CN110747439A - Preparation method of micron-sized ultrathin metal sheet for conductive adhesive filler - Google Patents
Preparation method of micron-sized ultrathin metal sheet for conductive adhesive filler Download PDFInfo
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- CN110747439A CN110747439A CN201910859678.8A CN201910859678A CN110747439A CN 110747439 A CN110747439 A CN 110747439A CN 201910859678 A CN201910859678 A CN 201910859678A CN 110747439 A CN110747439 A CN 110747439A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0005—Separation of the coating from the substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
- C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5873—Removal of material
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Abstract
The invention provides a preparation method of a micron-sized ultrathin metal sheet for conductive adhesive, which comprises the following steps: (1) coating the cracking liquid on a substrate; (2) controlling the temperature, the humidity and the time to enable the cracking liquid to naturally crack to form a cracking template of micron-sized cracking blocks; (3) depositing a metal film on the cracking template in a vacuum coating mode; (4) and separating the cracking block from the substrate, and then separating the metal film from the cracking block to obtain the micron-sized ultrathin metal sheet. Compared with the traditional mechanical ball milling method, light induction method, template method, chemical reduction method and the like, the preparation method of the invention has the advantages of simplicity, low manufacturing cost, high yield, industrialized production and no pollution; the prepared micron-sized ultrathin metal sheet has the advantages of good thickness uniformity, super-large specific surface area, excellent electrical property, no introduction of impurity atoms, and controllable size and thickness dimension of the micron-sized ultrathin metal sheet through different concentrations of cracking liquid, deposition power and time.
Description
Technical Field
The invention belongs to the field of electronic components, and particularly relates to a preparation method of a micron-sized ultrathin metal sheet for a conductive adhesive filler.
Background
The electronic component manufacturing industry is a main component of the electronic component industry and is also the basis of the electronic information industry, and the technical level and the production capacity of the electronic component manufacturing industry directly influence the development of the whole industry. The conductive adhesive has high conductivity, excellent adhesion performance, weldability and other mechanical properties, and becomes a key functional material for producing various electronic component products. The conductive adhesive is an adhesive with certain conductive performance after being cured or dried, and generally takes matrix resin and conductive filler, namely conductive particles as main components, and the conductive particles are combined together through the bonding action of the matrix resin to form a conductive path so as to realize the conductive connection of the bonded materials. The conductive adhesive is widely applied to the fields of microelectronic assembly, low-temperature electric welding, solar cells and the like. Silver is selected as the conductive filler of the solar cell conductive adhesive, and the conductive adhesive has the following advantages: (1) the silver has good electric conduction and heat conduction properties; (2) the reduction sintering temperature range of the silver conductive adhesive is wide and is 400-900 ℃; (3) silver has good oxidation resistance and weldability. At present, the conductive adhesive market is basically occupied by foreign manufacturers, and the conductive adhesive still depends on import due to the difference of the conductivity and the cost of the domestic silver conductive adhesive.
The silver powder plays a central role in the silver conductive adhesive, and the shape structure, the granularity, the distribution characteristic, the loose packing and tap density, the specific surface area, the sintering performance, the corrosion resistance and the like of the silver powder can influence the service performance of the conductive adhesive. In the preparation of the silver conductive adhesive, the granularity of the silver powder with excellent performance meets the requirements of the conductive adhesive. The silver powder has an excessively small average particle diameter, and needs to be wetted with more organic vehicle, resulting in a low conductive gel content. The average particle size of the silver powder is too large, so that more interstitial holes are reserved when the silver conductive adhesive is sintered, and the contact resistance and the series resistance are higher.
In general, silver powders have two methods of classification. One of them is divided into four kinds of fine, superfine and nano silver powder according to the size of particle. The second one can be divided into spherical, flaky, dendritic and mixed silver powder according to their morphology. In the existing research, spherical, dendritic and flake silver powders have been used for silver conductive paste, wherein the silver conductive paste prepared from dendritic silver powder has proved to have the worst electrical performance because the dendritic silver powder has a large spatial structure, and although there are many contact points, there are many pores in the sintered film and the surface is rough. And for the point contact between the spherical silver powder, the flaky silver particles are in surface contact and line contact, the contact surface is larger, meanwhile, the flaky silver powder can also form the overlapping of an upper lamella and a lower lamella in the slurry, and the powder flowability is better, so that the formed conductive channel has lower resistance and better conductivity. Particularly, the silver conductive adhesive prepared from the flake silver powder has more obvious electrical property advantages under the state of low solid content. And the flake silver powder has high tap density, and the high tap density is beneficial to reducing the using amount of the organic carrier and improving the solid content. Meanwhile, the specific surface area of the flake silver powder is large, so that the use amount of silver is reduced, and the cost can be reduced.
At present, the preparation methods of flake silver powder on the market are various, such as a mechanical ball milling method, a photoinduction method, a template method, a chemical reduction method and the like. The mechanical ball milling method is the main method for industrially producing the flake silver powder at present, has the advantages of simple process, high yield, relatively low cost and the like, but still has the following problems that the size of the ground silver powder is not easy to control, the uniformity is inconsistent, new impurities are easily brought in, and the energy consumption of a ball mill is high. The process and equipment for preparing the flaky silver powder by the light induction method are simple, but the light irradiation time is long, the production efficiency is low, the prepared flaky silver powder is not bright in color, and the sintered silver powder is dark and yellow in appearance. Therefore, the conventional photoinduction method for preparing the flake silver powder is difficult to realize industrialization. The template method has the advantages of simple process, good reaction reproducibility, easy control and the like for preparing nano materials with special shapes, but the method has good effect only in the aspect of preparing nano silver sheets, and still has many problems to be solved for preparing micron-level silver sheets with larger sheet diameters. The flake silver powder prepared by the chemical reduction method is free from further pollution caused by mechanical ball milling, has high purity and uniform particle structure, can accurately control reaction conditions, and is favorable for obtaining the flake silver with controllable particle size and shape. However, the silver particle concentration is low, the cost is high, the yield is low, the requirement for a large amount of flake silver powder cannot be met, and the problems that the shape of the silver nanoparticle is uncontrollable, the particle size distribution range is wide and the like can be caused by increasing the silver particle concentration of a reaction system. In order to ensure good dispersibility, it is generally necessary to add more dispersants (protectors), which are difficult to remove completely in the subsequent washings, and some of them even contain elemental sulphur.
Disclosure of Invention
The invention aims to provide a preparation method of a micron-sized ultrathin metal sheet for a conductive adhesive filler, wherein the micron-sized ultrathin metal sheet is simple in preparation method and low in cost; the prepared micron-sized ultrathin metal sheet has large specific surface area and excellent performance.
The above purpose of the invention is realized by the following technical scheme:
a preparation method of micron-sized ultrathin metal sheets for conductive adhesive fillers comprises the following steps:
(1) coating the cracking liquid on a substrate;
(2) controlling the temperature, the humidity and the time to enable the cracking liquid to naturally crack to form a cracking template of micron-sized cracking blocks;
(3) depositing a metal film on the cracking template in a vacuum coating mode;
(4) and separating the cracking block from the substrate, and then separating the metal film from the cracking block to obtain the micron-sized ultrathin metal sheet.
In the preparation method, the substrate can be made of different materials, the hard substrate is glass, and the soft substrate is polyethylene terephthalate (PET) or polyethylene naphthalate (PEN).
In the preparation method, the cracking liquid comprises protein sol, polymer coating or oxide sol.
Preferably, the protein sol is natural egg white or artificial protein powder colloid, the high polymer coating is methyl oil CA600, and the oxide sol is titanium dioxide sol.
In the preparation method, the coating method of the cracking liquid comprises spray coating, dip coating, blade coating or spin coating. Preferably, a doctor blade is used.
In the preparation method, the cracking temperature of the cracking liquid is controlled to be 40-80 ℃, the humidity is controlled to be 60-80% RH, and the time is controlled to be 8-12 min.
Preferably, the cracking temperature of the cracking liquid is controlled at 60 ℃, the humidity is controlled at 70% RH, and the time is controlled at 10 min.
In the preparation method, the diameter of the micron-sized schizophyllum commune blocks is 20-400 microns.
In the preparation method of the invention, before the surface of the substrate is coated with the cracking liquid, the substrate can be pretreated: the substrate is firstly placed into deionized water for ultrasonic heating and cleaning, then nitrogen is introduced for drying, and then plasma cleaning is carried out after drying.
In the preparation method, the vacuum coating method comprises thermal evaporation, chemical vapor deposition, ion sputtering or magnetron sputtering; the thickness of the metal film is 20-500 nm.
Preferably, the vacuum coating is carried out by magnetron sputtering. The film prepared by magnetron sputtering has good quality and low cost.
Further, when magnetron sputtering is adopted for plating a metal film, a roll-to-roll mode is selected for sputtering the metal film on the surface of the PET substrate, and the magnetron sputtering power is 1-100 KW.
In the preparation method, the metal film formed on the surface of the cracking template is Ag, Ni, Cu, Au or an alloy among the Ag, Ni, Cu and Au.
In the preparation method, the separation of the schizophyllum commune blocks and the substrate is to wash or ultrasonically clean the substrate by using deionized water or other solvents, filter and separate water after standing, and obtain the schizophyllum commune blocks with the metal films attached to the surfaces.
In the preparation method, the metal film layer is separated from the cracking block, namely, the cracking block attached with the metal film is washed for many times by deionized water or ethanol and dried to obtain the micron-sized ultrathin metal sheet.
The principle of the invention is as follows: coating the cracking liquid on a substrate to form a layer of colloid film, then heating, drying and curing to form micron-sized cracking blocks by self-cracking, reserving gaps among different cracking blocks, and plating a layer of metal film by vacuum plating. Because the cracking material loses water and is dried in the heat treatment process, stress is released to form the cracking blocks, the sizes of the cracking blocks can be adjusted by different supercooling degrees, different cracking liquid concentrations and types and different cracking times; the thickness of the metal film is adjusted by adjusting related parameters of vacuum plating, and the thickness of the metal film is adjusted by controlling the sputtering power and sputtering time of magnetron sputtering during magnetron sputtering. The metal film on the surface of the tortoise split block can be directly washed by deionized water or cleaned by low-power ultrasonic waves to fall off from the surface of the substrate. And further removing the cracking material on the metal film, thereby obtaining the micron-sized ultrathin metal sheet.
Compared with the prior art, the invention has the following beneficial effects:
(1) compared with the traditional mechanical ball milling method, the photoinduction method, the template method, the chemical reduction method and the like, the preparation method for the micron-sized ultrathin metal sheet of the conductive adhesive filler is simple, low in manufacturing cost, high in yield, green and pollution-free, and capable of realizing industrial production;
(2) the micron-sized ultrathin metal sheet prepared by the method has the advantages of good uniformity, overlarge specific surface area, excellent electrical property and no impurity atom, and the size and the thickness dimension of the micron-sized ultrathin metal sheet can be controlled by regulating and controlling different cracking liquids, cracking conditions, deposition power and deposition time.
Drawings
Fig. 1 is a schematic view of a micron-sized ultra-thin metal sheet for a conductive adhesive filler prepared according to the present invention.
FIG. 2 is a process flow diagram of the method for preparing micron-sized ultra-thin metal sheets filled with conductive adhesive according to the present invention.
FIG. 3 is a scanning electron microscope image (magnification 700) of silver powder prepared in example 1 of the present invention.
FIG. 4 is a lateral area size graph (magnification 1100 times) of silver powder prepared in example 1 of the present invention.
FIG. 5 is a thickness diagram (magnification: 10000 times) of silver powder prepared in example 1 of the present invention.
FIG. 6 is an XRD pattern of silver powder prepared in example 1 of the present invention.
Detailed Description
The present invention is further described below in conjunction with specific examples to better understand and implement the technical solutions of the present invention for those skilled in the art.
Example 1
As shown in fig. 2, the cracking material is protein powder, the substrate is selected from flexible PET, and (1) in fig. 2, the cracking liquid is coated; (2) naturally cracking the template; (3) carrying out magnetron sputtering on metallic silver; (4) separating and cleaning the metallic silver microchip.
The method comprises the following specific steps:
(1) application of crack liquid
And adding water into the protein powder, mixing, and stirring to prepare a cracking liquid, wherein the mass ratio of the protein powder to the water is 1: 1. The coiled material PET flexible substrate is pre-cleaned by ultrasound, dried by introducing nitrogen, and loaded on a coating machine for standby. The coater was turned on and the PET coil was sequentially cleaned by atmospheric plasma sputtering and coated with a cracking solution (step 1 in fig. 2). The coil winding speed is set to 1m/s, and the thickness of the applied cracking liquid film is about 20 to 40 μm.
(2) Natural crazing of form
Heating the heating table to 70-80 ℃, controlling the humidity to be 60-80% RH, and controlling the heat preservation time to be 8min so that the coiled material is spontaneously cracked on the heating table, wherein the size of a cracking block is 40-400 mu m (as shown in step 2 in figure 2).
(3) Magnetron sputtering metallic silver
Collecting the coiled material in a coiling mode, putting the coiled material into a reel-to-reel magnetron sputtering system, and vacuumizing to 5 x 10-4Pa, then adjusting the refrigeration system in the vacuum chamber to-2 ℃, setting the roll speed of the roll-to-roll system to 0.5m/s, and setting the tension to 4N. And then carrying out magnetron sputtering on the silver, wherein the sputtering power is 3KW, and the thickness of the metal silver is controlled to be 20-500nm through the time and the power (as shown in step 3 in figure 2). And after sputtering, opening the cavity, and taking out the silver-plated coiled material.
(4) Separating and cleaning micron-sized silver metal sheet
And (3) cleaning the obtained coiled material with deionized water, standing the cleaned water solution, filtering out silver powder, repeatedly cleaning the silver powder with deionized water for multiple times, finally cleaning with absolute ethyl alcohol, filtering out the silver powder (shown as step 4 in figure 2), and heating the silver powder in an oven to 60 ℃ for drying.
The silver powder after drying is shown in FIG. 3, and it can be seen that the silver powder has a plate shape. Fig. 1, 2, 4 and 5 show that the silver powder has a lateral diameter of 30-80 μm and a thickness of about 200nm, and the resulting sample is a micro-scale ultra-thin metal plate. Fig. 6 is an XRD pattern of the silver powder, from which it can be concluded that the obtained micro-scale ultra-thin metal sheet does not contain other impurities.
Example 2
The embodiment provides another preparation method for a micron-sized ultrathin metal sheet filled with a conductive adhesive, wherein a cracking material is methyl oil CA600, a substrate is selected to be flexible PEN, and (1) coating of a cracking liquid is performed; (2) naturally cracking the template; (3) carrying out magnetron sputtering on copper and silver; (4) separating and cleaning micron-sized copper-silver alloy metal sheets, which comprises the following specific steps:
(1) application of crack liquid
First, nail polish CA600 was filled into a beaker as a crack liquid for use. And then ultrasonically heating and cleaning the PEN flexible substrate, introducing nitrogen for drying, cleaning by using plasma after drying, and spreading on a coating machine after cleaning. And installing a coating cutter head, debugging the uniformity of the cutter head by using deionized water, and replacing the cutter head with the cracking liquid of methyl gasoline CA600 after the uniformity is adjusted.
(2) Natural crazing of form
Firstly, heating a heating table to 50-60 ℃, controlling the humidity to be 60-80% RH, controlling the heat preservation time to be 10min, then starting a coating machine, setting the winding speed to be 1m/s, starting coating, wherein the thickness of a coated cracking liquid film is about 10-60 mu m, and collecting the cracking liquid film after heating and drying.
(3) Magnetron sputtering metallic copper silver
Putting the collected PEN coiled material with the cracking liquid film into a roll-to-roll magnetron sputtering system, and vacuumizing to 5 multiplied by 10-4Pa, then adjusting the refrigeration system in the vacuum chamber to-2 ℃, setting the roll speed of the roll-to-roll system to 0.5m/s, and setting the tension to 4N. Then carrying out magnetron sputtering on copper with the sputtering power of 2.5KW, and then carrying out magnetron sputtering on silver with the sputtering power of 2 KW. And after sputtering, heating the vacuum cavity to 20 ℃, opening the cavity, and taking out the plated coiled material.
(4) Separating and cleaning micron-sized copper-silver alloy metal sheet
Washing the coiled material obtained by magnetron sputtering with diluted glacial acetic acid, filtering out silver powder from the washed solution, repeatedly washing the copper-silver alloy powder with the diluted glacial acetic acid for multiple times, finally washing with deionized water and absolute ethyl alcohol for multiple times respectively, filtering out the copper-silver alloy powder, heating in an oven to 60 ℃, drying and collecting. The lateral diameter of the obtained copper-silver alloy powder is 20-60 μm, and the thickness is about 180-300 nm.
Example 3
The embodiment provides a preparation method of a micron-sized ultrathin metal sheet for a conductive adhesive filler, wherein a cracking material is a natural egg white aqueous solution, a substrate is selected from rigid glass, and (1) the cracking solution is coated; (2) naturally cracking the template; (3) carrying out magnetron sputtering on metal copper; (4) separating and cleaning micron-sized copper metal sheets, which comprises the following specific steps:
(1) application of crack liquid
And adding water into the egg white, mixing, stirring to prepare a cracking liquid, wherein the volume ratio of the egg white to the water is 2: 1-3: 1, and filling the cracking liquid into a beaker for later use. And (3) ultrasonically heating and cleaning the rigid glass substrate, introducing nitrogen for drying, cleaning by using plasma after drying, and flatly laying and fixing the rigid glass substrate on an operation table after cleaning.
An aqueous solution of egg white was applied dropwise to one end of the glass and then knife coated with a 40 μm wire bar.
(2) Natural crazing of form
Firstly, heating a heating table to 50-60 ℃, controlling the humidity to be 60-80% RH, controlling the heat preservation time to be 10min, and then placing the glass substrate coated with the cracking liquid on the heating table to naturally crack, wherein the size of a cracking block is 60-400 mu m.
(3) Magnetron sputtering of metallic copper
Putting the glass-based cracking template into a magnetron sputtering system, and vacuumizing the main bin to 3 multiplied by 10-6And Pa, rotating the tray, applying a voltage of 6V, adjusting the tray to a proper height, then carrying out magnetron sputtering on copper, controlling the sputtering power to be 200W, controlling the argon flow to be 2.0mtorr, controlling the sputtering time to be 7min, and taking out a sample after the copper is plated.
(4) Separating and cleaning micron-sized copper metal sheet
Washing a sample obtained through magnetron sputtering by using deionized water, filtering out a copper sheet from a washed solution, then washing for multiple times by using the deionized water and absolute ethyl alcohol respectively, filtering out the copper sheet, and putting the copper sheet into an oven to be heated to 60 ℃ for drying and collection. The lateral diameter of the obtained copper powder is 60-400 μm, and the thickness is about 240 nm.
The method for preparing the micron-sized ultrathin metal sheet is not only suitable for preparing the micron-sized metal sheet of the metal silver, the metal copper and the metal copper-silver alloy, but also can be used for preparing the micron-sized ultrathin metal sheet of the metal silver, the metal copper and the metal copper-silver alloy by the method as long as the metal can be deposited by a vacuum coating process, and the metal comprises Ni, Ti, Zn, Cr, Mg, Nb, Sn, Al, In, Fe, ZrAl, TiAl, Zr, AlSi, Si, Ta, Ge, Co, Au, Gd, La, Y, Ce, NiCr, Hf, Mo, FeNi, W and stainless steel targets or alloys and oxides of the metals.
The above embodiments illustrate various embodiments of the present invention in detail, but the embodiments of the present invention are not limited thereto, and those skilled in the art can achieve the objectives of the present invention based on the disclosure of the present invention, and any modifications and variations based on the concept of the present invention fall within the scope of the present invention, which is defined by the claims.
Claims (10)
1. A preparation method of micron-sized ultrathin metal sheets for conductive adhesive fillers comprises the following steps:
(1) coating the cracking liquid on a substrate;
(2) controlling the temperature, the humidity and the time to enable the cracking liquid to naturally crack to form a cracking template of micron-sized cracking blocks;
(3) depositing a metal film on the cracking template in a vacuum coating mode;
(4) and separating the cracking block from the substrate, and then separating the metal film from the cracking block to obtain the micron-sized ultrathin metal sheet.
2. The method for preparing micron-sized ultrathin metal sheets for conductive adhesive fillers according to claim 1, wherein the cracking liquid comprises protein sol, polymer coating and oxide sol.
3. The method for preparing micron-sized ultrathin metal sheet as conductive adhesive filler according to claim 2, wherein the protein sol is natural egg white or artificial protein powder colloid, the high polymer coating is methyl oil CA600, and the oxide sol is titanium dioxide sol.
4. The method for preparing micron-sized ultrathin metal sheet for conductive adhesive filler according to any one of claims 1 to 3, characterized in that the cracking temperature of the cracking liquid is controlled to be 40-80 ℃, the humidity is controlled to be 60-80% RH, and the time is controlled to be 8-12 min.
5. The method for preparing micron-sized ultrathin metal sheet used as conductive adhesive filler according to claim 4, wherein the diameter of the micron-sized fissures is 20-400 microns.
6. The method for preparing micron-sized ultrathin metal sheet for conductive adhesive filler according to claim 5, characterized in that the substrate is pretreated before the cracking liquid is coated on the surface of the substrate: the substrate is firstly placed into deionized water for ultrasonic heating and cleaning, then nitrogen is introduced for drying, and then plasma cleaning is carried out after drying.
7. The method for preparing micron-sized ultra-thin metal sheets for conductive adhesive fillers according to claim 1 or 6, wherein the substrate is glass, polyethylene terephthalate (PET) or polyethylene naphthalate (PEN).
8. The method for preparing micron-sized ultra-thin metal sheet for conductive adhesive filler according to claim 7, wherein the vacuum coating method comprises thermal evaporation, chemical vapor deposition, ion sputtering, magnetron sputtering; the thickness of the metal film is 20-500 nm.
9. The method for preparing micron-sized ultrathin metal sheet for conductive adhesive filler according to claim 8, wherein the metal film formed on the surface of the cracking template is Ag, Ni, Cu, Au or alloy thereof.
10. The method for preparing micron-sized ultrathin metal sheet for conductive adhesive filler according to claim 1, characterized in that the separation of the schizophyllum commune from the substrate is carried out by washing the substrate with deionized water or other solvents or ultrasonic cleaning, standing, and then filtering and separating water to obtain the schizophyllum commune with the metal film attached to the surface; the metal film layer is separated from the cracking blocks, namely, the cracking blocks attached with the metal film are washed for multiple times by deionized water or ethanol and dried to obtain the micron-sized ultrathin metal sheet.
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Cited By (2)
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| CN113201709A (en) * | 2021-04-27 | 2021-08-03 | 青沃精密仪器(苏州)有限公司 | Preparation method of micron-sized ultrathin metal sheet for conductive adhesive |
| CN114457305A (en) * | 2021-11-10 | 2022-05-10 | 安徽正合雅聚新材料科技有限公司 | Nano silver film preparation process and nano silver film manufacturing equipment |
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