CN101186128A - High temperature resistant high photics reflexive conductive film and preparation method thereof - Google Patents
High temperature resistant high photics reflexive conductive film and preparation method thereof Download PDFInfo
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- CN101186128A CN101186128A CNA2007100097191A CN200710009719A CN101186128A CN 101186128 A CN101186128 A CN 101186128A CN A2007100097191 A CNA2007100097191 A CN A2007100097191A CN 200710009719 A CN200710009719 A CN 200710009719A CN 101186128 A CN101186128 A CN 101186128A
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Abstract
The invention relates to a conductive film with high optical reflection, which can be used in the atmosphere environmental with the temperature ranging from room temperature to 550 DEG C, and a preparation method of the conductive film. The conductive film provided by the invention comprises a basic piece, a film damping layer, a film conductive layer, a film protection layer, all of which are arranged layer by layer from bottom to top. The conductive layer is metal silver film with the thickness ranging from 150 nm to 300 nm; the lower surface of the conductive layer is the film damping layer with the thickness ranging from 10 nm to 40nm; the upper surface of the film conductive layer is a film protection layer with the thickness ranging from 5nm to 15nm. The preparation method is that plating technology is adopted; the damping layer, the conductive layer and the protection layer are sequentially plated on the basic piece layer, and finally the heat disposal is carried out by virtue of a muffle. By taking metal and metal oxide as the damping layer and the protection layer of the silver film, the invention can effectively restrict the agglomeration and coacervation of the silver film under high temperature, and implements that the prepared film can remain excellent conductive performance and high optical reflection performance under high temperature.
Description
Technical field
The present invention relates to a kind of conductive film and preparation method thereof, be specifically related to a kind of have high optical reflection, the conductive film that can under the atmospheric environment of room temperature to 550 ℃, use and the preparation method of film thereof.
Background technology
Film has been widely used in national defence, communication, Aeronautics and Astronautics and the industrial and agricultural production.The optics highly reflecting films are generally used for the aluminizer in the parabolic solar receiver in civilian mirror, the solar cooker, are used for the metallic-membrane plating reflector of large-scale astronomical instrument and precision optical instrument, high reflection film of all kinds of laser instruments or the like.Favorable conductive film (as: Al, Cu, Cr, Pt, Au, Ag film etc.) is usually used in semiconductor devices and integrated circuit or the like.Along with progress of science and technology, film characteristics has also been proposed special requirement, as: be used for the light emitting diode of GaN base, need use the film [Applied PhysicsLetters, 83,4990 (2003)] of low resistance and high reflection.
Optical reflectance coating adopts metal film or dielectric multi-layer optical thin film usually, because dielectric film is nonconducting, for the film that requires good conductive and high optical reflection, can only select metallic film.Silver is one of material that resistivity is minimum in all metal materials, and the optical reflection performance of silver is also fine, and therefore, silver-colored film has been widely used in the various opto-electronic devices.But silver-colored film is easy to take place cohesion and caking under hot conditions, makes the structural deterioration of silver-colored film, the conduction failure, and the optical reflection performance descends simultaneously.That is to say that the fine silver film can't be realized high optical reflection and favorable conductive characteristic under hot conditions.
Summary of the invention
At this situation, the objective of the invention is to prepare a kind of thin-film material with high optical reflection and good conductive that can under room temperature to 550 ℃ atmospheric conditions, use, and this preparation methods.
For realizing purpose of the present invention; the thin-film material that the present invention proposes with high optical reflection and good conductive; it is characterized in that: this thin-film material comprises the substrate layer that is made of inorganic oxide, is planted or film cushion that multiple metallic film constitutes, the film conductive layer that is made of argent, the thinfilm protective coating that is made of metal oxide by single, and to down and on successively arrange.The film of preparing has excellent conductive performance and optical reflection performance, can use under room temperature to 550 ℃ atmospheric conditions.
Film conductive layer of the present invention is made of argent, and its thickness is 150 to 300 nanometers.
Film cushion of the present invention is the single or multiple lift film that single kind or multiple metal simple-substance constitute, and its thickness is 10 to 40 nanometers.The metal that uses during single thin film is that copper, aluminium, iron, chromium, nickel, titanium or niobium simple substance constitute separately, or two or more metal mixed constitute in the above-mentioned metal; The metal that uses during plural layers can be the two-layer or plural layers that two or more metals are formed in copper, aluminium, iron, chromium, nickel, titanium or the niobium simple substance.
The thinfilm protective coating that metal oxide of the present invention constitutes is meant zinc oxide, tin oxide, titanium oxide, niobium oxide, silica, aluminium oxide, indium oxide, tin-doped indium oxide or Al-Doped ZnO, and protective layer thickness is 5 to 15 nanometers.
The substrate layer material that is made of inorganic oxide of the present invention is meant aluminium oxide, optical glass, quartz, silicon chip or mica.
Greater than 85%, resistivity is less than 10 at the optical reflectivity of visible-range for this film
-4Ω cm
2, utilize additional cushion layer and protective layer, can suppress cohesion and the caking phenomenon of silver-colored film under the high temperature atmosphere environment effectively, realize that film can use under the high temperature atmosphere environment.
A kind of method for manufacturing thin film with high optical reflection and good conductive of the present invention is characterized in that realizing by following steps:
1, the preparation of film cushion
Adopt known thermal evaporation or sputter or chemical vapor deposition coating technique that the surface that copper, aluminium, iron, chromium, nickel, titanium or niobium simple substance material are deposited on substrate layer is formed single thin film, or form two-layer the surface that two or more metals in copper, aluminium, iron, chromium, nickel, titanium or the niobium simple substance are deposited on basic unit or plural layers.The film buffer layer thickness is controlled between 10 to 40 nanometers.
2, the preparation of film conductive layer
Adopt sputter or known coating technique such as thermal evaporation or chemical vapor deposition plated metal silver film on the film cushion, the purity of used silver is more than 99.99%, and the thickness of silver-colored film is between 150 to 300 nanometers.
3, the preparation of thinfilm protective coating
Adopt known thermal evaporation or sputter or chemical vapor deposition coating technique that zinc oxide, tin oxide, titanium oxide, niobium oxide, silica, aluminium oxide, indium oxide, tin-doped indium oxide or Al-Doped ZnO are deposited on above the film conductive layer (silver), its THICKNESS CONTROL is between 5 to 15 nanometers.
4, the heat treatment of film
The above-mentioned film sample that contains cushion, conductive layer and protective layer is put into Muffle furnace; under atmospheric conditions; heat treatment temperature rises to 550 ℃ gradually; after under 550 ℃ of temperature constant 2 hours; close the power supply of Muffle furnace; temperature drops to room temperature naturally in the stove, takes out then, promptly prepares the film with high optical reflection and good conductive.
With respect to prior art, the bottom at silver-colored film among the present invention adds cushion, adds protective layer on silver-colored film, can overcome the cohesion and the caking of silver-colored film effectively.The film of preparation is after high-temperature heat treatment, under atmospheric environment, can in the temperature range of room temperature to 550 ℃, keep excellent conducting performance and high optical reflection performance, can be applicable to optoelectronic areas such as high brightness LED, solar cell and Aero-Space.
Accompanying drawing and description of drawings
Fig. 1 is the conducting membrane structure longitudinal sectional drawing of the high temperature resistant high optical reflection of the present invention.
Fig. 2 is the conductive film preparation method flow chart of high temperature resistant high optical reflection.
Among Fig. 1, the conductive film of high temperature resistant high optical reflection, the 4th, basic unit; The 3rd, the film cushion above basic unit; The 2nd, the film conductive layer above film cushion 3; The 1st, the thinfilm protective coating above film conductive layer 2.Wherein, film conductive layer 2 is argents, and the thickness of silver-colored film is the main material of realizing conduction and optical reflection between 150 to 300 nanometers.
Among Fig. 2, with the basic unit is base material, by thermal evaporation or sputter or chemical vapor deposition film plating process, elder generation is deposited on metal or metal mixture on the surface of basic unit, prepare the film cushion, its THICKNESS CONTROL is between 10 to 40 nanometers, and the metal of deposition can be copper, aluminium, chromium, nickel, titanium or niobium.Adopt identical film plating process, the silver-colored film of preparation on cushion, the THICKNESS CONTROL of silver-colored film is in 150 to 300 nanometers.And then with identical film plating process, deposit film protective layer above silver-colored film, protective layer material can be zinc oxide, tin oxide, titanium oxide, niobium oxide, silica, and protective layer thickness is controlled at 5 to 15 nanometers.The sample that will prepare is put into Muffle furnace at last, after the heat treatment, obtains the resistant to elevated temperatures high reflection film of conduction again under atmospheric conditions.
The specific embodiment
The present invention is further illustrated in the mode of embodiment below in conjunction with accompanying drawing:
Comprise basic unit 4; The film cushion 3 that in basic unit 4, is provided with; Attached to the film conductive layer on the cushion 32; Attached to the thinfilm protective coating on the film conductive layer 21.Wherein: base material is quartzy; Cushioning layer material is the aluminium film, and the film conductive layer material is a silver, and the thinfilm protective coating material is a silica.
1, the preparation of film cushion
Utilize magnetron sputtering deposition of aluminum film on quartz substrate, film thickness is 30 nanometers, and the sputtering target target material is a metallic aluminium, and sputtering power is 100 watts, and sputtering pressure is 0.9 handkerchief.
2, the preparation of film conductive layer silver
Utilize magnetron sputtering depositing the surface deposition argent film of aluminium film, the thickness of silver-colored film is 250 nanometers, and the sputtering target target material is a silver (purity 99.999%), and sputtering power is 120 watts, and sputtering pressure is 1.0 handkerchiefs.
3, the preparation of thinfilm protective coating
Utilize magnetron sputtering cvd silicon oxide film above silver-colored film, film thickness is 5 nanometers, and the working gas of sputter is an argon gas, sputtering target material is silicon (purity is 99.9%), aerating oxygen is as reacting gas during sputter, and sputtering power is 100 watts, and sputtering pressure is 0.9 handkerchief.
4, the heat treatment of sample
The sample that deposits film cushion, conductive layer and protective layer is put into Muffle furnace; under atmospheric conditions; the interior temperature of the stove that raises gradually arrives 550 ℃; constant temperature is 2 hours under 550 ℃ of temperature; close the Muffle furnace power supply then; after temperature drops to room temperature gradually in the stove, take out sample, obtain the conductive film of high temperature resistant high optical reflection.
Comprise basic unit 4; The film cushion 3 that on substrate 4, is provided with; Attached to the film conductive layer on the cushion 32; Attached to the thinfilm protective coating on the film conductive layer 21.Wherein: base material is a monocrystalline silicon piece; Cushioning layer material is aluminium, copper mixed film, and the film conductive layer material is a silver, and the thinfilm protective coating material is a zinc-oxide film.
1, the preparation of film cushion
Utilize magnetron sputtering deposited copper, aluminium mixed film on monocrystalline silicon substrate, film thickness is 30 nanometers, and the sputtering target target material is the mixture of metallic copper, aluminium, and the part by weight of copper and aluminium is 1: 1, and sputtering power is 100 watts, and sputtering pressure is 0.9 handkerchief.
2, the preparation of film conductive layer silver
Utilize magnetron sputtering depositing the surface deposition argent film of copper, aluminium mixed film, the thickness of silver-colored film is 250 nanometers, and the sputtering target target material is a silver (purity 99.999%), and sputtering power is 120 watts, and sputtering pressure is 1.0 handkerchiefs.
3, the preparation of thinfilm protective coating
Utilize magnetron sputtering depositing zinc oxide film above silver-colored film, film thickness is 10 nanometers, and the working gas of sputter is an argon gas, and sputtering target material is zinc oxide (purity is 99.9%), and sputtering power is 80 watts, and sputtering pressure is 0.9 handkerchief.
4, the heat treatment of sample
The sample that deposits film cushion, conductive layer and protective layer is put into Muffle furnace; under atmospheric conditions; the interior temperature of the stove that raises gradually arrives 550 ℃; constant temperature is 2 hours under 550 ℃ of temperature; close the Muffle furnace power supply then; after temperature drops to room temperature gradually in the stove, take out sample, obtain the conductive film of high temperature resistant high reflection.
Claims (8)
1. the conductive film of a high temperature resistant high optical reflection; it is characterized in that: this thin-film material comprises by the substrate layer that is made of inorganic oxide, is planted or film cushion that multiple metallic film constitutes, the film conductive layer that is made of argent, the thinfilm protective coating that is made of metal oxide by single, and to down and on successively arrange.
2. the conductive film of high temperature resistant high optical reflection according to claim 1 is characterized in that described film conductive layer is made of argent, and its thickness is the 150-300 nanometer.
3. the conductive film of high temperature resistant high optical reflection according to claim 1 is characterized in that described film cushion is the single or multiple lift film that single kind or multiple metal simple-substance constitute, and its thickness is 10 to 40 nanometers.
4. the conductive film of high temperature resistant high optical reflection according to claim 3, the metal that uses when it is characterized in that described single thin film is that copper, aluminium, iron, chromium, nickel, titanium or niobium simple substance constitute separately, or two or more metal mixed constitute in the above-mentioned metal.
5. conductive film according to claim 3, the metal that uses when it is characterized in that described plural layers can be the two-layer or plural layers that two or more metals are formed in copper, aluminium, iron, chromium, nickel, titanium or the niobium simple substance.
6. the conductive film of high temperature resistant high optical reflection according to claim 1; it is characterized in that described thinfilm protective coating is meant that zinc oxide, tin oxide, titanium oxide, niobium oxide, silica, aluminium oxide, indium oxide, tin-doped indium oxide or Al-Doped ZnO constitute, its thickness is the 5-15 nanometer.
7. the conductive film of high temperature resistant high optical reflection according to claim 1 is characterized in that described substrate layer material is meant aluminium oxide, optical glass, quartz, silicon chip or mica.
8. the preparation method of the conductive film of a high temperature resistant high optical reflection is characterized in that realizing by following steps:
(1) preparation of film cushion adopts coating technique that the material of film cushion is deposited on the surface of substrate layer, and its THICKNESS CONTROL is between 10 to 40 nanometers;
(2) preparation of film conductive layer adopts coating technique that the material of film conductive layer is deposited on above the film cushion, and its THICKNESS CONTROL is between 150 to 300 nanometers;
(3) preparation of thinfilm protective coating adopts coating technique that the material of thinfilm protective coating is deposited on above the film conductive layer, and its THICKNESS CONTROL is between 5 to 15 nanometers;
(4) heat treatment of the film film sample that will contain cushion, conductive layer and protective layer is put into Muffle furnace, under atmospheric conditions, 550 ℃ of heat treatment 2 hours.
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Cited By (15)
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| CN101992569A (en) * | 2009-08-19 | 2011-03-30 | 柏腾科技股份有限公司 | Base material with metalized surface |
| CN102097153A (en) * | 2009-11-11 | 2011-06-15 | 三星电子株式会社 | Conductive paste and solar cell |
| US8940195B2 (en) | 2011-01-13 | 2015-01-27 | Samsung Electronics Co., Ltd. | Conductive paste, and electronic device and solar cell including an electrode formed using the same |
| US8974703B2 (en) | 2010-10-27 | 2015-03-10 | Samsung Electronics Co., Ltd. | Conductive paste and electronic device and solar cell including an electrode formed using the same |
| US8987586B2 (en) | 2010-08-13 | 2015-03-24 | Samsung Electronics Co., Ltd. | Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste |
| US9105370B2 (en) | 2011-01-12 | 2015-08-11 | Samsung Electronics Co., Ltd. | Conductive paste, and electronic device and solar cell including an electrode formed using the same |
| CN105161220A (en) * | 2015-10-09 | 2015-12-16 | 重庆文理学院 | Preparation method of high-temperature-resistant silver conductive film |
| CN105244081A (en) * | 2013-10-16 | 2016-01-13 | 日立化成株式会社 | Laminate containig conductive fiber, photosensitive conductive film, method for producing conductive pattern, conductive pattern substrate, and touch panel |
| CN108456850A (en) * | 2018-03-07 | 2018-08-28 | 深圳大学 | A kind of Sandwich film and the preparation method and application thereof |
| CN109881152A (en) * | 2019-03-05 | 2019-06-14 | 深圳市烈变科技有限公司 | A kind of conductive film and preparation process of multilayered structure |
| CN110527959A (en) * | 2019-09-18 | 2019-12-03 | 依波精品（深圳）有限公司 | A kind of protective layer and preparation method thereof for the coat of metal |
| CN110970720A (en) * | 2019-12-03 | 2020-04-07 | 浙江清华柔性电子技术研究院 | High-temperature-resistant frequency-adjustable flexible antenna and manufacturing method thereof |
| CN112962064A (en) * | 2021-02-01 | 2021-06-15 | 国家纳米科学中心 | High-temperature-resistant optical reflecting film and preparation method and application thereof |
| CN113249724A (en) * | 2021-05-11 | 2021-08-13 | 中山大学 | Method for depositing silicon dioxide film on metal film |
| CN114231922A (en) * | 2021-11-30 | 2022-03-25 | 北京理工大学 | VO (volatile organic compound)2Method for preparing base multilayer film structure and product thereof |
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2007
- 2007-10-29 CN CNA2007100097191A patent/CN101186128A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101992569A (en) * | 2009-08-19 | 2011-03-30 | 柏腾科技股份有限公司 | Base material with metalized surface |
| CN102097153A (en) * | 2009-11-11 | 2011-06-15 | 三星电子株式会社 | Conductive paste and solar cell |
| US8987586B2 (en) | 2010-08-13 | 2015-03-24 | Samsung Electronics Co., Ltd. | Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste |
| US8974703B2 (en) | 2010-10-27 | 2015-03-10 | Samsung Electronics Co., Ltd. | Conductive paste and electronic device and solar cell including an electrode formed using the same |
| US9105370B2 (en) | 2011-01-12 | 2015-08-11 | Samsung Electronics Co., Ltd. | Conductive paste, and electronic device and solar cell including an electrode formed using the same |
| US8940195B2 (en) | 2011-01-13 | 2015-01-27 | Samsung Electronics Co., Ltd. | Conductive paste, and electronic device and solar cell including an electrode formed using the same |
| US10795469B2 (en) | 2013-10-16 | 2020-10-06 | Hitachi Chemical Company, Ltd. | Laminate containing conductive fiber, photosensitive conductive film, method for producing conductive pattern, conductive pattern substrate, and touch panel |
| CN105244081A (en) * | 2013-10-16 | 2016-01-13 | 日立化成株式会社 | Laminate containig conductive fiber, photosensitive conductive film, method for producing conductive pattern, conductive pattern substrate, and touch panel |
| CN105244081B (en) * | 2013-10-16 | 2019-03-26 | 日立化成株式会社 | Degradation inhibiting method, film and its manufacturing method and laminated body |
| CN105161220A (en) * | 2015-10-09 | 2015-12-16 | 重庆文理学院 | Preparation method of high-temperature-resistant silver conductive film |
| CN108456850A (en) * | 2018-03-07 | 2018-08-28 | 深圳大学 | A kind of Sandwich film and the preparation method and application thereof |
| CN109881152A (en) * | 2019-03-05 | 2019-06-14 | 深圳市烈变科技有限公司 | A kind of conductive film and preparation process of multilayered structure |
| CN110527959A (en) * | 2019-09-18 | 2019-12-03 | 依波精品（深圳）有限公司 | A kind of protective layer and preparation method thereof for the coat of metal |
| CN110970720A (en) * | 2019-12-03 | 2020-04-07 | 浙江清华柔性电子技术研究院 | High-temperature-resistant frequency-adjustable flexible antenna and manufacturing method thereof |
| CN112962064A (en) * | 2021-02-01 | 2021-06-15 | 国家纳米科学中心 | High-temperature-resistant optical reflecting film and preparation method and application thereof |
| CN113249724A (en) * | 2021-05-11 | 2021-08-13 | 中山大学 | Method for depositing silicon dioxide film on metal film |
| CN113249724B (en) * | 2021-05-11 | 2022-06-21 | 中山大学 | Method for depositing silicon dioxide film on metal film |
| CN114231922A (en) * | 2021-11-30 | 2022-03-25 | 北京理工大学 | VO (volatile organic compound)2Method for preparing base multilayer film structure and product thereof |
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Application publication date: 20080528 |