CN104060232A - Method for preparing hafnium-doped zinc oxide transparent conductive thin film - Google Patents
Method for preparing hafnium-doped zinc oxide transparent conductive thin film Download PDFInfo
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- CN104060232A CN104060232A CN201410278502.0A CN201410278502A CN104060232A CN 104060232 A CN104060232 A CN 104060232A CN 201410278502 A CN201410278502 A CN 201410278502A CN 104060232 A CN104060232 A CN 104060232A
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Abstract
The invention relates to a method for preparing a hafnium-doped zinc oxide transparent conductive thin film. The method is characterized by comprising the following steps: (1) pressing hafnium-doped zinc oxide nano-powder into a round blank; (2) sintering the blank in a high-temperature furnace, cooling to room temperature, and annealing to prepare a sputtering target material; (3) washing the target material with acetone and deionized water respectively, and putting into a magnetron sputtering machine; (4) washing a substrate material with acetone and deionized water respectively, putting into a magnetron sputtering machine, vacuumizing, introducing mixed gas of argon and oxygen, sputtering the target material to form a thin film on the surface of the substrate material; (5) insulating the substrate material in a heat treatment furnace, and cooling to room temperature to obtain the hafnium-doped zinc oxide transparent conductive thin film. The hafnium-doped zinc oxide transparent conductive thin film has excellent thermal stability and photoelectric performance, and is flat, compact and uniform in thickness.
Description
Technical field
The preparation method who the present invention relates to a kind of hafnium doped zinc oxide transparent conductive film, belongs to technical field of electronic materials.
Background technology
ZnO, as the typical functional materials of one, has the characteristic of many excellences: 1) have larger band gap length (Eg ~ 3.4 eV in the time of 300K) and exciton bind energy (~ 60 meV), the transparency of visible ray is fine; 2) there is stronger piezoelectric effect; 3) there is very high biological safety and biocompatibility.Therefore ZnO is called as " gordian technique material " (" key technological material) and is widely applied.In addition Zn contain abundantly, nontoxic, low price, makes ZnO class lower cost for material, therefore the progress of ZnO class material is rapid.Especially ZnO film performance can be comparable with ITO (nano indium tin), its crystalline structure is hexagonal wurtzite type, but than the easier etching of ITO, be easy to realize doping, and good stability in plasma body, thereby likely become the substitute products of ITO, especially in solar cell transparency electrode field.By adding doped element can regulate and control, improve film performance, the ZnO (AZO) that mixes at present Al is the best Zinc oxide doped material of current performance.
Research finds, the character of doping system (electric conductivity with thermostability etc.) is relevant with the correction for semi-diameter with matrix ion of dopant ion with the electronic configuration of doped element.Generally speaking, the two ionic radius is more approaching, and thermostability and conductivity are better.To recently seeing, no matter be out-shell electron quantity or ionic radius, Hf is more preferably doped element of one, the ZnO of Hf doping is expected to have more excellent performance.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of hafnium doped zinc oxide transparent conductive film is provided, sintering temperature is low, and technique is simple, with low cost; The hafnium doped zinc oxide transparent conductive film obtaining has good thermostability and photoelectric properties, and smooth densification, even thickness.
According to technical scheme provided by the invention, a kind of preparation method of hafnium doped zinc oxide transparent conductive film, feature is to comprise following processing step:
(1) prepare the zinc oxide nano-powder that hafnium adulterates:
A, take hafnium salt and zinc salt, ensure that the mol ratio of hafnium and zinc is 0.5:99.5～20:80; Hafnium salt and zinc salt are mixed;
In the mixture of b, the zinc salt obtaining to step a and hafnium salt, add deionized water, obtain the solution that concentration is 0.2mol/L～5 mol/L;
In c, the solution that obtains to step b, adding concentration is the aqueous solution of urea of 0.5 mol/L ~ 10 mol/L, and the volume ratio of the solution that aqueous solution of urea and step b obtain is 1～3:1, and mixes;
The pH value of the solution that d, regulating step c obtain is 6.5～8.5, and controlling solution temperature is 50～90 DEG C, carries out precipitin reaction 1～10 hour; Centrifugation obtains coprecipitate, coprecipitate is washed 3～8 times with deionized water, obtains white solid;
E, the white solid that steps d is obtained are dried 5～10 hours at 80～120 DEG C, obtain presoma; Presoma, 400～800 DEG C of sintering 1～5 hour, is obtained to described hafnium nanometer doped zinc oxide conductive powder material;
(2) zinc oxide nano-powder of hafnium doping is pressed into the circular base substrate that diameter is 20～100mm, pressure is 50～85MPa;
(3) base substrate step (2) being obtained carries out sintering in High Temperature Furnaces Heating Apparatus, and sintering temperature is 1400～1500 DEG C, and sintering time is 2～4 hours; Speed of cooling with 2～10 DEG C is cooled to room temperature, then 700～800 DEG C of annealing 1～6 hour, makes sputtering target material;
(4) target step (3) being obtained adopt respectively acetone and washed with de-ionized water clean, put into magnetic control sputtering device;
(5) after base material being used respectively acetone and washed with de-ionized water clean, put into magnetic control sputtering device, being first evacuated to vacuum tightness is 0.2 × 10
-4～2 × 10
-4pa, then pass into the mixed gas of argon gas and oxygen, the pressure of argon gas is 0.2～2Pa, and the pressure of oxygen is 0.2～4Pa, then target is carried out to sputter, and sputtering power is 50～500W, and sputtering time is 10～200 minutes; Thereby form film at substrate material surface;
(6) step (5) base material after treatment is incubated in heat treatment furnace, temperature is 400～600 DEG C, and soaking time is 1～2 hour, is then cooled to room temperature, obtains described hafnium doped zinc oxide transparent conductive film.
Further, described base material is glass slide, silicate glass or PET film.
Further, described zinc salt is zinc nitrate, and hafnium salt is hafnium chloride.
The present invention has the following advantages: adopting hafnium doped zinc oxide nano conductive powder body is that starting material are prepared target, and sintering temperature is low, and the target density that obtains is high, good uniformity, stable performance, and composition is controlled; Utilize made target to adopt magnetron sputtering method deposition to obtain transparent conductive film, smooth densification, even thickness, Heat stability is good, photoelectric properties excellence, and sintering temperature is low, technique is simple, with low cost, be easy to realize suitability for industrialized production, can be applicable to the field such as flat-panel monitor, solar cell.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment mono-: a kind of preparation method of hafnium doped zinc oxide transparent conductive film, comprises following processing step:
(1) prepare the zinc oxide nano-powder that hafnium adulterates:
A, take 114.3g zinc nitrate and 32g hafnium chloride, magnetic agitation mixes;
B, obtain adding 550mL deionized water in mixture to step a, obtain settled solution;
C, 62g urea is added in 550mL deionized water and makes aqueous solution of urea, in the solution obtaining to step b, add aqueous solution of urea, and mix;
The pH value of the solution that d, regulating step c obtain is 6.5, and controlling solution temperature is 85 DEG C, carries out precipitin reaction 1 hour under the agitation condition of 600 revs/min; Centrifugation obtains coprecipitate, coprecipitate is washed 3 times with deionized water, obtains white solid;
E, the white solid that steps d is obtained are dried 10 hours at 80 DEG C, obtain presoma; Presoma, 400 DEG C of sintering 5 hours, is obtained to described hafnium nanometer doped zinc oxide conductive powder material;
(2) zinc oxide nano-powder of hafnium doping is pressed into the circular base substrate that diameter is 30mm, pressure is 60MPa;
(3) base substrate step (2) being obtained carries out sintering in High Temperature Furnaces Heating Apparatus, and sintering temperature is 1400 DEG C, and sintering time is 4 hours; Speed of cooling with 2 DEG C is cooled to room temperature, then 700 DEG C of annealing 6 hours, makes sputtering target material;
(4) target step (3) being obtained adopt respectively acetone and washed with de-ionized water clean, put into magnetic control sputtering device;
(5) after silicate glass base material being used respectively acetone and washed with de-ionized water clean, put into magnetic control sputtering device, being first evacuated to vacuum tightness is 1 × 10
-4pa, then pass into the mixed gas of argon gas and oxygen, the pressure of argon gas is 0.6Pa, and the pressure of oxygen is 1Pa, then target is carried out to sputter, and sputtering power is 200W, and sputtering time is 25 minutes; Thereby form film at silicate glass substrate material surface;
(6) step (5) base material after treatment (described base material is glass slide, silicate glass or PET film) is incubated in heat treatment furnace, temperature is 400 DEG C, soaking time is 2 hours, is then cooled to room temperature, obtains described hafnium doped zinc oxide transparent conductive film.
Adopt scanning electronic microscope, atomic force microscope, four-point probe measurment instrument, ultraviolet-visible infrared spectrophotometer to measure thickness, surfaceness, resistivity and the visible light transmissivity of prepared hafnium doping zinc-oxide film.Result shows: the thickness of film is about 100 nm, and surfaceness is 50nm, and the resistivity of film is 4.1 × 10
-3Ω cm, the average transmittances of visible ray exceedes 83%.
Embodiment bis-: a kind of preparation method of hafnium doped zinc oxide transparent conductive film, comprises following processing step:
(1) prepare the zinc oxide nano-powder that hafnium adulterates:
A, take 50.8g zinc nitrate and 32g hafnium chloride, mix;
B, obtain adding 275mL deionized water in mixture to step a, obtain settled solution;
C, 31g urea is added in 275mL deionized water and makes aqueous solution of urea, in the solution obtaining to step b, add aqueous solution of urea, and mix;
The pH value of the solution that d, regulating step c obtain is 7, and controlling solution temperature is 90 DEG C, carries out precipitin reaction 10 hours under the agitation condition of 600 revs/min; Centrifugation obtains coprecipitate, coprecipitate is washed 8 times with deionized water, obtains white solid;
E, the white solid that steps d is obtained are dried 5 hours at 120 DEG C, obtain presoma; Presoma, 800 DEG C of sintering 1 hour, is obtained to described hafnium nanometer doped zinc oxide conductive powder material;
(2) zinc oxide nano-powder of hafnium doping is pressed into the circular base substrate that diameter is 20mm, pressure is 70MPa;
(3) base substrate step (2) being obtained carries out sintering in High Temperature Furnaces Heating Apparatus, and sintering temperature is 1500 DEG C, and sintering time is 3 hours; Speed of cooling with 10 DEG C is cooled to room temperature, then 800 DEG C of annealing 1 hour, makes sputtering target material;
(4) target step (3) being obtained adopt respectively acetone and washed with de-ionized water clean, put into magnetic control sputtering device;
(5) after glass slide being used respectively acetone and washed with de-ionized water clean, put into magnetic control sputtering device, being first evacuated to vacuum tightness is 0.2 × 10
-4pa, then pass into the mixed gas of argon gas and oxygen, the pressure of argon gas is 0.2Pa, and the pressure of oxygen is 0.2Pa, then target is carried out to sputter, and sputtering power is 50W, and sputtering time is 200 minutes; Thereby form film on glass slide surface;
(6) step (5) base material after treatment (described base material is glass slide, silicate glass or PET film) is incubated in heat treatment furnace, temperature is 600 DEG C, soaking time is 1 hour, is then cooled to room temperature, obtains described hafnium doped zinc oxide transparent conductive film.
Adopt scanning electronic microscope, atomic force microscope, four-point probe measurment instrument, ultraviolet-visible infrared spectrophotometer to measure thickness, surfaceness, resistivity and the visible light transmissivity of prepared hafnium doping zinc-oxide film.Result shows: the thickness of film is about 120 nm, and surfaceness is 30nm, and the resistivity of film is 2.2 × 10
-4Ω cm, the average transmittances of visible ray exceedes 89%.
Embodiment tri-: a kind of preparation method of hafnium doped zinc oxide transparent conductive film, comprises following processing step:
(1) prepare the zinc oxide nano-powder that hafnium adulterates:
A, take 228g zinc nitrate and 32g hafnium chloride, mix;
B, obtain adding 900mL deionized water in mixture to step a, obtain settled solution;
C, 31g urea is added in 900mL deionized water and makes aqueous solution of urea, in the solution obtaining to step b, add aqueous solution of urea, and mix;
The pH value of the solution that d, regulating step c obtain is 8.5, and controlling solution temperature is 80 DEG C, carries out precipitin reaction 6 hours; Centrifugation obtains coprecipitate, coprecipitate is washed 5 times with deionized water, obtains white solid;
E, the white solid that steps d is obtained are dried 6 hours at 100 DEG C, obtain presoma; Presoma, 600 DEG C of sintering 2 hours, is obtained to described hafnium nanometer doped zinc oxide conductive powder material;
(2) zinc oxide nano-powder of hafnium doping is pressed into the circular base substrate that diameter is 100mm, pressure is 80MPa;
(3) base substrate step (2) being obtained carries out sintering in High Temperature Furnaces Heating Apparatus, and sintering temperature is 1550 DEG C, and sintering time is 2.5 hours; Speed of cooling with 5 DEG C is cooled to room temperature, then 750 DEG C of annealing 2 hours, makes sputtering target material;
(4) target step (3) being obtained adopt respectively acetone and washed with de-ionized water clean, put into magnetic control sputtering device;
(5) after PET film being used respectively acetone and washed with de-ionized water clean, put into magnetic control sputtering device, being first evacuated to vacuum tightness is 2 × 10
-4pa, then pass into the mixed gas of argon gas and oxygen, the pressure of argon gas is 2Pa, and the pressure of oxygen is 4Pa, then target is carried out to sputter, and sputtering power is 200W, and sputtering time is 60 minutes; Thereby form film at PET film surface;
(6) PET film after treatment step (5) is incubated in heat treatment furnace, temperature is 500 DEG C, and soaking time is 1.5 hours, is then cooled to room temperature, obtains described hafnium doped zinc oxide transparent conductive film.
Adopt scanning electronic microscope, atomic force microscope, four-point probe measurment instrument, ultraviolet-visible infrared spectrophotometer to measure thickness, surfaceness, resistivity and the visible light transmissivity of prepared hafnium doping zinc-oxide film.Result shows: the thickness of film is about 120 nm, and surfaceness is 45nm, and the resistivity of film is 4.2 × 10
-4Ω cm, the average transmittances of visible ray exceedes 86%.
Claims (3)
1. a preparation method for hafnium doped zinc oxide transparent conductive film, is characterized in that, comprises following processing step:
(1) prepare the zinc oxide nano-powder that hafnium adulterates:
A, take hafnium salt and zinc salt, ensure that the mol ratio of hafnium and zinc is 0.5:99.5～20:80; Hafnium salt and zinc salt are mixed;
In the mixture of b, the zinc salt obtaining to step a and hafnium salt, add deionized water, obtain the solution that concentration is 0.2mol/L～5 mol/L;
In c, the solution that obtains to step b, adding concentration is the aqueous solution of urea of 0.5 mol/L ~ 10 mol/L, and the volume ratio of the solution that aqueous solution of urea and step b obtain is 1～3:1, and mixes;
The pH value of the solution that d, regulating step c obtain is 6.5～8.5, and controlling solution temperature is 50～90 DEG C, carries out precipitin reaction 1～10 hour; Centrifugation obtains coprecipitate, coprecipitate is washed 3～8 times with deionized water, obtains white solid;
E, the white solid that steps d is obtained are dried 5～10 hours at 80～120 DEG C, obtain presoma; Presoma, 400～800 DEG C of sintering 1～5 hour, is obtained to described hafnium nanometer doped zinc oxide conductive powder material;
(2) zinc oxide nano-powder of hafnium doping is pressed into the circular base substrate that diameter is 20～100mm, pressure is 50～85MPa;
(3) base substrate step (2) being obtained carries out sintering in High Temperature Furnaces Heating Apparatus, and sintering temperature is 1400～1500 DEG C, and sintering time is 2～4 hours; Speed of cooling with 2～10 DEG C is cooled to room temperature, then 700～800 DEG C of annealing 1～6 hour, makes sputtering target material;
(4) target step (3) being obtained adopt respectively acetone and washed with de-ionized water clean, put into magnetic control sputtering device;
(5) after base material being used respectively acetone and washed with de-ionized water clean, put into magnetic control sputtering device, being first evacuated to vacuum tightness is 0.2 × 10
-4～2 × 10
-4pa, then pass into the mixed gas of argon gas and oxygen, the pressure of argon gas is 0.2～2Pa, and the pressure of oxygen is 0.2～4Pa, then target is carried out to sputter, and sputtering power is 50～500W, and sputtering time is 10～200 minutes; Thereby form film at substrate material surface;
(6) step (5) base material after treatment is incubated in heat treatment furnace, temperature is 400～600 DEG C, and soaking time is 1～2 hour, is then cooled to room temperature, obtains described hafnium doped zinc oxide transparent conductive film.
2. the preparation method of hafnium doped zinc oxide transparent conductive film as claimed in claim 1, is characterized in that: described base material is glass slide, silicate glass or PET film.
3. the preparation method of hafnium doped zinc oxide transparent conductive film as claimed in claim 1, is characterized in that: described zinc salt is zinc nitrate, and hafnium salt is hafnium chloride.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114477993A (en) * | 2022-01-24 | 2022-05-13 | 仲恺农业工程学院 | ZnO material and basic property research method and application thereof |
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