CN109694492A - A kind of Cr layer that can improve PI flexible substrate Yu Au electrode adhesion performance - Google Patents

A kind of Cr layer that can improve PI flexible substrate Yu Au electrode adhesion performance Download PDF

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CN109694492A
CN109694492A CN201910135902.9A CN201910135902A CN109694492A CN 109694492 A CN109694492 A CN 109694492A CN 201910135902 A CN201910135902 A CN 201910135902A CN 109694492 A CN109694492 A CN 109694492A
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Abstract

The present invention relates to flexible gas sensor production technical fields, and a kind of Cr layer that can improve PI flexible substrate Yu Au electrode adhesion performance is disclosed, the described Cr layers raw material including following parts by weight proportion: 60-75g nanometers of Cr powder, 5-8g glass powder, 2-5mL aqueous epoxy resins, 2-4g polyvinyl alcohol, 1-3g rosin, 1-2mL ethyl acrylate, 5-10mL dehydrated alcohol, 2.8-3.2g salicylic acid, 1-1.6gK2S2O8, 3-4g vinyltrimethoxysilane.The present invention solves the gas sensor based on PI flexible substrate, in the long-term use, the technical issues of cementation power between PI flexible substrate and Au electrode weakens.

Description

A kind of Cr layer that can improve PI flexible substrate Yu Au electrode adhesion performance
Technical field
The present invention relates to flexible gas sensor production technical fields, specially a kind of to improve PI flexible substrate and Au electricity The Cr layer of pole adhesive property.
Background technique
Based on the sensor of flexible substrate since its is light, at low cost, flexible flexible, can the technologies such as large-area manufacturing it is excellent It puts and is concerned.As depicted in figs. 1 and 2, the gas sensor based on PI flexible substrate includes PI flexible substrate 1, first will be clear The PI flexible substrate 1 of wash clean is handled by photoetching, development and bottoming glue, then uses electron beam on 1 surface of PI flexible substrate Method of evaporating first evaporates one layer of Cr as adhesion layer, and re-evaporation layer of Au obtains Cr adhesion layer 2 and Au is pitched by lift-off processing Refer to electrode layer 3, finally deposits one layer of gas sensitization film 4 on 3 surface of Au interdigital electrode layer, that is, be prepared based on PI flexible substrate Gas sensor；Wherein, PI is polyimides.
In the manufacturing process of above-mentioned flexible gas sensor, had additional between PI flexible substrate 1 and Au interdigital electrode layer 3 One layer of Cr adhesion layer 2, Cr adhesion layer 2 primarily serve the skill of adhesive property between enhancing PI flexible substrate 1 and Au interdigital electrode layer 3 Art purpose.
But, due to the interface layer active force between metal Cr and PI flexible substrate 1 and Au interdigital electrode layer 3 compared with It is weak, so, in the long-term use, with PI flexible substrate 1 and Au interdigital electrode layer 3 interface point can occur for Cr adhesion layer 2 From phenomenon, weakens the cementation power between PI flexible substrate 1 and Au interdigital electrode layer 3, cause in flexible gas sensor Portion's structure changes, and finally influences whether the detection performance of flexible gas sensor.
The present invention provides a kind of Cr layer that can improve PI flexible substrate Yu Au electrode adhesion performance, it is intended to solve soft based on PI The gas sensor of property substrate, in the long-term use, the cementation power between PI flexible substrate and Au electrode subtracts Weak technical problem.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, PI flexible substrate and Au electrode adhesion performance can be improved the present invention provides a kind of Cr layers, solves the gas sensor based on PI flexible substrate, in the long-term use, between PI flexible substrate and Au electrode Cementation power the technical issues of weakening.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
A kind of Cr layer that can improve PI flexible substrate Yu Au electrode adhesion performance, described Cr layers includes that following parts by weight are matched The raw material of ratio: 60-75g nanometers of Cr powder, 5-8g glass powder, 2-5mL aqueous epoxy resins, 2-4g polyvinyl alcohol, 1-3g rosin, 1- 2mL ethyl acrylate, 5-10mL dehydrated alcohol, 2.8-3.2g salicylic acid, 1-1.6gK2S2O8, 3-4g vinyl trimethoxy silicon Alkane.
Preferably, average grain diameter≤10um of the Cr powder.
Preferably, the glass powder by 5g average grain diameter≤3um PbO, 1g average grain diameter≤3um SiO2, 1g it is average Partial size≤3um TiO2Composition.
Preferably, Cr layers of the preparation method the following steps are included:
S1. 60-75g nanometers of Cr powder are taken, it is spare；
S2. it is configured to glass powder；
S3. with 2-5mL aqueous epoxy resins, 2-4g polyvinyl alcohol, 1-3g rosin, 1-2mL ethyl acrylate, 5-10mL without Water-ethanol is raw material, and adhesion promoting component is prepared；
S4. the Cr powder in step S1, the glass powder in step S2, the adhesion promoting component in step S3 are placed in ball grinder together Cr slurry is prepared in middle ball milling；
S5. first the Cr slurry in step S4 is coated on PI flexible substrate surface using method for printing screen, is then deposited Layer of Au interdigital electrode layer, is placed in vacuum oven, is dried in vacuo 3h at 68 DEG C, is prepared Cr layers.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
The present invention mainly prepares the Cr with excellent adhesive property by raw material of Cr powder, glass powder and organic tackifier Layer；
After tested, the peel strength between Cr of the invention layer and PI flexible substrate is 50.6-61.3N/cm, with comparative example In Cr layer compared with the peel strength 29.5-34.9N/cm between PI flexible substrate, achieve significantly improve Cr layers it is soft with PI The technical effect of cementation power between property substrate；
Peel strength between Cr prepared by the present invention layers and Au interdigital electrode layer is 38.5-41.8N/cm, and right Cr layer in ratio achieves compared with the peel strength 15.8-16.1N/cm between Au interdigital electrode layer and significantly improves Cr layers The technical effect of cementation power between Au interdigital electrode layer；
To this technical solution, compared with prior art, achieves and significantly improve Cr layers and PI flexible substrate and Au fork Refer to the technical effect of the mutual interlaminar bonding active force of electrode layer.
Detailed description of the invention
Fig. 1 is the structural schematic diagram one of the gas sensor in the prior art based on PI flexible substrate；
Fig. 2 is the structural schematic diagram two of the gas sensor in the prior art based on PI flexible substrate.
It is indicated in figure: 1-PI flexible substrate, 2-Cr adhesion layer, 3-Au interdigital electrode layer, 4- gas sensitization film.
Specific embodiment
Embodiment one:
Cr layers include following raw material: 65g average grain diameter≤10um Cr powder, 7g glass powder, 5mL aqueous epoxy resins, 2g Polyvinyl alcohol, 3g rosin, 2mL ethyl acrylate, 10mL dehydrated alcohol, 3.2g salicylic acid, 1.6gK2S2O8, 3.5g vinyl three Methoxy silane；
Wherein, glass powder by 5g average grain diameter≤3um PbO, 1g average grain diameter≤3um SiO2, 1g average grain diameter≤ The TiO of 3um2Composition；
Above-mentioned Cr layers of preparation method the following steps are included:
S1. 65g average grain diameter≤10um Cr powder is taken, it is spare；
S2. the SiO of 5g average grain diameter≤3um PbO, 1g average grain diameter≤3um are taken2, 1g average grain diameter≤3um TiO2 It is configured to glass powder；
S3. in the deionized water for taking 5mL aqueous epoxy resins to be dissolved in 15mL together with 2g polyvinyl alcohol, thickening group is prepared Divide A；
S4. it takes 3g rosin to be dissolved in 10mL dehydrated alcohol together with 2mL ethyl acrylate, adhesion promoting component B is prepared；
S5. by the Cr powder in step S1, the glass powder in step S2, the adhesion promoting component A in step S3, the increasing in step S4 Viscous component B and 3.2g salicylic acid, 1.6gK2S2O8, 3.5g vinyltrimethoxysilane be placed in ball grinder together, using diameter The zirconium pearl of 3mm, ratio of grinding media to material 2:1, in N2Under protection, Cr slurry is prepared in ball milling 2.5h；
S6. first the Cr slurry in step S5 is coated on 1 surface of PI flexible substrate using method for printing screen, is then deposited Layer of Au interdigital electrode layer 3, is placed in vacuum oven, is dried in vacuo 3h at 68 DEG C, is prepared Cr layers.
Embodiment two:
Cr layers include following raw material: 65g average grain diameter≤10um Cr powder, 5g glass powder, 4mL aqueous epoxy resins, 3g Polyvinyl alcohol, 2g rosin, 1mL ethyl acrylate, 5mL dehydrated alcohol, 3g salicylic acid, 1.2gK2S2O8, 3g vinyl trimethoxy Silane；
Wherein, glass powder by 3g average grain diameter≤3um PbO, 1g average grain diameter≤3um SiO2, 1g average grain diameter≤ The TiO of 3um2Composition；
Above-mentioned Cr layers of preparation method the following steps are included:
S1. 65g average grain diameter≤10um Cr powder is taken, it is spare；
S2. the SiO of 3g average grain diameter≤3um PbO, 1g average grain diameter≤3um are taken2, 1g average grain diameter≤3um TiO2 It is configured to glass powder；
S3. in the deionized water for taking 4mL aqueous epoxy resins to be dissolved in 15mL together with 3g polyvinyl alcohol, thickening group is prepared Divide A；
S4. it takes 2g rosin to be dissolved in 5mL dehydrated alcohol together with 1mL ethyl acrylate, adhesion promoting component B is prepared；
S5. by the Cr powder in step S1, the glass powder in step S2, the adhesion promoting component A in step S3, the increasing in step S4 Viscous component B and 3g salicylic acid, 1.2gK2S2O8, 3g vinyltrimethoxysilane be placed in ball grinder together, using diameter 3mm Zirconium pearl, ratio of grinding media to material 4:1, in N2Under protection, Cr slurry is prepared in ball milling 3h；
S6. the preparation method of this step is identical as the preparation method of step S6 in embodiment one, is prepared Cr layers.
Embodiment three:
Cr layers include following raw material: 65g average grain diameter≤10um Cr powder, 8g glass powder, 2mL aqueous epoxy resins, 4g Polyvinyl alcohol, 1g rosin, 2mL ethyl acrylate, 8mL dehydrated alcohol, 2.8g salicylic acid, 1gK2S2O8, 4g vinyl trimethoxy Silane；
Wherein, glass powder by 6g average grain diameter≤3um PbO, 1g average grain diameter≤3um SiO2, 1g average grain diameter≤ The TiO of 3um2Composition；
Above-mentioned Cr layers of preparation method the following steps are included:
S1. 65g average grain diameter≤10um Cr powder is taken, it is spare；
S2. the SiO of 6g average grain diameter≤3um PbO, 1g average grain diameter≤3um are taken2, 1g average grain diameter≤3um TiO2 It is configured to glass powder；
S3. in the deionized water for taking 2mL aqueous epoxy resins to be dissolved in 15mL together with 4g polyvinyl alcohol, thickening group is prepared Divide A；
S4. it takes 1g rosin to be dissolved in 8mL dehydrated alcohol together with 2mL ethyl acrylate, adhesion promoting component B is prepared；
S5. by the Cr powder in step S1, the glass powder in step S2, the adhesion promoting component A in step S3, the increasing in step S4 Viscous component B and 2.8g salicylic acid, 1gK2S2O8, 4g vinyltrimethoxysilane be placed in ball grinder together, using diameter 3mm Zirconium pearl, ratio of grinding media to material 10:1, in N2Under protection, Cr slurry is prepared in ball milling 2h；
S6. the preparation method of this step is identical as the preparation method of step S6 in embodiment one, is prepared Cr layers.
Example IV:
Cr layers include following raw material: 60g average grain diameter≤10um Cr powder, 7g glass powder, 5mL aqueous epoxy resins, 2g Polyvinyl alcohol, 3g rosin, 2mL ethyl acrylate, 10mL dehydrated alcohol, 3.2g salicylic acid, 1.6gK2S2O8, 3.5g vinyl three Methoxy silane；
Wherein, glass powder by 5g average grain diameter≤3um PbO, 1g average grain diameter≤3um SiO2, 1g average grain diameter≤ The TiO of 3um2Composition；
Above-mentioned Cr layers of preparation method the following steps are included:
S1. 65g average grain diameter≤10um Cr powder is taken, it is spare；
S2. the SiO of 5g average grain diameter≤3um PbO, 1g average grain diameter≤3um are taken2, 1g average grain diameter≤3um TiO2 It is configured to glass powder；
S3. in the deionized water for taking 5mL aqueous epoxy resins to be dissolved in 15mL together with 2g polyvinyl alcohol, thickening group is prepared Divide A；
S4. it takes 3g rosin to be dissolved in 10mL dehydrated alcohol together with 2mL ethyl acrylate, adhesion promoting component B is prepared；
S5. by the Cr powder in step S1, the glass powder in step S2, the adhesion promoting component A in step S3, the increasing in step S4 Viscous component B and 3.2g salicylic acid, 1.6gK2S2O8, 3.5g vinyltrimethoxysilane be placed in ball grinder together, using diameter The zirconium pearl of 3mm, ratio of grinding media to material 2:1, in N2Under protection, Cr slurry is prepared in ball milling 2.5h；
S6. the preparation method of this step is identical as the preparation method of step S6 in embodiment one, is prepared Cr layers.
Embodiment five:
Cr layers include following raw material: 70 average grain diameters≤10um Cr powder, 5g glass powder, 4mL aqueous epoxy resins, 3g are poly- Vinyl alcohol, 2g rosin, 1mL ethyl acrylate, 5mL dehydrated alcohol, 3g salicylic acid, 1.2gK2S2O8, 3g vinyl trimethoxy silicon Alkane；
Wherein, glass powder by 3g average grain diameter≤3um PbO, 1g average grain diameter≤3um SiO2, 1g average grain diameter≤ The TiO of 3um2Composition；
Above-mentioned Cr layers of preparation method the following steps are included:
S1. 65g average grain diameter≤10um Cr powder is taken, it is spare；
S2. the SiO of 3g average grain diameter≤3um PbO, 1g average grain diameter≤3um are taken2, 1g average grain diameter≤3um TiO2 It is configured to glass powder；
S3. in the deionized water for taking 4mL aqueous epoxy resins to be dissolved in 15mL together with 3g polyvinyl alcohol, thickening group is prepared Divide A；
S4. it takes 2g rosin to be dissolved in 5mL dehydrated alcohol together with 1mL ethyl acrylate, adhesion promoting component B is prepared；
S5. by the Cr powder in step S1, the glass powder in step S2, the adhesion promoting component A in step S3, the increasing in step S4 Viscous component B and 3g salicylic acid, 1.2gK2S2O8, 3g vinyltrimethoxysilane be placed in ball grinder together, using diameter 3mm Zirconium pearl, ratio of grinding media to material 4:1, in N2Under protection, Cr slurry is prepared in ball milling 3h；
S6. the preparation method of this step is identical as the preparation method of step S6 in embodiment one, is prepared Cr layers.
Embodiment six:
Cr layers include following raw material: 75g average grain diameter≤10um Cr powder, 8g glass powder, 2mL aqueous epoxy resins, 4g Polyvinyl alcohol, 1g rosin, 2mL ethyl acrylate, 8mL dehydrated alcohol, 2.8g salicylic acid, 1gK2S2O8, 4g vinyl trimethoxy Silane；
Wherein, glass powder by 6g average grain diameter≤3um PbO, 1g average grain diameter≤3um SiO2, 1g average grain diameter≤ The TiO of 3um2Composition；
Above-mentioned Cr layers of preparation method the following steps are included:
S1. 65g average grain diameter≤10um Cr powder is taken, it is spare；
S2. the SiO of 6g average grain diameter≤3um PbO, 1g average grain diameter≤3um are taken2, 1g average grain diameter≤3um TiO2 It is configured to glass powder；
S3. in the deionized water for taking 2mL aqueous epoxy resins to be dissolved in 15mL together with 4g polyvinyl alcohol, thickening group is prepared Divide A；
S4. it takes 1g rosin to be dissolved in 8mL dehydrated alcohol together with 2mL ethyl acrylate, adhesion promoting component B is prepared；
S5. by the Cr powder in step S1, the glass powder in step S2, the adhesion promoting component A in step S3, the increasing in step S4 Viscous component B and 2.8g salicylic acid, 1gK2S2O8, 4g vinyltrimethoxysilane be placed in ball grinder together, using diameter 3mm Zirconium pearl, ratio of grinding media to material 10:1, in N2Under protection, Cr slurry is prepared in ball milling 2h；
S6. the preparation method of this step is identical as the preparation method of step S6 in embodiment one, is prepared Cr layers.
Comparative example one:
Cr layers include following raw material: 60g average grain diameter≤10um Cr powder, 7g glass powder；
Wherein, glass powder by 5g average grain diameter≤3um PbO, 1g average grain diameter≤3um SiO2, 1g average grain diameter≤ The TiO of 3um2Composition；
Above-mentioned Cr layers of preparation method the following steps are included:
S1. 65g average grain diameter≤10um Cr powder is taken, it is spare；
S2. the SiO of 5g average grain diameter≤3um PbO, 1g average grain diameter≤3um are taken2, 1g average grain diameter≤3um TiO2 It is configured to glass powder；
S3. the Cr powder in step S1, the glass powder in step S2 are placed in ball grinder together with 100mL dehydrated alcohol, Using the zirconium pearl of diameter 3mm, ratio of grinding media to material 2:1, in N2Under protection, Cr slurry is prepared in ball milling 2.5h；
S4. the preparation method of this step is identical as the preparation method of step S6 in embodiment one, is prepared Cr layers.
Comparative example two:
Cr layers include following raw material: 70 average grain diameters≤10um Cr powder, 5g glass powder；
Wherein, glass powder by 3g average grain diameter≤3um PbO, 1g average grain diameter≤3um SiO2, 1g average grain diameter≤ The TiO of 3um2Composition；
Above-mentioned Cr layers of preparation method the following steps are included:
S1. 65g average grain diameter≤10um Cr powder is taken, it is spare；
S2. the SiO of 3g average grain diameter≤3um PbO, 1g average grain diameter≤3um are taken2, 1g average grain diameter≤3um TiO2 It is configured to glass powder；
S3. the Cr powder in step S1, the glass powder in step S2 are placed in ball grinder together with 100mL dehydrated alcohol, Using the zirconium pearl of diameter 3mm, ratio of grinding media to material 4:1, in N2Under protection, Cr slurry is prepared in ball milling 3h；
S4. the preparation method of this step is identical as the preparation method of step S6 in embodiment one, is prepared Cr layers.
Performance test:
One, above-described embodiment and the Cr layer in comparative example and the peel strength between PI flexible substrate 1, test result are tested It is shown in Table 1；
Table 1
Two, the peel strength between above-described embodiment and Cr layer and Au interdigital electrode layer 3 in comparative example is tested, test is tied Fruit is shown in Table 2.
Table 2
Sample Peel strength (N/cm) between Cr layers and Au interdigital electrode layer 3
Embodiment one 41.8
Embodiment two 38.8
Embodiment three 39.1
Example IV 40.6
Embodiment five 40.9
Embodiment six 38.5
Comparative example one 15.8
Comparative example two 16.1

Claims (4)

1. a kind of Cr layer that can improve PI flexible substrate Yu Au electrode adhesion performance, it is characterised in that: described Cr layers includes following Parts by weight proportion raw material: 60-75g nanometers of Cr powder, 5-8g glass powder, 2-5mL aqueous epoxy resins, 2-4g polyvinyl alcohol, 1-3g rosin, 1-2mL ethyl acrylate, 5-10mL dehydrated alcohol, 2.8-3.2g salicylic acid, 1-1.6gK2S2O8, 3-4g vinyl Trimethoxy silane.
2. Cr layers according to claim 1, it is characterised in that: average grain diameter≤10um of the Cr powder.
3. Cr layers according to claim 1, it is characterised in that: the glass powder is by 5g average grain diameter≤3um PbO, 1g Average grain diameter≤3um SiO2, 1g average grain diameter≤3um TiO2Composition.
4. Cr layers according to claim 1, it is characterised in that: Cr layers of the preparation method the following steps are included:
S1. 60-75g nanometers of Cr powder are taken, it is spare；
S2. it is configured to glass powder；
S3. with 2-5mL aqueous epoxy resins, 2-4g polyvinyl alcohol, 1-3g rosin, 1-2mL ethyl acrylate, the anhydrous second of 5-10mL Alcohol is raw material, and adhesion promoting component is prepared；
S4. the Cr powder in step S1, the glass powder in step S2, the adhesion promoting component in step S3 are placed in ball in ball grinder together Cr slurry is prepared in mill；
S5. first the Cr slurry in step S4 is coated on PI flexible substrate surface using method for printing screen, then deposits one layer Au interdigital electrode layer, is placed in vacuum oven, is dried in vacuo 3h at 68 DEG C, is prepared Cr layers.
CN201910135902.9A 2019-02-19 2019-02-19 A kind of Cr layer that can improve PI flexible substrate Yu Au electrode adhesion performance Pending CN109694492A (en)

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CN103489501A (en) * 2013-09-13 2014-01-01 厦门大学 Composite conductive thick molybdenum liquid and a method using same to prepare back electrode of copper indium gallium selenium thin-film solar cell
US20160018350A1 (en) * 2007-04-18 2016-01-21 The Research Foundation Of State University Of New York Flexible multi-moduled nanoparticle-structured sensor array on polymer substrate and methods for manufacture
CN105319241A (en) * 2014-07-04 2016-02-10 中国科学院苏州纳米技术与纳米仿生研究所 Flexible gas-sensitive sensor and making method thereof
CN107870487A (en) * 2017-09-19 2018-04-03 合肥惠科金扬科技有限公司 The preparation method of show electrode in a kind of TFT LCD displays

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Publication number Priority date Publication date Assignee Title
US20160018350A1 (en) * 2007-04-18 2016-01-21 The Research Foundation Of State University Of New York Flexible multi-moduled nanoparticle-structured sensor array on polymer substrate and methods for manufacture
CN101792634A (en) * 2010-03-17 2010-08-04 山东天诺光电材料有限公司 Conductive coating and preparation method thereof
CN103033537A (en) * 2012-12-20 2013-04-10 中国科学院微电子研究所 Preparation method of gas sensor sensitive film based on flexible substrate
CN103489501A (en) * 2013-09-13 2014-01-01 厦门大学 Composite conductive thick molybdenum liquid and a method using same to prepare back electrode of copper indium gallium selenium thin-film solar cell
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