阅读说明：本技术 水溶性胶体、导电薄膜及其制备方法 (Water-soluble colloid, conductive film and preparation method thereof ) 是由 戴晓 于 2020-06-10 设计创作，主要内容包括：本发明涉及一种水溶性胶体,其为糖类和聚乙烯亚胺的混合水溶液,该胶体流动性好、粘度可调节、易溶于水且无毒无害；还涉及一种利用该水溶性胶体的导电薄膜的制备方法以及利用该方法制得的导电薄膜,生产工艺简化、过程对环境友好,所制得的导电薄膜均匀性、一致性好,电导率高。(The invention relates to a water-soluble colloid which is a mixed aqueous solution of saccharides and polyethyleneimine, has good fluidity and adjustable viscosity, is easily dissolved in water, and is non-toxic and harmless; the preparation method of the conductive film using the water-soluble colloid is also disclosed, and the conductive film prepared by the method is simple in production process, environment-friendly in process, good in uniformity and consistency and high in conductivity.)

1. The water-soluble colloid is a mixed aqueous solution of polyethyleneimine and saccharides, wherein the content ratio of the polyethyleneimine to the saccharides is 10:1-1:10, the total concentration of the surfactant and the saccharides is 1% -35%, the polyethyleneimine is linear or branched, and the molecular weight of the polyethyleneimine is 1000-100000; the saccharide is one or more of glucose, maltose, sucrose or fructose.

2. The water-soluble colloid according to claim 1, wherein the saccharide is maltose.

3. A preparation method of a conductive film comprises the following steps:

the method comprises the following steps: providing a planar latticed silk screen, and attaching the silk screen to a substrate to form a first substrate;

step two: coating the water-soluble colloid according to any one of claims 1 to 2 on the first substrate to form a second substrate in which the thickness of the water-soluble colloid is not higher than that of the screen;

step three: baking the second substrate at 70-115 ℃ to solidify the water-soluble colloid into a water-soluble colloid block, and taking down the silk screen to form a colloid block template;

step four: forming a conducting layer on the glue block template by using a film coating method to obtain a transition film, wherein the conducting layer comprises a conducting grid film formed on the substrate and a conducting sheet formed on the water-soluble glue block, and the thickness of the conducting grid film is smaller than that of the water-soluble glue block;

step five: and cleaning the transition film by water to enable the water-soluble glue block to be dissolved in water, and enabling the conducting strip to fall off to obtain the conducting film.

4. The method of manufacturing a conductive film according to claim 3, wherein the mesh has a pore size of 10 to 500 μm and a diameter of 500nm to 5 μm.

5. The method for preparing a conductive film according to claim 3, wherein in the second step, the concentration of the water-soluble colloid is 5% -30%.

6. The method for preparing a conductive film according to claim 3, wherein in the second step, the thickness of the water-soluble colloid is smaller than that of the screen.

7. The method of preparing a conductive film according to claim 3, wherein the conductive mesh film has a film thickness of 200nm to 1 μm.

8. The method of claim 7, wherein the conductive mesh film is a single-layer structure and is made of copper.

9. The method of producing a conductive film according to claim 3, wherein the mesh of the screen is square.

10. An electroconductive film, characterized in that the electroconductive film is prepared by the preparation method according to any one of claims 3 to 9.

[ technical field ] A method for producing a semiconductor device

The invention relates to the field of flexible electronic manufacturing, in particular to a water-soluble colloid, a preparation method of a conductive film using the water-soluble colloid and the prepared conductive film.

[ background of the invention ]

[ summary of the invention ]

Based on the above, the invention provides a water-soluble colloid, a preparation method of a conductive film using the water-soluble colloid, and the prepared conductive film, and solves the technical problems of complex production process, environmental friendliness, high cost, poor uniformity and consistency and the like in the prior art.

The invention provides a water-soluble colloid which is a mixed aqueous solution of polyethyleneimine and saccharides, wherein the content ratio of the polyethyleneimine to the saccharides is 10:1-1:10, the total concentration of a surfactant and the saccharides is 1% -35%, the polyethyleneimine is linear or branched, and the molecular weight of the polyethyleneimine is 1000-100000; the saccharide is one or more of glucose, maltose, sucrose or fructose.

Preferably, the saccharide is maltose.

Also provided is a method for preparing a conductive film, comprising the steps of: the method comprises the following steps: providing a planar latticed silk screen, and attaching the silk screen to a substrate to form a first substrate; step two: coating the water-soluble colloid according to any one of claims 1 to 2 on the first substrate to form a second substrate in which the thickness of the water-soluble colloid is not higher than that of the screen; step three: baking the second substrate at 70-115 ℃ to solidify the water-soluble colloid into a water-soluble colloid block, and taking down the silk screen to form a colloid block template; step four: forming a conducting layer on the glue block template by using a film coating method to obtain a transition film, wherein the conducting layer comprises a conducting grid film formed on the substrate and a conducting sheet formed on the water-soluble glue block, and the thickness of the conducting grid film is smaller than that of the water-soluble glue block; step five: and cleaning the transition film by water to enable the water-soluble glue block to be dissolved in water, and enabling the conducting strip to fall off to obtain the conducting film.

Preferably, the pore diameter of the silk screen is 10-500 μm, and the silk diameter is 500nm-5 μm.

Preferably, in the second step, the concentration of the water-soluble colloid is 5% -30%.

Preferably, in the second step, the thickness of the water-soluble colloid is smaller than that of the silk screen.

Preferably, the thickness of the film layer of the conductive grid film is 200nm-1 μm.

Preferably, the conductive grid film is of a single-layer structure and is made of copper.

Preferably, the meshes of the screen are square.

Also provides a conductive film prepared by the method.

The technical scheme provided by the invention has the following beneficial effects: firstly, the preparation method adopts an environment-friendly physical method to avoid the generation of toxic and harmful chemical waste liquid; secondly, the uniformity and the consistency of the conductive film are good, the conductive film is integrally formed without an interface, and the conductivity is high; thirdly, the conductive material is rich in selection and low in cost.

[ description of the drawings ]

FIG. 1 is a schematic flow chart of a preparation method in the first embodiment of the present invention;

FIGS. 2(a) -2(f) are schematic diagrams showing the detailed process of the preparation method in the first embodiment of the present invention;

FIG. 3 is a schematic view of a part of the structure of a water-soluble colloid after solidification in step three according to an embodiment of the present invention;

fig. 4 is a schematic partial structure diagram of a conductive film according to a first embodiment of the present invention.

[ detailed description ] embodiments

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The water-soluble colloid is a mixed aqueous solution of polyethyleneimine and saccharides, wherein the content ratio of the polyethyleneimine to the saccharides is 10:1-1:10, the total concentration of the polyethyleneimine and the saccharides is 1% -35%, the polyethyleneimine is linear or branched, and the molecular weight of the polyethyleneimine is 1000-100000; the saccharide is one or more of glucose, maltose, sucrose or fructose. Preferably, the total concentration of the polyethyleneimine and the saccharide is 5% -30%, and maltose is used as the saccharide, so that coagulation is facilitated, and the growth of the conductive layer is facilitated.

A preparation method of a conductive film comprises the following steps:

the method comprises the following steps: providing a planar latticed silk screen, and attaching the silk screen to a substrate to form a first substrate. The shape and size of the silk screen and the substrate can be adjusted according to the size of an actual product, and the pore diameter of the silk screen is 10-500 μm, preferably 20-200 μm; the diameter of the filament is 500nm-5 μm.

The mesh shape may be square, rectangular, circular, oval, diamond, parallelogram, or other polygonal shape.

The substrate may be an inorganic glass substrate, or may be an organic flexible substrate, such as a polyester film (PET), a polyimide film (PI), or the like.

In order to ensure good printing effect, the silk screen and the substrate need to be closely attached without gaps, so that a complete conductive film with good consistency can be formed in the subsequent steps.

Step two: and coating the water-soluble colloid on the first substrate, coating the water-soluble colloid on the silk screen by a blade coating method, and enabling the water-soluble colloid to permeate into meshes of the silk screen and contact with the substrate.

After the blade coating is completed, a second substrate is formed, in the second substrate, the thickness of the water-soluble colloid is not higher than that of the silk screen, and the upper surface of the silk screen far away from the substrate needs to be exposed outside, namely the upper surface of the water-soluble colloid is flush with or lower than the upper surface of the silk screen, so that the silk screen can be removed in the subsequent step.

The total concentration of said polyethyleneimine and said saccharide in the water-soluble colloid is 1% to 35%, preferably in the range of 5% to 30%, in which the water-soluble colloid has good fluidity and is easily solidified to be separated from the screen in a subsequent step.

Step three: and baking the second substrate at 70-115 ℃ to evaporate water in the water-soluble colloid and reduce the fluidity, so that the water-soluble colloid in the meshes is solidified into water-soluble colloid blocks, the thickness of the water-soluble colloid blocks is smaller than that of the water-soluble colloid, taking down the silk screen, attaching the water-soluble colloid blocks in the meshes to the surface of the substrate, forming clear intervals among the water-soluble colloid blocks, and completely exposing the surface of the substrate in the intervals to form a colloid block template.

The environment temperature of baking is controlled between 70 ℃ and 115 ℃, the solidification speed of the water-soluble colloid can be accelerated, the production period is shortened, and meanwhile, the chemical components of the water-soluble colloid cannot be damaged, so that the solidified water-soluble colloid block has a complete shape and clear edges, the yield of the conductive film is improved, and the cost is reduced. When the environmental temperature is lower than 70 ℃, the water-soluble colloid is slowly solidified, the production period is prolonged, and when the environmental temperature is higher than 115 ℃, the physical properties of the water-soluble colloid are destroyed, and the water-soluble colloid can not be dissolved in water again due to the solidification reaction.

Step four: and forming a conductive layer on the rubber block template by using a film coating method to obtain a transition film, wherein the conductive layer comprises a conductive grid film formed on the substrate and a conductive sheet formed on the water-soluble rubber block, and in order to separate the conductive grid film in the subsequent step, the thickness of the conductive grid film needs to be smaller than that of the water-soluble rubber block, so that the conductive grid film and the conductive sheet are prevented from being adhered.

Specifically, a conductive layer can be grown on the surface of the rubber block template by a coating method such as evaporation, magnetron sputtering, electron beam deposition, vapor phase chemical deposition or pulse laser deposition, and the thickness of the conductive layer is 50nm-1 μm.

In addition, the conducting layer can be a single-layer structure, and the thickness is between 200nm and 1 μm, preferably between 400nm and 600 nm; the thickness of each layer can be adjusted according to the performance requirement and the material characteristics, for example, in a three-layer structure, two peripheral layers are made of materials with good chemical stability, such as aluminum, nickel or corrosion-resistant alloy, and the thickness is 50nm-150nm, and an intermediate layer is made of materials with good conductivity, such as copper and silver, and the thickness is 300nm-500nm, so that the requirement of conductivity and light transmittance can be met, the requirements of corrosion resistance and ageing resistance can be met, and the sum of the thicknesses of the layers is smaller than that of the water-soluble glue block.

The conductive material is also rich in selection, can be simple substance metal or alloy metal, and can also be graphene or other conductive materials.

Step five: and cleaning the transition film by water to enable the water-soluble glue block to be dissolved in water, and enabling the conducting strip to fall off to obtain the conducting film. The water flow speed and the cleaning direction need to be controlled in the cleaning process so as to prevent the falling conducting strips from damaging the structure of the conducting grid film.

(embodiment one)

Referring to fig. 1, fig. 2(a) -2(d), and fig. 3-4, the method for preparing the conductive film in this embodiment includes the following steps:

the method comprises the following steps: a planar grid-like screen 102 of nickel with dimensions of 10cm x 10cm, square meshes with a pore diameter of 100 μm and a wire diameter of 2 μm is provided. The screen 102 is attached to the surface of the substrate 101 to form the first substrate 11. In this example, the substrate is a PET film.

Step two: the water-soluble colloid 103 having a concentration of 30% was spread on the first substrate 11 to form the second substrate 12, in which second substrate 12 the thickness of the water-soluble colloid 103 was not higher than that of the screen 102, and the water-soluble colloid 103 was allowed to penetrate into the meshes of the screen 102 and adhered to the PET substrate 101.

Step three: and baking the second substrate 12 for 2-10 minutes at the temperature of 100 ℃ to remove moisture, solidifying the water-soluble colloid 103 into a water-soluble colloid block 104, wherein the thickness of the water-soluble colloid block 104 is smaller than that of the water-soluble colloid block 103, and taking down the silk screen 102 to obtain the PET film printed with the micro-nano array of the water-soluble colloid block 104, namely the colloid block template 13. The printed water-soluble glue block 104 has a stable block shape with block sides of 100 μm, block gaps of 2 μm, and the bottom of the gap is the bare PET substrate 101. Fig. 3 is a schematic front view of the glue block stencil and the screen after baking and before removing the screen.

Step four: forming a conductive layer 105 on the glue block template 13 by using a magnetron sputtering method to obtain a transition film 14, wherein the conductive layer 105 is uniformly deposited on the surface of the water-soluble glue block 104 and in a slit between the water-soluble glue blocks, the conductive layer 105 comprises a conductive grid film 1052 formed on the substrate 101 and a conductive sheet 1051 formed on the water-soluble glue block 104, the thicknesses of the conductive grid film 1052 and the conductive sheet 1051 are the same, and the thickness of the conductive grid film 1052 is smaller than that of the water-soluble glue block 104; in this embodiment, the conductive layer 105 is made of copper and has a thickness of 500 nm.

Step five: the transition thin film 14 is washed with water, so that the water-soluble glue block 104 is dissolved in water, the conductive sheet 1051 falls off, and the copper film 1052 in the slit remains on the surface of the substrate 101, thereby obtaining the conductive thin film 10 (a transparent conductive micro-nano copper thin film), as shown in fig. 4, a front structural schematic diagram of the conductive thin film 10 is shown.

The square resistance of the prepared conductive film 10 is 0.95 omega, the conductivity is high, the transmittance of the 350nm-750nm wavelength is more than 85%, and the transparency is good. And in the preparation process, no toxic and harmful chemical waste liquid is generated, and the production process is safe.

In conclusion, according to the water-soluble colloid disclosed by the invention, the colloid has good fluidity and adjustable viscosity, is easy to dissolve in water, is non-toxic and harmless, and a compact and uniform conductive layer can be formed on the surface of a conductive material in a coating process. The transparent conductive film has the following beneficial effects: firstly, the preparation method adopts an environment-friendly physical method to avoid the generation of toxic and harmful chemical waste liquid; secondly, the uniformity and the consistency of the conductive film are good, the conductive film is integrally formed without an interface, and the conductivity is high; thirdly, the material selection is abundant and the cost is low.

The conductive film has a wide application range, for example, the obtained conductive film is covered on the surface of a substrate, a capacitive touch panel can be obtained after processing, and after the capacitive touch panel is connected with a controller and a software driver, the capacitive touch panel can realize single-point touch and multi-point touch functions, has very good flexibility and achieves the expected target. For another example, the obtained conductive films are respectively covered on two sides of a plastic liquid crystal film, the conductive films on the two sides are used as electrodes to form a planar capacitor with a sandwich structure, and when a certain voltage is applied to the two electrodes, an electric field can be formed between the electrodes, so that the originally atomized liquid crystal film becomes transparent, the function of electro-dimming is realized, and the electro-dimming glass can be applied to electro-dimming glass of buildings or intelligent windows of automobiles.

The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the inventive concept of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.