CN101260512B - Method for preparing tantalum doping tin oxide transparent conductive film - Google Patents
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- CN101260512B CN101260512B CN2008100583122A CN200810058312A CN101260512B CN 101260512 B CN101260512 B CN 101260512B CN 2008100583122 A CN2008100583122 A CN 2008100583122A CN 200810058312 A CN200810058312 A CN 200810058312A CN 101260512 B CN101260512 B CN 101260512B
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- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 51
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 48
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 25
- 229910001887 tin oxide Inorganic materials 0.000 title claims description 44
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000005477 sputtering target Methods 0.000 claims abstract description 18
- 239000013077 target material Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000010408 film Substances 0.000 claims description 89
- 238000004544 sputter deposition Methods 0.000 claims description 27
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- 239000012535 impurity Substances 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000003570 air Substances 0.000 claims description 7
- 239000000356 contaminant Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 8
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 231100000419 toxicity Toxicity 0.000 abstract description 5
- 230000001988 toxicity Effects 0.000 abstract description 5
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 abstract 1
- 238000002834 transmittance Methods 0.000 description 7
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 238000000280 densification Methods 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 231100001234 toxic pollutant Toxicity 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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Abstract
The invention relates to a method for preparing tantalum jewellers putty-doped transparent conductive film. The method is characterized in that Ta2O5 powder and SnO2 powder with 99.99 percent purity quotient are fully mixed according to weight ratio between 1:99 to 10:90, pressed, molded and sintered into a tantalum jewellers putty-doped sputtering target material under the temperature between 1500 DEG C and 1650 DEG C, then a jewellers putty-doped transparent conductive film with different tantalum contents is prepared by a magnetron sputtering method. The prepared film has the characteristics of smooth and compact surface, uniform film thickness, excellent photoelectric performance, simple preparation technology, low cost and easy realization of industrialized production, etc. and also has good mechanical performance, chemical durability, high-temperature thermal stability and biocompatibility. The film can not only be used for a flat-panel dispaly, a solar battery, a transparent electromagnetic shielding and antistatic device but also used for a resistance type touch screen, a biosensor, etc. which have special needs on the toxicity and biocompatibility of the film.
Description
Technical field
The present invention relates to a kind of preparation method of tantalum doping tin oxide transparent conductive film, especially a kind of method that adopts magnetron sputtering method to prepare tantalum doping tin oxide transparent conductive film belongs to technical field of electronic materials.
Background technology
The transparent conductive metal oxide film since to visible light have very high transmitance (＞85%), resistivity is very low (can reach 10
-3～10
-4Ω cm) etc. excellent photoelectric properties, thereby obtained in fields such as flat-panel monitor, solar cell, transparency electromagnetic wave shield and anti static device, resistive touch screen and biosensors using widely, wherein using maximum transparent conductive films is tin-doped indium oxide (Indium Tin Oxide is called for short ITO) film.Although the ITO transparent conductive film is widely used in a lot of fields, but because it exists complicated process of preparation, the poor high temperature stability (problem that has the indium diffusion when comparatively high temps uses, can influence the performance of device), (indium is a noble metal to the cost height, the nature reserves seldom) etc. shortcoming, particularly mechanical properties in films, chemical durability are poor, and indium and compound thereof have certain bio-toxicity, thereby have limited its range of application greatly.For example, not only require film to have excellent photoelectric properties, also require it to have good mechanical performance, chemical durability, thermostability, and film can not be toxic for transparent conductive film as the resistive touch screen electrode materials.As the transparent conductive film of biosensor solid support material, have the excellent electric property in addition, also require it to have excellent chemical durability and biocompatibility except requiring film.
Stannic oxide (SnO
2) film not only can obtain excellent photoelectric properties after by some elements that mix, and film has good mechanical performance, chemical durability, thermostability, wherein studying many is fluorine-doped tin oxide (Fluorin Tin Oxide, be called for short FTO) and antimony-doped tin oxide (Antimony Tin Oxide is called for short ATO) film.But fluorine and antimony element have certain bio-toxicity, when they use as resistive touch screen electrode materials or biosensor solid support material, can produce certain influence to device performance.Tantalum (Ta) is a kind of 5 valency elements, and it can be significantly improved electric property, optical property, chemical durability and the thermostability of film as the doped element of SnO 2 thin film.The Ta element does not have toxicity and has excellent biocompatibility simultaneously.Therefore, the adulterated SnO 2 thin film of tantalum element not only can be used for flat-panel monitor, solar cell, transparency electromagnetic wave shield and anti static device, and can be used for that film toxicity, biocompatibility are had fields such as the resistive touch screen of particular requirement and biosensor.
At present, the preparation method of doped stannum oxide film mainly contains spraying method, spray heating decomposition, chemical Vapor deposition process (CVD) and magnetron sputtering method or the like, it is poor that wherein there is film forming thickness evenness in first three methods, be difficult to be controlled to membrane process, can produce toxic pollutant during film forming, shortcomings such as material cost is higher, and production efficiency is low.And when preparing the doped stannum oxide film with magnetron sputtering method, have thicknesses of layers evenly and be easy to control, the smooth densification of film surface, rete and substrate adhesion by force, preparation is simple, production efficiency height and advantage such as with low cost.Therefore, become the main method of preparation doped tin oxide transparent conductive film on the current industrial.Find by retrieval the prior art document, though Y.W.Kim and S.W.Lee etc. adopt Metalorganic Chemical Vapor Deposition (MOCVD, belong to a kind of of CVD method) prepared the adulterated SnO 2 thin film of tantalum, and the film of this method preparation has good optical and electric property, but when preparing film with the MOCVD method, but exist metallorganics material cost height, membrane uniformity poor, can produce many deficiencies such as toxic pollutant, production efficiency are low." microtexture of the tantalum doping tin oxide film of Metalorganic Chemical Vapor Deposition preparation develops and electric property " referring to people such as Y.W.Kim, " thin solid film " (Thin SolidFilms, 2002, Vol.405,256～262, " Microstructural evolution and electricalproperty of Ta-doped SnO
2Films grown on Al
2O
3(0001) by metalorganicchemical vapor deposition "); People's such as S.W.Lee " Scium trioxide of Metalorganic Chemical Vapor Deposition preparation and the characteristic of tantalum doping tin oxide optical coating ", " Materials Science and Engineering B " (MaterialsScience and Engineering B, 2003, Vol.99,134～137, " Characterization ofMOCVD grown optical coatings of Sc
2O
3And Ta-doped SnO
2").Also do not find as yet about the report for preparing the tantalum element doped tin oxide transparent conductive film with magnetron sputtering method at present.
Summary of the invention
The present invention is directed to existing doped tin oxide transparent conductive film and preparation method thereof above shortcomings, a kind of preparation method of tantalum doping tin oxide transparent conductive film is provided.
The present invention is achieved by the following technical solutions: a kind of preparation method of tantalum doping tin oxide transparent conductive film is characterized in that through following process steps:
(1) with purity is 99.99% tantalum oxide (Ta
2O
5) and stannic oxide (SnO
2) the powder thorough mixing, after being pressed into base under the pressure of 60～80Mpa, put into high temperature sintering furnace, 1500～1650 ℃ of following sintering are 3～5 hours in air, sinter the tantalum doping tin oxide sputtering target material into;
(2) prepared tantalum doping tin oxide sputtering target material is fully cleaned with analytical pure acetone and deionized water, 120～140 ℃ of insulations 2～3 hours, remove impurity such as surface and oil contaminant then;
(3) adopt common slide glass as the film substrate material, before sputter,, be incubated 1～2 hour at 80～90 ℃ afterwards, with impurity such as removal surface and oil contaminants earlier with analytical pure acetone and washed with de-ionized water;
(4) sputtering target material and the slide that will handle through step (2) and (3) put into magnetic control sputtering device, vacuumizes to make sputtering chamber base vacuum degree reach 1 * 10
-4Pa continues to charge into purity and is the mixed gas of the oxygen of 99.999% argon gas and 99.99% then, then to the pre-sputter 5min of target, remove surface impurity after, keep 25～100 ℃ of substrate of glass temperature, again target is carried out sputter, make sputter attitude film;
(5) (4) step gained film being put into heat treatment furnace, is 400～600 ℃ in temperature, heat-treats under the condition that is incubated 0.5～3 hour, afterwards sample is cooled to room temperature, promptly gets tantalum doping tin oxide transparent conductive film.
In the described step (1), the composition of tantalum doping tin oxide sputtering target material: Ta in the target
2O
5Quality percentage composition (wt.%) be controlled at 1～10%, all the other are SnO
2
Thin film sputtering processing condition in the described step (4) are: sputtering power 50～400W, in the sputter procedure, argon pressure is 0.4～1Pa in the control sputtering chamber, and oxygen partial pressure is 0.5～1.5Pa, so that the blending ratio of control argon gas and oxygen, sputtering time 15～50min.
Heat-treating atmosphere in the described step (5) is air, nitrogen or argon gas.
The tantalum doping tin oxide transparent conductive film of the inventive method preparation is compared following advantage with existing transparent conductive film: adopt the tantalum doping tin oxide transparent conductive film of magnetron sputtering method preparation have thicknesses of layers evenly, the densification that has an even surface, rete and substrate adhesion by force, preparation is simple, production efficiency and advantage such as with low cost.Film not only has excellent photoelectric properties, and (resistivity can reach 10
-3～10
-4Ω cm is to average transmittances＞85% of visible light), and have good mechanical performance, chemical durability, high high-temp stability, film is nontoxic and have an excellent biocompatibility.Prepared film not only can be used for flat-panel monitor, solar cell, transparency electromagnetic wave shield and anti static device, and can be used in film toxicity, biocompatibility are had fields such as the resistive touch screen of particular requirement and biosensor.
Description of drawings
Fig. 1 is the resistivity of the doped tin oxide transparent conductive film of different tantalum contents.
Fig. 2 is the transmitance of the doped tin oxide transparent conductive film of different tantalum contents.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is further described.
(1) with purity is 99.99% Ta
2O
5And SnO
2The powder thorough mixing after being pressed into base under the pressure of 80Mpa, is put into high temperature sintering furnace through 1650 ℃ of following sintering 3 hours, obtains the tantalum doping tin oxide sputtering target material, Ta in the target
2O
5Quality percentage composition (wt.%) be 1%, SnO
2Quality percentage composition (wt.%) be 99%, target is of a size of: diameter 60mm, thickness 6mm;
(2) prepared tantalum doping tin oxide sputtering target material is fully cleaned with analytical pure acetone and deionized water, insert then in the baking oven,, remove impurity such as surface and oil contaminant 120 ℃ of insulations 3 hours;
(3) adopt common slide glass as the film substrate material, before sputter, fully clean, put into baking oven then, 80 ℃ of insulations 2 hours with analytical pure acetone and deionized water;
(4) (2) and (3) step is pretreated target and slide are installed, are put into magnetic control sputtering device, vacuumize to make sputtering chamber base vacuum degree reach 1 * 10
-4Pa, continue to charge into purity then and be the mixed gas of the oxygen of 99.999% argon gas and 99.99%, then, behind the removal surface impurity, substrate of glass is heated to 100 ℃ to the pre-sputter 5min of target, again to target as sputter 25min, thereby make sputter attitude tantalum doping tin oxide film, the sputtering technology condition is: sputtering power 200W, in the sputter procedure, Ar Pressure is 0.6Pa in the control sputtering chamber, and oxygen partial pressure is 1Pa;
(5) film that (4) step is made is put into heat treatment furnace and is heat-treated, and heat-treating atmosphere is an air, 600 ℃ of temperature, and soaking time 0.5 hour is cooled to room temperature with sample afterwards, promptly gets tantalum doping tin oxide transparent conductive film.
Adopt surface profiler, atomic force microscope, four-point probe measurment instrument, UV, visible light infrared spectrophotometer to measure thickness, surfaceness, resistivity and the visible light transmissivity of prepared tantalum doping tin oxide film respectively.The result shows: the thickness of film is about 120nm, and surfaceness (RMS) is about 5～6nm, and the resistivity of film is 9.2 * 10
-3About Ω cm, film surpasses 86% to the average transmittances of visible light.Illustrate prepared film have an even surface densification, have excellent photoelectric properties.
Except that the composition of sputtering target material and preparation parameter and embodiment 1 are different: be 99.99% Ta with purity
2O
5And SnO
2The powder thorough mixing after being pressed into base under the pressure of 80Mpa, is put into high temperature sintering furnace through 1600 ℃ of following sintering 4 hours, obtains the tantalum doping tin oxide sputtering target material, Ta in the target
2O
5Quality percentage composition (wt.%) be 5%, SnO
2Quality percentage composition (wt.%) be 95%, target is of a size of diameter 60mm, thickness 6mm;
All the other processing steps are identical with embodiment 1.
Measuring result shows: the thickness of film is about 120nm, and surfaceness (RMS) is about 4～5nm, and the resistivity of film is 2.1 * 10
-3About Ω cm, film surpasses 90% to the average transmittances of visible light.
Except that the composition of sputtering target material and preparation parameter and embodiment 1 are different: be 99.99% Ta with purity
2O
5And SnO
2The powder thorough mixing after being pressed into base under the pressure of 60Mpa, is put into high temperature sintering furnace through 1500 ℃ of following sintering 5 hours, obtains the tantalum doping tin oxide sputtering target material, Ta in the target
2O
5Quality percentage composition (wt.%) be 10%, SnO
2Quality percentage composition (wt.%) be 90%, target is of a size of diameter 60mm, thickness 6mm.
All the other processing steps are identical with embodiment 1.
Measuring result shows: the thickness of film is about 130nm, and surfaceness (RMS) is about 5～6nm, and the resistivity of film is 7.9 * 10
-3About Ω cm, film surpasses 86% to the average transmittances of visible light.
(1) with purity is 99.99% Ta
2O
5And SnO
2The powder thorough mixing after being pressed into base under the pressure of 80Mpa, is put into high temperature sintering furnace through 1600 ℃ of following sintering 4 hours, obtains the tantalum doping tin oxide sputtering target material, Ta in the target
2O
5Quality percentage composition (wt.%) be 5%, SnO
2Quality percentage composition (wt.%) be 95%, target is of a size of diameter 60mm, thickness 6mm;
(2) prepared tantalum doping tin oxide sputtering target material is fully cleaned with analytical pure acetone and deionized water, insert then in the baking oven,, remove impurity such as surface and oil contaminant 140 ℃ of insulations 2 hours;
(3) adopt common slide glass as the film substrate material, before sputter, fully clean, put into baking oven then, 90 ℃ of insulations 1 hour with analytical pure acetone and deionized water;
(4) (2) and (3) step is pretreated target and slide are installed, are put into magnetic control sputtering device, vacuumize to make sputtering chamber base vacuum degree reach 1 * 10
-4Pa, continue to charge into purity then and be the mixed gas of the oxygen of 99.999% argon gas and 99.99%, then, behind the removal surface impurity, substrate of glass is heated to 50 ℃ to the pre-sputter 5min of target, again to target as sputter 50min, thereby make sputter attitude tantalum doping tin oxide film, the sputtering technology condition is: sputtering power 50W, in the sputter procedure, Ar Pressure is 1Pa in the control sputtering chamber, and oxygen partial pressure is 1.5Pa;
(5) film that (4) step is made is put into heat treatment furnace and is heat-treated, and heat-treating atmosphere is an air, 500 ℃ of temperature, and soaking time 1.5 hours is cooled to room temperature with sample afterwards, promptly gets tantalum doping tin oxide transparent conductive film.
Adopt surface profiler, atomic force microscope, four-point probe measurment instrument, UV, visible light infrared spectrophotometer to measure thickness, surfaceness, resistivity and the visible light transmissivity of prepared tantalum doping tin oxide film equally respectively.The result shows: the thickness of film is about 100nm, and surfaceness (RMS) is about 4～5nm, and the resistivity of film is 4.1 * 10
-3About Ω cm, film surpasses 87% to the average transmittances of visible light.Illustrate prepared film have an even surface densification, have excellent photoelectric properties.
(1) with purity is 99.99% Ta
2O
5And SnO
2The powder thorough mixing after being pressed into base under the pressure of 80Mpa, is put into high temperature sintering furnace through 1600 ℃ of following sintering 4 hours, obtains the tantalum doping tin oxide sputtering target material, Ta in the target
2O
5Quality percentage composition (wt.%) be 5%, SnO
2Quality percentage composition (wt.%) be 95%, target is of a size of diameter 60mm, thickness 6mm;
(2) prepared tantalum doping tin oxide sputtering target material is fully cleaned with analytical pure acetone and deionized water, insert then in the baking oven,, remove impurity such as surface and oil contaminant 140 ℃ of insulations 2 hours;
(3) adopt common slide glass as the film substrate material, before sputter, fully clean, put into baking oven then, 90 ℃ of insulations 1 hour with analytical pure acetone and deionized water;
(4) (2) and (3) step is pretreated target and slide are installed, are put into magnetic control sputtering device, vacuumize to make sputtering chamber base vacuum degree reach 1 * 10
-4Pa, continue to charge into purity then and be the mixed gas of the oxygen of 99.999% argon gas and 99.99%, then to the pre-sputter 5min of target, behind the removal surface impurity, the substrate of glass temperature is 25 ℃, again to target as sputter 15min, thereby make sputter attitude tantalum doping tin oxide film, the sputtering technology condition is: sputtering power 400W, in the sputter procedure, Ar Pressure is 0.4Pa in the control sputtering chamber, and oxygen partial pressure is 0.5Pa;
(5) film that (4) step is made is put into heat treatment furnace and is heat-treated, and heat-treating atmosphere is an air, 400 ℃ of temperature, and soaking time 3 hours is cooled to room temperature with sample afterwards, promptly gets tantalum doping tin oxide transparent conductive film.
Measuring result shows: the thickness of film is about 150nm, and surfaceness (RMS) is about 6～7nm, and the resistivity of film is 4.6 * 10
-3About Ω cm, film surpasses 87% to the average transmittances of visible light.Illustrate prepared film have an even surface densification, have excellent photoelectric properties.
The foregoing description is the result show, the prepared tantalum doping tin oxide transparent conductive film of the present invention have the densification of having an even surface, thicknesses of layers evenly, rete and substrate adhesion is strong, excellent (resistivity can reach 10 to photoelectric properties
-3～10
-4Ω cm is to average transmittances＞85% of visible light), preparation is simple, with low cost, is easy to realize characteristics such as suitability for industrialized production; Also have good mechanical performance, chemical durability, high high-temp stability simultaneously, film is nontoxic and have an excellent biocompatibility.The gained film not only can be used for flat-panel monitor, solar cell, transparency electromagnetic wave shield and anti static device, and can be used in film toxicity, biocompatibility are had fields such as the resistive touch screen of particular requirement and biosensor.
Claims (2)
1. the preparation method of a tantalum doping tin oxide transparent conductive film is characterized in that through following process steps:
(1) with purity is 99.99% Ta
2O
5And SnO
2The powder thorough mixing after being pressed into base under the pressure of 60～80Mpa, is put into high temperature sintering furnace, and 1500～1650 ℃ of following sintering are 3～5 hours in air, sinter the tantalum doping tin oxide sputtering target material into, Ta in the target
2O
5The quality percentage composition be controlled at 1～10%, all the other are SnO
2
(2) prepared tantalum doping tin oxide sputtering target material is fully cleaned with analytical pure acetone and deionized water, 120～140 ℃ of insulations 2～3 hours, remove surface and oil contaminant impurity then;
(3) adopt common slide glass as the film substrate material, before sputter,, be incubated 1～2 hour at 80～90 ℃ afterwards, to remove surface and oil contaminant impurity earlier with analytical pure acetone and washed with de-ionized water;
(4) sputtering target material and the common slide glass that will handle through step (2) and (3) put into magnetic control sputtering device, vacuumizes to make sputtering chamber base vacuum degree reach 1 * 10
-4Pa, continue to charge into purity then and be the mixed gas of the oxygen of 99.999% argon gas and 99.99%, then to the pre-sputter 5min of target, remove surface impurity after, keep 25～100 ℃ of common slide glass base reservoir temperatures, again target is carried out sputter, make sputter attitude film, the thin film sputtering processing condition are: sputtering power 50～400W, in the sputter procedure, argon pressure is 0.4～1Pa in the control sputtering chamber, and oxygen partial pressure is 0.5～1.5Pa, sputtering time 15～50min;
(5) (4) step gained film being put into heat treatment furnace, is 400～600 ℃ in temperature, heat-treats under the condition that is incubated 0.5～3 hour, afterwards film is cooled to room temperature, promptly gets tantalum doping tin oxide transparent conductive film.
2. by the preparation method of the described a kind of tantalum doping tin oxide transparent conductive film of claim 1, it is characterized in that the heat-treating atmosphere in the described step (5) is air, nitrogen or argon gas.
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| CN103695854A (en) * | 2013-12-12 | 2014-04-02 | 宁夏东方钽业股份有限公司 | Process for preparing corrosion resistant metal material through coating tantalum or niobium with PVD (physical vapor deposition) method |
| JP2019142761A (en) * | 2018-02-19 | 2019-08-29 | 住友化学株式会社 | Tin oxide-based sintered body and method for manufacturing the same |
| CN108546993A (en) * | 2018-05-14 | 2018-09-18 | 山东大学 | A kind of rutile structure tantalum doping tin oxide monocrystal thin films and preparation method thereof of edge [101] crystal orientation growth |
| CN114822987B (en) * | 2022-04-22 | 2023-04-14 | 厦门大学 | Ultraviolet-visible-near infrared transparent high-conductivity Ta doped SnO 2 Film and preparation method |
| CN116813329A (en) * | 2023-05-30 | 2023-09-29 | 芜湖映日科技股份有限公司 | Preparation method of high-density tin-tantalum oxide target |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000281431A (en) * | 1999-03-30 | 2000-10-10 | Mitsui Mining & Smelting Co Ltd | Tin dioxide-based sintered compact, material for thin film formation and electroconductive film |
| US20080099731A1 (en) * | 2006-10-31 | 2008-05-01 | H.C. Starck Inc. | Tin oxide-based sputtering target, low resistivity, transparent conductive film, method for producing such film and composition for use therein |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000281431A (en) * | 1999-03-30 | 2000-10-10 | Mitsui Mining & Smelting Co Ltd | Tin dioxide-based sintered compact, material for thin film formation and electroconductive film |
| US20080099731A1 (en) * | 2006-10-31 | 2008-05-01 | H.C. Starck Inc. | Tin oxide-based sputtering target, low resistivity, transparent conductive film, method for producing such film and composition for use therein |
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