CN103617830B - A kind of preparation method of conductive metal film - Google Patents
A kind of preparation method of conductive metal film Download PDFInfo
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- CN103617830B CN103617830B CN201310513245.XA CN201310513245A CN103617830B CN 103617830 B CN103617830 B CN 103617830B CN 201310513245 A CN201310513245 A CN 201310513245A CN 103617830 B CN103617830 B CN 103617830B
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Abstract
The present invention relates to field of electronic materials, the preparation method disclosing a kind of metallic film, especially the preparation method of metallic transparent conductive film, it is possible to increase the adhesiveness between conductive metal film and substrate, and it is maintained with the high electric conductivity of metallic film and long-term reliability.The preparation method of this conductive metal film includes: S1, alginic acid and the N kind material containing basic group dissolved in the first solvent, and described N is the integer more than or equal to 1；S2, mix homogeneously with the N kind material containing basic group with the described alginic acid of dissolving by the dispersion liquid containing metal nanometer line or containing the dispersion liquid of granule, obtain the first solution；S3, by described first solution film forming in substrate, dry, obtain conductive metal film.
Description
Technical field
The present invention relates to field of electronic materials, particularly to the preparation method of a kind of conductive metal film.
Background technology
Nano silver wire transparent conductive film, has good electric conductivity, and has high transmission rate in visible-range, be widely used in the fields such as flat pannel display, thin-film solar cells, sensor, touch screen and extending electronics.
But, nano silver wire transparent conductive film is poor with the adhesiveness of substrate, and when being uncovered by the adhesive tape sticking to nano silver wire conductive film surface, nano silver wire conductive film almost all can come off from substrate.At present, one of the method for adhesion issues between nano silver wire conductive film and substrate that solves is addition polymer adhesive in the dispersion liquid of nano silver wire, polymer adhesive film forming together with nano silver wire, after drying out the solvent, nano silver wire and substrate are tightly sticked together by polymer adhesive.Another kind of method is that the nano silver wire surface after film forming covers one layer of polymeric, and the method also can strengthen the adhesion between nano silver wire conductive film and substrate.But, due to nano silver wire one layer of stabilizer polyvinylpyrrolidone of parcel peripheral itself, after in first method, polymer adhesive is attached to nano silver wire periphery, between silver wire, contact resistance will sharply increase, in second method, the polymer itself owing to covering silver surface insulate, and also seriously reduces the electric conductivity of nano silver wire conductive film；Secondly, to realize large-scale commercial application, product keeps long-term reliability will be very necessary and important, therefore the physics of the polymer adhesive added or the polymer of covering and chemical property are had to the requirement of harshness: certain film property, inviscid after drying, it is not easy to the moisture absorption, solvent can be resisted, steady in a long-term in atmosphere exist, and Conductivity is little etc..But because of the needs of film-forming process, nano silver wire is generally dispersed in lower boiling ethanol or isopropanol, the polymer adhesive therefore added allows for being dispersed or dissolved in these solvents.But it is possible to the ability as its opposing solvent of the material in ethanol or these polar solvents of isopropanol and wet environment that is dissolved in is often poor, namely the reliability of this polymer adhesive is poor.Therefore, the reliability of the nano silver wire electrically conducting transparent laminated film that it is prepared is also poor.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of conductive metal film, it is possible to increase the adhesiveness between conductive metal film and substrate, and it is maintained with higher electric conductivity and long-term reliability.
For solving above-mentioned technical problem, the preparation method that embodiments of the present invention provide a kind of conductive metal film, comprise the following steps:
S1, alginic acid and the N kind material containing basic group being dissolved in the first solvent, described N is the integer more than or equal to 1；
S2, mix homogeneously with the N kind material containing basic group with the described alginic acid of dissolving by the dispersion liquid containing metal nanometer line or containing the dispersion liquid of granule, obtain the first solution；
S3, by described first solution film forming in substrate, dry, obtain conductive metal film.
Embodiment of the present invention is in terms of existing technologies, utilize alginic acid and the material containing basic group to improve conductive metal film and substrate adhesion, wherein the material containing basic group can improve the dissolubility of alginic acid, make alginic acid can directly apply in the dispersion liquid of metal nanometer line or granule so that the technique of water-laid film is possibly realized.Meanwhile, along with after film forming, the volatilization of alkaline matter removes, alginic acid dissolubility sharply declines so that it is possesses the ability of outstanding opposing solvent and humidity after film forming, improves the long-term reliability of metal nanometer line conductive film.It addition, utilize its electric conductivity of transparent conductive film not dramatic drop-off along with adhering raising that this method obtains.
It addition, when the described N kind material containing basic group includes Dopaminergics material, after described S1, before described S2, described method is further comprising the steps of:
S4, in described first solvent being dissolved with described alginic acid and the described N kind material containing basic group, add the poor solvent of alginic acid described in M kind, described M is the integer more than or equal to 1, and the addition of the poor solvent of described alginic acid is more than the content of water in described first solution；
S5, the complex that described alginic acid and described Dopaminergics material are formed by the poor solvent of described alginic acid precipitate out, and the described alginic acid of described dissolving and the N kind material containing basic group are the complex that described alginic acid is formed with described Dopaminergics material.
By adding the poor solvent of alginic acid, it is possible to precipitate out the complex that alginic acid is formed with Dopaminergics material.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the preparation method of the conductive metal film of first embodiment of the invention；
Fig. 2 is the schematic flow sheet of the preparation method of the conductive metal film of second embodiment of the invention；
Fig. 3 is structure of matter phenogram in technique；
Fig. 4 is the nano silver wire transparent conductive film under scanning electron microscope；
Fig. 5 is the hot and humid reliability test result schematic diagram of nano silver wire transparent conductive film.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, the embodiments of the present invention are explained in detail.But, it will be understood by those skilled in the art that in each embodiment of the present invention, propose many ins and outs in order to make reader be more fully understood that the application.But, even without these ins and outs with based on the many variations of following embodiment and amendment, it is also possible to realize the application each claim technical scheme required for protection.
The preparation method that first embodiment of the invention provides a kind of conductive metal film, as it is shown in figure 1, comprise the following steps:
Step 101, alginic acid and one or more materials containing basic group are dissolved in the first solvent.
Alginic acid is by the polysaccharide of monosaccharide aldehydic acid linear polymerization, and monomer is β-D-manna aldehydic acid (M) and α-L-guluronic acid (G).M and G unit becomes block copolymer with the compound mode of M-M, G-G or M-G by Isosorbide-5-Nitrae glycosidic bond is connected.The empirical formula of alginic acid is (C6H8O6)n, molecular weight ranges is from 1 ten thousand to 60 ten thousand not etc..The finished product of alginic acid is pale yellow powder, almost tasteless, insoluble in water, methanol, ethanol, acetone, chloroform, has good film property, inviscid after drying.The bad dissolubility of alginic acid makes it possess the ability of outstanding opposing solvent and humidity after film forming, be conducive to improving the long-term reliability of product, simultaneously because of in structure containing substantial amounts of carboxyl, when using as adhesive, it is likely less on the impact of metallic film electric conductivity.
In example, the described material containing basic group can be ammonia.Containing a certain amount of water and ethanol in first solvent.At room temperature by alginic acid, ammonia, water and ethanol mix homogeneously, obtain the clear solution of alginic acid.
Step 102, the utilization dispersion liquid containing metal nanometer line or the dispersion liquid containing granule are mixed homogeneously with the alginic acid of dissolving, obtain the first solution.
Example, what step 101 obtained is the clear solution of alginic acid, this solution is added the dispersion liquid containing metal nanometer line, obtains the first solution.In the first solution, the mass ratio of the clear solution of metal nanometer line or granule and alginic acid is the number more than or equal to 1 and less than or equal to 100, it is preferable that 5～20, and N is the integer more than or equal to 1.
Step 103, by the first solution film forming in substrate, dry, obtain conductive metal film.
Specifically, it is possible to first by the mode of spraying by the first solution film forming in polyethylene terephthalate (PET) substrate, prepared thin film is carried out performance characterization.Further, it is also possible to utilize the mode of blade coating, printing or spin coating to the first solution film forming in substrate.Wherein substrate is not limited, it is possible to for the substrate of rigidity or flexible material, it is possible to for the substrate of organic or inorganic material, it is also possible to for transparent or opaque material substrate.
It addition, utilize spraying, blade coating, the mode of printing or spin coating is by the first solution in substrate during film forming, and technological temperature controls below 100 degree.
Conductive metal film includes nano silver wire transparent conductive film.
Embodiment of the present invention is in terms of existing technologies, utilize alginic acid and the material containing basic group to improve conductive metal film and substrate adhesion, wherein the material containing basic group can improve the dissolubility of alginic acid, make alginic acid can directly apply in the dispersion liquid of metal nanometer line or granule so that the technique of water-laid film is possibly realized.Meanwhile, along with after film forming, the volatilization of alkaline matter removes, alginic acid dissolubility sharply declines so that it is possesses the ability of outstanding opposing solvent and humidity after film forming, improves the long-term reliability of metal nanometer line conductive film.It addition, utilize its electric conductivity of transparent conductive film not dramatic drop-off along with adhering raising that this method obtains.
The preparation method that second embodiment of the present invention relates to a kind of conductive metal film.Second embodiment has done further improvement on the first embodiment basis, as shown in Figure 2, mainly the improvement is that: when the described N kind material containing basic group includes Dopaminergics material, after step 101 performs, before step 102 execution, first carry out following steps:
Step 104, adding the poor solvent of one or more alginic acid in the first solvent being dissolved with alginic acid and one or more materials containing basic group, the addition of the poor solvent of alginic acid is more than the content of water in the first solution.
Step 105, the complex that alginic acid and Dopaminergics material are formed by the poor solvent of alginic acid precipitate out.
Example, the first solvent can be ammonia.Step 101, particularly as follows: at room temperature weigh alginic acid and Dopaminergics material for 8:1 in mass ratio, adds ammonia, makes alginic acid and Dopaminergics material all dissolve.It should be noted that polyreaction can occur Dopaminergics material in ammonia, generating poly-Dopaminergics material, all can there is complex reaction in alginic acid and Dopaminergics material and poly-Dopaminergics material, generate the complex of alginic acid and poly-Dopaminergics material.
After execution of step 101, then perform step 104 and step 105.The solution that the complex of alginic acid and poly-Dopaminergics material and ammonia are mainly formed by step 104 and step 105 is easily separated purification, extracts the complex of alginic acid and poly-Dopaminergics material.Present embodiment adopts the method for co-precipitation to extract the complex that in the first solution, alginic acid is formed with poly-Dopaminergics material.Concrete, step 104 includes: add the poor solvent of one or more alginic acid in the complex of alginic acid and poly-Dopaminergics material and the solution of ammonia formation, the addition of the poor solvent of alginic acid is more than the content of water in the first solution, the poor solvent of alginic acid can be organic solvent, such as ethanol, isopropanol, acetone.Example, the poor solvent of alginic acid can be ethanol.Then performing step 105, step 105 includes: after a few hours, when the complex of alginic acid with Dopaminergics material is precipitated out by ethanol, adopts the complex of centrifugal separation separation alginic acid and poly-Dopaminergics material.In order to separate thoroughly as far as possible, it is possible to be easily separated in triplicate.It should be noted that when separating, it is possible to artificially in the first solution, leave a small amount of ammonia.
By adding the poor solvent of alginic acid, it is possible to precipitate out the complex that alginic acid is formed with Dopaminergics material.
Then step 102 is performed.Step 102 specifically includes: is disperseed by the complex of the dispersion liquid containing metal nanometer line or the dispersion liquid containing granule and alginic acid and poly-Dopaminergics material, obtains the first solution.When in dispersion liquid not moisture time, firstly the need of adding a kind of solvent, the complex of alginic acid and poly-Dopaminergics material is dissolved, this solvent is the solvent containing water, then recycling metal nanometer line or particle dispersion mix with the complex solution of alginic acid and Dopaminergics material, obtain the second solution.The preferred low boiling point organic solvent of solvent added in step 102, the consideration of the technique that preferred low boiling point solvent is mainly based upon in step 103, because last film forming procedure is to be removed by solvent, and high boiling solvent seasoning time is long, the quality of film forming can be affected because the aggravation of solvent blockage effect when film forming.Example, when the second solvent is ethanol, step 102 specifically includes: the alginic acid that first can step 105 be obtained dissolves with the complex water of poly-Dopaminergics material and the mixed solvent of ethanol, obtains complex solvent soln, and wherein water is about 1:1 with the mass ratio of ethanol；Then being joined by complex solution in the dispersion liquid of metal nanometer line, obtain the first solution, wherein metal nanometer line can be 8 with the mass ratio of alginic acid.When in dispersion liquid containing water, then need not add the solvent complex to alginic acid and poly-Dopaminergics material and dissolve, it is possible to directly complex is dissolved in the dispersion liquid of metal nanometer line, obtain the first solution.
It should be noted that when step 105 separates, the ammonia of residual makes the second solution be alkalescence.Although final complex dissolubility is strengthened, but needs for certain alkalescence and ensure its dissolubility in a solvent.
Finally perform step 103.The execution method of step 103 is identical with the first embodiment, and therefore not to repeat here for the present invention.
The following is some experimental analysis data that the present invention conductive metal film to preparing does, wherein, Fig. 3 is to structure of matter phenogram in technique.Wherein, abscissa represents wave number, unit be centimetre point one, vertical coordinate represents light transmittance, and 301 is the performance characterization of alginic acid, and 302 is the performance characterization of poly-Dopaminergics material, and 303 is the performance characterization of alginic acid and poly-Dopaminergics material.Fig. 4 is the nano silver wire transparent conductive film under scanning electron microscope, wherein figure a is fine silver nano wire transparent conductive film, as seen from the figure, fine silver nano wire is piled up loose, and fine silver nano wire does not bend, essentially straight, the nano silver wire transparent conductive film that figure b is is binding agent with alginic acid, nano silver wire is piled up closely, and line is at lap-joint's visible deformation, and such conductive effect can be better.Fig. 5 is the hot and humid reliability test result of nano silver wire transparent conductive film, and condition is 85 DEG C (degree Celsius)/85%RH(relative humidity).Wherein, abscissa represents the reliability test time, and unit is sky, and vertical coordinate represents sheet resistance, and unit is ohm often side.As seen from Figure 5, under hot and humid condition, nano silver wire transparent conductive film sheet resistance is without big change.Being experiments show that by every, prepared metal nanometer line conductive film, sheet resistance during light transmittance 89% is 16.3 Ω/ (ohm is side often).Carrying out adhesive tape adhesion test with the sample that sheet resistance value is 34.2 Ω/, its value is only increased to 42.4 Ω/, and after 100 adhesive tape adhesion tests, sheet resistance is still less than 100 Ω/, and the metal nanometer line that adhesion is purer significantly improves；Hot and humid experiments show that, the transparent conductive film of preparation possesses stable long-term reliability；Being placed in acetone or water a few hours, prepared conductive film still has adhesiveness, possesses good solvent resistant performance.
Embodiment of the present invention is in terms of existing technologies, utilize alginic acid and the material containing basic group to improve conductive metal film and substrate adhesion, wherein the material containing basic group can improve the dissolubility of alginic acid, make alginic acid can directly apply in the dispersion liquid of metal nanometer line or granule so that the technique of water-laid film is possibly realized.Meanwhile, along with after film forming, the volatilization of alkaline matter removes, alginic acid dissolubility sharply declines so that it is possesses the ability of outstanding opposing solvent and humidity after film forming, improves the long-term reliability of metal nanometer line conductive film.It addition, utilize its electric conductivity of the transparent conductive film arrived not dramatic drop-off along with adhering raising of this method.
It will be understood by those skilled in the art that the respective embodiments described above are to realize specific embodiments of the invention, and in actual applications, it is possible in the form and details it is done various change, without departing from the spirit and scope of the present invention.
Claims (10)
1. the preparation method of a conductive metal film, it is characterised in that comprise the following steps:
S1, alginic acid and the N kind material containing basic group being dissolved in the first solvent, described N is the integer more than or equal to 1；
S2, mix homogeneously with the N kind material containing basic group with the described alginic acid of dissolving by the dispersion liquid containing metal nanometer line or containing the dispersion liquid of granule, obtain the first solution；
S3, by described first solution film forming in substrate, dry, obtain conductive metal film.
2. the preparation method of conductive metal film according to claim 1, it is characterised in that when the described N kind material containing basic group includes Dopaminergics material, after described S1, before described S2, described method is further comprising the steps of:
S4, in described first solvent being dissolved with described alginic acid and the described N kind material containing basic group, add the poor solvent of alginic acid described in M kind, described M is the integer more than or equal to 1, and the addition of the poor solvent of described alginic acid is more than the content of water in described first solution；
S5, the complex that described alginic acid and described Dopaminergics material are formed by the poor solvent of described alginic acid precipitate out, and the described alginic acid of described dissolving and the N kind material containing basic group are the complex that described alginic acid is formed with described Dopaminergics material.
3. the preparation method of conductive metal film according to claim 1, it is characterised in that in described S1, the described material containing basic group contains amido, containing water or highly polar material in described first solvent.
4. the preparation method of conductive metal film according to claim 3, it is characterised in that the described material containing basic group is ammonia or Dopaminergics material.
5. the preparation method of conductive metal film according to claim 2, it is characterised in that the poor solvent of described alginic acid is organic solvent.
6. the preparation method of conductive metal film according to claim 5, it is characterised in that described organic solvent is: ethanol, isopropanol, acetone.
7. the preparation method of conductive metal film according to claim 1, it is characterized in that, in described S2, described metal nanometer line or described granule are the number more than or equal to 1 and less than or equal to 100 with the described alginic acid of described dissolving and the mass ratio of the N kind material containing basic group.
8. the preparation method of conductive metal film according to claim 1, it is characterised in that in described S3, utilizes the mode of spraying, blade coating, printing or spin coating by described first solution film forming in substrate.
9. the preparation method of conductive metal film according to claim 8, it is characterised in that in described S3, utilizes spraying, blade coating, and the mode of printing or spin coating is by described first solution in substrate during film forming, and technological temperature controls below 100 degree.
10. the preparation method of conductive metal film according to claim 1, it is characterised in that in described S3, described substrate is transparent, translucent or opaque flexibility or rigidity material.
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| CN104804206B (en) * | 2015-04-28 | 2017-11-10 | 中科院广州化学有限公司南雄材料生产基地 | A kind of method that transparent conductive film is prepared based on nano-silver thread modification |
| CN104934094B (en) * | 2015-05-27 | 2018-10-16 | 复旦大学 | A kind of metal nanometer line compound transparent electricity conductive film, preparation method and application |
| CN105602201B (en) * | 2016-03-21 | 2018-01-12 | 西南科技大学 | A kind of preparation method of high-strength conductive high molecule nano composite material |
| CN107154283B (en) * | 2017-04-11 | 2020-10-16 | 复旦大学 | Electromigration-resistant silver nanowire composite film and preparation method thereof |
| US10664077B2 (en) | 2017-12-06 | 2020-05-26 | Wuhan China Optoelectronics Semiconductor Display Technology Co., Ltd. | AgNW transparent conductive film and manufacturing method thereof and touch panel |
| CN107808708A (en) * | 2017-12-06 | 2018-03-16 | 武汉华星光电半导体显示技术有限公司 | Nano Silver nesa coating and preparation method thereof and touch-screen |
| CN108892811B (en) * | 2018-06-21 | 2020-02-07 | 中国科学技术大学 | Inorganic material-organic polymer composite material and preparation method thereof |
| CN109438139A (en) * | 2018-11-09 | 2019-03-08 | 中国农业科学院农业资源与农业区划研究所 | A kind of preparation method with the alginic acid synergistic carrier for slowing down urea conversion |
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