sealed bottle are quartz sealed bottles 3, the upper airtight glove box 1 is provided with a ventilation and filtration system, and the upper airtight glove box 1 and the lower airtight glove box 9 are both provided with operating holes, operating gloves and airtight doors. An upper tool box 6 and a lower tool box 10 are respectively provided inside the upper airtight glove box 1 and the lower airtight glove box 9 for storing experimental equipment required for preparing silver conductive ink.

[0034] The upper airtight glove box 1 is provided with an upper operation hole 101, an upper rubber glove 102 and an upper airtight door 103, and the lower airtight glove box 9 is provided with a lower operation hole 901, a lower rubber glove 902 and a lower airtight door 903. The silver conductive ink material is prepared in the upper airtight glove box 1 and the lower airtight glove box 9 of the silver conductive ink material preparation device, which effectively ensures the safety of the test personnel, avoids the inhalation of volatile harmful gases generated by ammonia water and precipitated nano silver particles, and keeps the environment of the silver conductive ink material preparation process relatively clean, reducing the dust particles from entering the silver conductive ink material.

[0035] like Figure 1As shown, in another embodiment of the present application, the magnetic stirrer 2 is provided with m×n pieces, wherein m is the number of rows, n is the number of columns, m≥2, n≥2. Based on the high-throughput design concept, m×n heating stirrers 2 are provided, and m×n groups of experiments are carried out at the same time, which can fully maintain the consistency of experimental conditions and experimental environment, based on the silver acetate powder injector 4 with three degrees of freedom movement and powder injection quality servo control function, and the formic acid injector 5 with three degrees of freedom movement and drip volume servo control function, silver acetate and formic acid are added according to the high-throughput design amount gradient, and m×n kinds of silver conductive ink materials are obtained under the same experimental environment conditions.

[0036] like Figure 1 As shown, in another embodiment of the present application, the ventilation and filtration system is arranged on the top of the upper airtight glove box 1. Ammonia water volatilizes to produce ammonia gas, which has a density lower than that of air and moves upward after volatilization. The ventilation and filtration system is arranged on the top of the upper airtight glove box 1, which can quickly remove the ammonia gas in the silver conductive ink material preparation device for conformal circuits provided by the present application.

[0037] like Figure 1 As shown, in another embodiment of the present application, an air curtain device is provided at the top of the airtight door. An air curtain device for supplying air from top to bottom is provided at the top of the upper airtight door 103 and the lower airtight door 903. When the airtight door is opened, the air curtain device reduces the number of dust particles entering the upper airtight glove box 1 and the lower airtight glove box 9.

[0038] like Figure 4 As shown, in another embodiment of the present application, the pore size of the filter membrane 806 is 0.2 microns. In an environment with a high pH value, the agglomeration effect between the nanosilver particles is weakened, but the agglomeration phenomenon still exists. The part of the nanosilver particles prepared by silver ammonia complexation that is not effectively dispersed in the silver conductive ink and the part with too large particle size can be effectively intercepted by the 0.2 micron filter membrane 806, thereby improving the dispersion effect of the nanosilver particles in the prepared silver conductive ink.

[0039] like Figure 4 As shown, in another embodiment of the present application, the sealing ring 807 is made of fluororubber, and the filter membrane 806 is made of polytetrafluoroethylene or polypropylene. Both fluororubber and polytetrafluoroethylene contain carbon-fluorine bonds and have strong chemical stability, among which fluororubber has better elasticity and is used for the sealing ring 807. Since the silver conductive ink material preparation device for conformal circuit provided by the present application is operated in a room temperature environment, as a feasible alternative, the filter membrane 806 can be made of polypropylene.

[0040] The present application also provides a method for preparing a silver conductive ink material for a conformal circuit, which is manufactured using any of the aforementioned devices for preparing a silver conductive ink material for a conformal circuit.

[0041] like Figures 1 to 4 As shown, in another embodiment of the present application, the following steps are included:

[0042] S1: Place the quartz sealed bottle 3 encapsulated with ammonia water, the quartz sealed bottle 3 encapsulated with formic acid, the empty quartz sealed bottle 3 and the vacuum-packed silver acetate powder package 7 into the upper airtight glove box 1, place the empty quartz sealed bottle 3 into the lower airtight glove box 9, complete the sealing of the upper airtight glove box 1 and the lower airtight glove box 9, and start the ventilation and filtration system;

[0043] S2: Stirring ammonia water and adding it to the silver acetate powder injector 4 and the formic acid liquid injector 5;

[0044] S3: Add silver acetate to the ammonia water through the silver acetate powder injector 4, and stir until the silver acetate is completely dissolved to generate a silver acetate ammonia complex, the chemical formula of which is as follows:

[0045] 2NH3+CH3CO2Ag→[Ag(NH3)2]CH3CO2;

[0046] S4: Formic acid is added to the ammonia water containing the silver acetate ammonia complex through the formic acid injector 5 to generate formic acid ammonia, and the chemical formula is as follows:

[0047] HCO2H+NH3→NH4CO2H;

[0048] The quartz sealed bottle 3 loaded with ammonia water, ammonium formate and silver acetate ammonia complex is sealed and left to stand for 24 hours to obtain a silver conductive ink material containing precipitated silver particles;

[0049] S5: separating the precipitated silver particles and the silver conductive ink material by a solid-liquid separation device 8;

[0050] S6: Performing harmless recovery treatment on the separated silver;

[0051] S7: Silver conductive ink is printed on the curved surface component by inkjet printing to prepare a conformal circuit. The chemical formula is as follows:

[0052] 2[Ag(NH3)2]CH3CO2+NH4CO2H→2Ag+5NH3+2CH3CO2H+CO2;

[0053] The fabricated conformal circuits were subjected to material and electrical tests.

[0054] like Figures 1 to 4As shown, in another embodiment of the present application, step S5 includes: placing the silver conductive ink material containing the precipitated silver particles into the funnel 801 of the solid-liquid separator 8, placing the inner cylinder 805 into the funnel 801 from top to bottom, so that the silver conductive ink material enters the inner cylinder 805 through the sieve holes of the filter membrane 806, and the silver particles are intercepted by the filter membrane 806 in the area between the inner cylinder 805 and the funnel 801. The liquid level 808 of the silver conductive ink material is controlled not to exceed the bottom surface of the upper airtight glove box, the height of the outer cylinder 802 below the bottom surface of the upper airtight glove box that can accommodate liquid is 20-40 cm, and the pressure above the plug 803 is controlled, and the plug 803 and the outer cylinder 802 are made of polytetrafluoroethylene.

[0055] like Figures 1 to 4 As shown, in another embodiment of the present application, step S6 includes collecting the silver particles, drying them in a drying oven 11 and sealing and storing them in a quartz sealing bottle 3, and cleaning the inner cylinder 805 and the sealing cone surface 804.

[0056] The above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. These modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present application, and should all be included in the protection scope of the present application.

Claims

1. A device for preparing silver conductive ink material for conformal circuits, characterized in that: It comprises an upper airtight glove box and a lower airtight glove box stacked up and down, a solid-liquid separator is arranged between the upper airtight glove box and the lower airtight glove box, the solid-liquid separator comprises an inner cylinder, a funnel arranged in the upper airtight glove box and an outer cylinder arranged in the lower airtight glove box, the bottom of the outer cylinder is locked by a plug through a Morse taper seal, and a filter membrane is fixed to the bottom of the inner cylinder through a sealing ring; a magnetic stirrer, a silver acetate powder injector, a formic acid liquid injector, an ammonia water sealed bottle and a silver conductive ink sealed bottle are arranged inside the upper airtight glove box, a ventilation and filtration system is arranged in the upper airtight glove box, and both the upper airtight glove box and the lower airtight glove box are provided with operating holes, operating gloves and airtight doors.

2. The device for preparing silver conductive ink material for conformal circuit according to claim 1, characterized in that: The magnetic stirrers are provided in m×n numbers, wherein m is the number of rows, n is the number of columns, m≥2, n≥2.

3. The device for preparing silver conductive ink material for conformal circuit according to claim 1, characterized in that: The ventilation and filtering system is arranged on the top of the upper airtight glove box.

4. The device for preparing silver conductive ink material for conformal circuit according to claim 2, characterized in that: An air curtain device is arranged on the top of the airtight door.

5. The device for preparing silver conductive ink material for conformal circuit according to claim 3, characterized in that: The pore size of the filter membrane is 0.2 microns.

6. The device for preparing silver conductive ink material for conformal circuit according to claim 5, characterized in that: The sealing ring is made of fluororubber, and the filter membrane is made of polytetrafluoroethylene or polypropylene.

7. A method for preparing a silver conductive ink material for a conformal circuit, characterized in that: The method is manufactured using the silver conductive ink material preparation device for conformal circuits as described in any one of claims 1 to 6.

8. The method for preparing the silver conductive ink material for conformal circuits according to claim 7, characterized in that: The following steps are involved: S1: Place a sealed quartz bottle containing ammonia water, a sealed quartz bottle containing formic acid, an empty sealed quartz bottle, and vacuum-packed silver acetate powder into an upper airtight glove box, place the empty sealed quartz bottle into a lower airtight glove box, complete the sealing of the upper and lower airtight glove boxes, and start the ventilation and filtration system; S2: Stirring ammonia water and adding to the silver acetate powder injector and formic acid liquid injector; S3: adding silver acetate to the ammonia water through a silver acetate powder injector, stirring until the silver acetate is completely dissolved to form a silver acetate ammonia complex; S4: adding formic acid to the ammonia water containing the silver acetate ammonia complex through a formic acid injector to generate ammonia formate, sealing a quartz sealed bottle loaded with ammonia water, ammonia formate and the silver acetate ammonia complex, and letting it stand for 24 hours to obtain a silver conductive ink material containing precipitated silver particles; S5: separating the precipitated silver particles and the silver conductive ink material by a solid-liquid separation device; S6: Performing harmless recovery treatment on the separated silver; S7: Silver conductive ink is printed on a curved surface component by inkjet printing to form a conformal circuit, and the conformal circuit is subjected to material and electrical tests.

9. The method for preparing the silver conductive ink material for conformal circuits according to claim 8, characterized in that: Step S5 includes: placing the silver conductive ink material containing the precipitated silver particles into the funnel of the solid-liquid separator, placing the inner tube into the funnel from top to bottom, allowing the silver conductive ink material to enter the inner tube through the sieve holes of the filter membrane, and the silver particles are intercepted by the filter membrane in the area between the inner tube and the funnel.

10. The method for preparing the silver conductive ink material for conformal circuits according to claim 8, characterized in that: Step S6 includes collecting the silver particles, drying them in a drying oven, sealing and storing them in a quartz sealed bottle, and cleaning the inner cylinder and the sealing cone surface.

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