CN101378091A - n-ZnO nanometer line/p-NiO alloplasm heterogeneous pn junction diode and preparation method thereof - Google Patents
n-ZnO nanometer line/p-NiO alloplasm heterogeneous pn junction diode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an n-zinc oxide nanowire/p-nickle oxide heterogeneous pn diode, which at least comprises a pn junction and an ohmic contact electrode. The pn junction consists of an n type ZnO film seed layer or an n type ZnO nanowire grown on a film seed layer doped with ZnO; and NiO material is plated on the ZnO nanowire to obtain heterogeneous pn junction. The invention first uses magnetron sputtering technology to prepare a ZnO or AZO seed layer on a glass substrate or an n type silicon chip; then adopts hydro-thermal reaction to grow the n type nanowire; and then the NiO layer is plated on the ZnO nanowire to form the heterogeneous pn junction; finally a sputtering method or thermal evaporation method is adopted to make an electrode on the pn junction; and the electrode forms ohmic contact through post annealing and alloying. The pn diode has low forward start voltage, high breakdown reverse voltage, big forward current density, good ultraviolet light sensitive characteristic, as well as simple technology of the preparation method and low cost.
Description
Technical field
The present invention relates to a kind of nano-wire array diode of heterogenous pn junction---n-ZnO nano wire/p-NiO diode of heterogenous pn junction and preparation method thereof belongs to nano material and field of optoelectronic devices.
Background technology
ZnO is a kind of novel II-VI family direct band gap semiconductor material with wide forbidden band.The energy gap of ZnO is 3.37eV in room temperature, emission wavelength is equivalent to black light wavelength (368nm), be suitable for very much making short-wave long light-emitting and light-sensitive device, ZnO is still similar to GaN on energy gap in lattice structure, cell parameter, and have than higher fusing point of GaN and bigger exciton bind energy, have the threshold value of lower luminescence generated by light and stimulated radiation and good electromechanical coupling characteristics, thermal stability and chemical stability again.Thereby great potential is arranged in the application aspect royal purple light-emitting diode, laser and the relative photo electric device thereof.ZnO is considered to the desirable substitution material of GaN.Along with since some unique characteristics of nano material are found, the low dimensional structures of ZnO also expects to have physics and the chemical property that film and body monocrystalline are not had.
Summary of the invention
For improving the performance of traditional plane pn junction diode, the invention provides a kind of diode of heterogenous pn junction based on ZnO nano wire (bar) and preparation method thereof, the n-ZnO/p-NiO diode of heterogenous pn junction of preparation has lower forward cut-in voltage and big forward current density.With respect to traditional plane pn junction diode, its rectification characteristic and photosensitive property are improved.
Technical scheme of the present invention: the nickel oxide heterogeneous pn junction diode of a kind of n-zinc oxide nanowire/p-, at least comprise pn knot and Ohm contact electrode, described pn knot is by the n type ZnO nano wire that grows on n type ZnO film Seed Layer or the ZnO thin film doped Seed Layer; Be packed into insulating material plating NiO material on the ZnO nano wire again in the slit between nano wire earlier, or the direct heterogenous pn junction that on the ZnO nano wire, plates the NiO material and obtain.
Described insulating material is a silicon dioxide.
The preparation method of the nickel oxide heterogeneous pn junction diode of said n-zinc oxide nanowire/p-: at first prepare ZnO or AZO Seed Layer at glass substrate or on n type silicon chip with magnetron sputtering technique; Adopt the hydro-thermal reaction method to grow n type ZnO nano wire then; Plating NiO layer forms heterogenous pn junction on the ZnO nano wire then, or plates NiO layer formation heterogenous pn junction again with the space that the method for whirl coating is gone into filling insulating material earlier between nano wire on the ZnO nano wire; Adopt sputtering method or thermal evaporation to make electrode at last at the pn knot; Wherein, NiO surface sputtering nickel/platinum or nickel/gold electrode or ITO electrode plate indium electrode or aluminium electrode at ZnO or AZO edge; Electrode forms ohmic contact by the after annealing alloying.
Above-mentioned ZnO or AZO Seed Layer are to clean glass substrate or n type silicon chip by conventional semiconductor processing; Carry out the preparation of direct current or rf magnetron sputtering then under the following conditions: target is that ZnO ceramic target or AZO ceramic target, base vacuum degree are better than 10
-3Pa, underlayer temperature is 100～400 ℃, Ar air pressure is that 0.5～5Pa, power bracket 80～150W, sputtering time are 20 minutes～2 hours during deposition.
Being grown in the hydrothermal reaction kettle of above-mentioned nano wire finished, with etc. the hexamethylenetetramine and the zinc nitrate hexahydrate of mol ratio be dissolved in the deionized water, be configured to the equal proportion mixed solution of 0.05～0.5mol/L; 30～60mL mixed solution is put into the hydrothermal reaction kettle kettle, then the glass substrate that is shaped on ZnO or AZO Seed Layer on it or n type silicon chip Seed Layer are faced down and put on the support of solution, sealing is put into high temperature furnace and is heated to 70～130 ℃, constant temperature 5～48h naturally cools to room temperature then; Use rinsed with deionized water, oven dry gets n type ZnO nano wire.
It is the Ni metallic target of 50mm that the present invention adopts diameter, at relative partial pressure of oxygen O
2/ (O
2+ Ar)=60%, the cavity base vacuum degree before the sputter is better than 5 * 10
-4Pa, sputtering pressure are 0.5～1.5Pa, under sputtering power 100～250W condition, and plating NiO film on n type ZnO nano wire, the plated film time is 30～80min, underlayer temperature is 150～400 ℃.
The present invention utilizes ZnO nano wire (bar) array, has been compounded to form heterogenous pn junction structure with the p-NiO film.By to the control of conditions such as ZnO nano wire (bar) growth, NiO film preparation, the optimization of pn junction structure etc., improved the heterogenous pn junction performance, it is improved in the performance aspect the photosensitive detection, gives full play to the ZnO nano rod as the original advantage of monodimension nanometer material in the heterogenous pn junction application facet.
Description of drawings
Fig. 1 is that the present invention has filled SiO
2N-ZnO nano wire/p-NiO film heterogenous pn junction structure schematic diagram (embodiment one);
Fig. 2 is the I-V curve (embodiment one) that the present invention reflects the electrode ohm contact performance;
Fig. 3 is the I-V curve (embodiment one) that the present invention reflects the heterojunction rectification characteristic;
Fig. 4 is that the present invention does not fill SiO
2N-ZnO nano rod/p-NiO film heterogenous pn junction structure schematic diagram (embodiment two to four);
Fig. 5 is the I-V curve (embodiment two) that the present invention reflects the electrode ohm contact performance;
Fig. 6 is the I-V curve (embodiment two) that the present invention reflects the heterojunction rectification characteristic;
Fig. 7 is the I-V curve (embodiment three) that the present invention reflects the electrode ohm contact performance;
Fig. 8 is the I-V curve (embodiment three) that the present invention reflects the heterojunction rectification characteristic;
Fig. 9 is the I-V curve (embodiment four) that the present invention reflects the electrode ohm contact performance;
Figure 10 is the I-V curve (embodiment four) that the present invention reflects the heterojunction rectification characteristic.
Embodiment
The nickel oxide heterogeneous pn junction diode of n-zinc oxide nanowire/p-of the present invention comprises pn knot and Ohm contact electrode at least, and described pn knot is by the n type ZnO nano wire that grows on n type ZnO film Seed Layer or the ZnO thin film doped Seed Layer; Be packed into insulating material plating NiO material on the ZnO nano wire again in the slit between nano wire earlier, or the direct heterogenous pn junction that on the ZnO nano wire, plates the NiO material and obtain.
Its concrete preparation process is as follows:
(1) adopt the cleaning method in the semiconductor technology to clean glass substrate and silicon chip and oven dry;
(2) growth ZnO or AZO Seed Layer: used conditional parameter is when carrying out rf magnetron sputtering: target is that the good AZO ceramic target of ZnO ceramic target or conductivity, base vacuum degree are less than 10
-3Pa, underlayer temperature is 100～400 ℃, Ar air pressure is 0.5～5Pa during deposition, sputtering power scope 80～150W, sputtering time be 20 minutes～120 minutes (as document Guojia Fang, et al., Influence of post-deposition annealingon the properties of transparent conductive nanocrystalline AZO (ZnO:Al) thin filmsprepared by RF magnetron sputtering with highly conductive ceramic target, ThinSolid Films, 2002,418 (2): 156-162);
(3) growth of nano wire (bar): adopt the hydro-thermal reaction synthesis technique (as document Shuang Ma, Guojia Fang, Chun Li, Su Sheng, Linggang Fang, Qiang Fu, Xing-Zhong Zhao, ControllableSynthesis of Vertically Aligned ZnO Nanorod Arrays in Aqueous Solution, Journal ofNanoscience ﹠amp; Nanotechnology, 2006,6 (7), 2062-2066.), being grown in the hydrothermal reaction kettle of nano rod finished, and the main material of reactor is the 1Cr18Ni9Ti stainless steel, and the lining material is a polytetrafluoroethylene, and the volume of still is 100mL.It is pure that predecessor that uses in this experiment and catalyst are commercially available analysis, the hexamethylenetetramine ((CH of mol ratio such as disposes in the experimentation
2)
6N
4, HMT) and zinc nitrate hexahydrate (Zn (NO
3)
26H
2O), it is dissolved in the deionized water, is configured to the equal proportion mixed solution of 0.05～0.5mol/L.Stir 30min under the room temperature.Evenly 20～70mL mixed solution is put into kettle, substrate coating is faced down vertically put on the support of solution then, sealing is put into high temperature furnace and is heated to temperature requiredly, keeps constant temperature to required time, naturally cools to room temperature then.This experiment employing condition is 70～130 ℃ of temperature, time 5～48h.Use rinsed with deionized water, oven dry gets n type ZnO nano wire (bar) array;
(4) preparation of p-NiO: adopting diameter is the Ni metallic target of 50mm.Report (I.Hotovy, J.Huran, J. according to people such as I.Hotovy
Et al., Deposition and properties of nickel oxide filmsproduced by DC reactive magnetron sputtering, Vacuum, 1998,51 (2): 157.), the NiO film of reactive magnetron sputtering preparation, the O in mixed atmosphere
2When ratio raise, the resistivity of film can rise thereupon, and light transmittance then can descend thereupon, to make the NiO film and had higher electric conductivity and light transmission simultaneously, the relative partial pressure of oxygen O that we adopt in order to make
2/ (O
2+ Ar)=30%～40% this is traded off and measures.Cavity base vacuum degree before the sputter is better than 5 * 10
-4Pa, sputtering pressure are 0.5～1.5Pa, sputtering power 100～250W.Before plated film, pre-sputter 10min is to remove the impurity of target material surface.Growing plating NiO film on the substrate of having got well ZnO nano wire (bar).The plated film time is 30～80min, and underlayer temperature is 150～400 ℃.
(5) preparation of electrode: adopt surface and ZnO or the AZO edge making electrode of methods such as sputtering method or thermal evaporation (as: Tang Weizhong work, thin-film material preparation principle, technology and application, metallurgical industry publishing house 1998 front pages) at NiO.NiO surface sputtering platinum or nickel/platinum or nickel/gold electrode or ito transparent electrode, ZnO edge plate indium electrode or aluminium electrode.Electrode forms ohmic contact by the after annealing alloying.
(6) can increase the filling step of insulating barrier between step (3) and (4), promptly with the whirl coating method filling insulating material be gone into space, bottom between the ZnO nano wire, drying forms a layer insulating.The insulating barrier the selection of material is: silicon dioxide.
(7) test
With the ohmic contact characteristic of Keithley 2400 detecting electrodes and the I of diode of heterogenous pn junction-V characteristic (rectification characteristic).
Above-mentioned substrate is glass or silicon chip.
Embodiment one:
1. substrate cleans: adopt normal silicate glass as substrate, be cut into 25mm * 30mm size, adopt alcohol, acetone, deionized water ultrasonic cleaning 30min respectively, dry up with nitrogen gun at last.
2. the growth of Seed Layer: use the method for radio frequency frequency magnetron sputtering to go up deposition AZO film (2) (as the Seed Layer of subsequent growth nano wire) at substrate (1).Target is selected the good AZO ceramic target of conductivity for use, and base vacuum is less than 10
-3Pa, deposition substrate temperature: 300 ℃; Ar air pressure: 1.0Pa during deposition; Sputtering power 140W; Sputtering time: 20min.
3. the growth of nano wire: it is reaction vessel that employing has the teflon-lined high-pressure hydrothermal reaction kettle, and its volume is 100mL.The hexamethylenetetramine ((CH of configuration 0.05mol/L
2)
6N
4, HMT) and zinc nitrate hexahydrate (Zn (NO
3)
26H
2O) mixed solution is put into 20mL in kettle, substrate coating is faced down vertically put on the support of solution, and 90 ℃ kept 7 hours, and promptly obtained ZnO nano rod (3).
4. the filling of insulating barrier adopts the whirl coating method that the colloidal sol of silicon dioxide is packed into space, bottom between the ZnO nano wire, and drying forms a layer insulating (7), and (preparation technology of silicon dioxide gel sees document: side country, Liu Zuli, Yao Kailun, nanometer micropore SiO
2The Sol-Gel preparation of film and porosity control, functional material, 1999,30 (2): 190).
5.p-NiO preparation: the method for using reactive sputtering is deposition NiO film (4) on the long sheet glass that the ZnO nano rod arranged.Target is selected highly purified metal Ni target for use, and base vacuum is less than 10
-3Pa, deposition substrate temperature: 300 ℃; Deposition pressure: 1.0Pa, wherein Ar:O
2=6:4; Power: 80W, sputtering time: 80min.
6. the preparation of electrode: adopt the method for rf magnetron sputtering to prepare Ni/Pt electrode (6) under NiO film surface normal temperature, wherein the sedimentation time of metal Ni is 30s, and the sedimentation time of metal Pt is 200s.The AZO film of substrate surface uses In as electrode (5).The structure chart that obtains at last as shown in Figure 1.
7. test: be ohmic contact with Keithley 2400 detecting electrodes, the contact performance curve as shown in Figure 2.Record this diode of heterogenous pn junction I-the V characteristic curve as shown in Figure 3.
Embodiment two:
1. substrate cleans: adopt normal silicate glass as substrate, be cut into 25mm * 30mm size, adopt alcohol, acetone, deionized water ultrasonic cleaning 30min respectively, dry up with nitrogen gun at last.
2. the growth of Seed Layer: use the method for radio frequency frequency magnetron sputtering to go up deposition AZO film (2) (as the Seed Layer of subsequent growth nano wire) at substrate (1).Target is selected the good AZO ceramic target of conductivity for use, and base vacuum is less than 10
-3Pa, deposition substrate temperature: 100 ℃; Ar air pressure: 2.0Pa during deposition; Power 120W; Sputtering time: 50min.
3. the growth of nano rod: it is reaction vessel that employing has the teflon-lined high-pressure hydrothermal reaction kettle, and its volume is 100mL.The hexamethylenetetramine ((CH of configuration 0.2mol/L
2)
6N
4, HMT) and zinc nitrate hexahydrate (Zn (NO
3)
26H
2O) mixed solution is put into 30mL in kettle, substrate coating is faced down vertically put on the support of solution, and 70 ℃ kept 5 hours, and promptly obtained ZnO nano rod (3).
4.p-NiO preparation: the method for using reactive sputtering is deposition NiO film (4) on the long sheet glass that the ZnO nano rod arranged.Target is selected highly purified metal Ni target for use, and base vacuum is less than 10
-3Pa, deposition substrate temperature: 150 ℃; Deposition pressure: 0.5Pa, wherein Ar:O
2=7:3; Power: 250W, sputtering time: 30min.
5. the preparation of electrode: adopt the method normal temperature of rf magnetron sputtering to prepare Pt electrode (6) down, its sedimentation time is 200s.The AZO film of substrate surface uses In as electrode (5).The structure chart that obtains at last as shown in Figure 4.
6. test: be ohmic contact with Keithley 2400 detecting electrodes, the contact performance curve as shown in Figure 5.Record this diode of heterogenous pn junction I-the V characteristic curve as shown in Figure 6.
Embodiment three:
1. substrate cleans: adopt normal silicate glass as substrate, be cut into 25mm * 30mm size, adopt alcohol, acetone, deionized water ultrasonic cleaning 30min respectively, dry up with nitrogen gun at last.
2. the growth of Seed Layer: use radio frequency method (1) deposition AZO film (2) (as the Seed Layer of subsequent growth nano wire) on substrate of magnetron sputtering frequently.Target is selected the good AZO ceramic target of conductivity for use, and base vacuum is less than 10
-3Pa, deposition substrate temperature: 200 ℃; Ar air pressure: 0.5Pa during deposition; Power 150W; Sputtering time: 20min.
3. the growth of nano rod: it is reaction vessel that employing has the teflon-lined high-pressure hydrothermal reaction kettle, and its volume is 100mL.The hexamethylenetetramine ((CH of configuration 0.5mol/L
2)
6N
4, HMT) and zinc nitrate hexahydrate (Zn (NO
3)
26H
2O) mixed solution is put into 30mL in kettle, substrate coating is faced down vertically put on the support of solution, and 130 ℃ kept 48 hours, and promptly obtained ZnO nano rod (3).
4.p-NiO preparation: the method for using reactive sputtering is deposition NiO film (4) on the long sheet glass that the ZnO nano rod arranged.Target is selected highly purified metal Ni target for use, and base vacuum is less than 10
-3Pa, deposition substrate temperature: 300 ℃; Deposition pressure: 1.5Pa, wherein Ar:O
2=7:3; Power: 250W, sputtering time: 50min.
5. the preparation of electrode: the method that adopts the radio frequency magnetron reactive sputtering is at NiO surface preparation transparent ITO electrode (6).Sputtering target material adopts In/Ga metallic target (wherein In content is 90%), and base vacuum is less than 10
-3Pa, deposition substrate temperature: 300 ℃; Deposition pressure: 1.0Pa, wherein Ar:O
2=7:3; Power: 160W, sputtering time: 20min.The AZO film of substrate surface uses In as electrode (5).The structure chart that obtains at last as shown in Figure 4.
6. test: be ohmic contact with Keithley 2400 detecting electrodes, the contact performance curve as shown in Figure 7.Record this diode of heterogenous pn junction I-the V characteristic curve as shown in Figure 8.
Embodiment four:
1. substrate cleans: adopt n type (100) orientation silicon chip as substrate.Adopt No. 1 liquid commonly used in the semiconductor technology and the method for No. 2 liquid to come cleaning silicon chip.The prescription of No. 1 liquid is: concentrated ammonia liquor: 30% hydrogen peroxide: deionized water=1:2:7 (volume ratio); The prescription of No. 2 liquid is: concentrated hydrochloric acid: 30% hydrogen peroxide: deionized water=1:2:7 (volume ratio).Earlier boil silicon chip, make it boiling for a moment, treat that its cooling cleans up with deionized water again with No. 1 liquid.Put into No. 2 liquid then and boil silicon chip, make it boiling for a moment, treat the last taking-up of its cooling, clean up with deionized water again, at last oven dry.
2. the growth of Seed Layer: method (1) deposition ZnO film (2) (as the Seed Layer of subsequent growth nano wire) on substrate that uses rf magnetron sputtering.Target is selected the ZnO ceramic target for use, and base vacuum is less than 10
-3Pa, deposition substrate temperature: 400 ℃; Ar air pressure: 5.0Pa during deposition; Power 80W; Sputtering time: 120min.
3. the growth of nano rod: it is reaction vessel that employing has the teflon-lined high-pressure hydrothermal reaction kettle, and its volume is 100mL.The hexamethylenetetramine ((CH of configuration 0.1mol/L
2)
6N
4, HMT) and zinc nitrate hexahydrate (Zn (NO
3)
26H
2O) mixed solution is put into 70mL in kettle, substrate coating is faced down vertically put on the support of solution, and 80 ℃ kept 7 hours, and promptly obtained ZnO nano rod (3).
4.p-NiO preparation: the method for using reactive sputtering is deposition NiO film (4) on the long sheet glass that the ZnO nano rod arranged.Target is selected highly purified metal Ni target for use, and base vacuum is less than 10
-3Pa, deposition substrate temperature: 300 ℃; Deposition pressure: 1.0Pa, wherein Ar:O
2=6:4; Power: 100W, sputtering time: 80min.
5. the preparation of electrode: at NiO surface preparation Ni/Au electrode (6), its sedimentation time is 200s under the method normal temperature of employing magnetron sputtering.The ZnO film evaporating Al of substrate surface is as electrode (5).The structure chart that obtains at last as shown in Figure 4.
6. test: be ohmic contact with Keithley 2400 detecting electrodes, the contact performance curve as shown in Figure 9.Record this diode of heterogenous pn junction I-the V characteristic curve as shown in figure 10.
Claims (6)
1, the nickel oxide heterogeneous pn junction diode of a kind of n-zinc oxide nanowire/p-comprises pn knot and Ohm contact electrode at least, it is characterized in that: described pn knot is by the n type ZnO nano wire that grows on n type ZnO film Seed Layer or the ZnO thin film doped Seed Layer; Be packed into insulating material plating NiO material on the ZnO nano wire again in the slit between nano wire earlier, or the direct heterogenous pn junction that on the ZnO nano wire, plates the NiO material and obtain.
2, the nickel oxide heterogeneous pn junction diode of n-zinc oxide nanowire/p-according to claim 1, it is characterized in that: described insulating material is a silicon dioxide.
3, the preparation method of claim 1 or the nickel oxide heterogeneous pn junction diode of 2 described n-zinc oxide nanowire/p-is characterized in that: at first prepare ZnO or AZO Seed Layer at glass substrate or on n type silicon chip with magnetron sputtering technique; Adopt the hydro-thermal reaction method to grow n type ZnO nano wire then; Plating NiO layer forms heterogenous pn junction on the ZnO nano wire then, or plates NiO layer formation heterogenous pn junction again with the space that the method for whirl coating is gone into filling insulating material earlier between nano wire on the ZnO nano wire; Adopt sputtering method or thermal evaporation to make electrode at last at the pn knot; Wherein, NiO surface sputtering nickel/platinum or nickel/gold electrode or ITO electrode plate indium electrode or aluminium electrode at ZnO or AZO edge; Electrode forms ohmic contact by the after annealing alloying.
4, preparation method according to claim 3 is characterized in that: ZnO or AZO Seed Layer are to clean glass substrate or n type silicon chip by conventional semiconductor processing; Carry out the preparation of direct current or rf magnetron sputtering then under the following conditions: target is that ZnO ceramic target or AZO ceramic target, base vacuum degree are better than 10
-3Pa, underlayer temperature is 100～400 ℃, Ar air pressure is that 0.5～5Pa, power bracket 80～150W, sputtering time are 20 minutes～2 hours during deposition.
5, preparation method according to claim 3, it is characterized in that: being grown in the hydrothermal reaction kettle of above-mentioned nano wire finished, with etc. the hexamethylenetetramine and the zinc nitrate hexahydrate of mol ratio be dissolved in the deionized water, be configured to the equal proportion mixed solution of 0.05～0.5mol/L; 30～60mL mixed solution is put into the hydrothermal reaction kettle kettle, then the glass substrate that is shaped on ZnO or AZO Seed Layer on it or n type silicon chip Seed Layer are faced down and put on the support of solution, sealing is put into high temperature furnace and is heated to 70～130 ℃, constant temperature 5～48h naturally cools to room temperature then; Use rinsed with deionized water, oven dry gets n type ZnO nano wire.
6, according to claim 3 or 4 or 5 described preparation methods, it is characterized in that: adopting diameter is the Ni metallic target of 50mm, at relative partial pressure of oxygen O
2/ (O
2+ Ar)=60%, the cavity base vacuum degree before the sputter is better than 5 * 10
-4Pa, sputtering pressure are 0.5～1.5Pa, under sputtering power 100～250W condition, and plating NiO film on n type ZnO nano wire, the plated film time is 30～80min, underlayer temperature is 150～400 ℃.
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2008
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