CN101413105B - Membrane thickness modulation method for optimizing ZnO film field emission characteristic - Google Patents
Membrane thickness modulation method for optimizing ZnO film field emission characteristic Download PDFInfo
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- CN101413105B CN101413105B CN2008101511795A CN200810151179A CN101413105B CN 101413105 B CN101413105 B CN 101413105B CN 2008101511795 A CN2008101511795 A CN 2008101511795A CN 200810151179 A CN200810151179 A CN 200810151179A CN 101413105 B CN101413105 B CN 101413105B
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Abstract
The invention discloses a method for modulating the thickness of the film to optimize the characteristic of field emission of a ZnO film. The method comprises the following steps: Si is selected as an underlayer; a metal zinc target is used as a target material; the underlayer is boiled through a mixed solution of ammonia, hydrogen peroxide and deionized water and is cleaned through the deionized water; the underlayer is subjected to supersonic cleaning through a toluene solution, an acetone solution and an ethanol solution sequentially; the underlayer is sent to a radio frequency magnetic control sputtering device and is vacuumized; the vacuum degree of the back of the underlayer, the proportion of Ar to O2, the working pressure, the cardinal distance of the target, the sputtering power and the temperature of the underlayer are adjusted to proper values; and the ZnO films with different thicknesses are obtained through changing the sputtering time for film plating. Through controlling the length of sputtering time, the thickness of the ZnO film is controlled to obtain the thickness value of the film with optimal field emission performance; therefore, the optimal field emission performance reaches the level of actual application. The optimized design is beneficial for shortening the development period of a field emission device of the film, saves research and development cost, and has obvious application prospect and potential economic benefit.
Description
Technical field
The invention belongs to technical field of flat panel display, relate to a kind of thickness modulation method, especially a kind of thickness modulation method of optimizing the ZnO film field emission characteristic.
Background technology
" emission " has in vacuum microelectronic device very extensively and important use, and like EED, great-power electronic emissive source etc., and one of technology of these device most criticals is exactly the selection and the manufacture craft of negative electrode.Therefore field emmision material has become a hot fields in the microelectronic material research.
Wide bandgap semiconductor ZnO has the characteristic of numerous excellences, especially: good chemicalstability, little even negative electron affinity; High thermal conductivity; Oxidation-resistance, high thermal resistance, big breaking down field strength and high carrier mobility; Big transmitter current makes its emission research field on the scene gain great popularity.But the research of ZnO filed emission cathode material mainly concentrates on the monodimension nanometer material aspect of chemical process preparation at present, and the research physical method prepares the field emission performance of ZnO film and reports but seldom.Because the film of magnetron sputtering method preparation has many advantages with respect to chemical process; Good such as tack, compact structure, pin hole is few and purity is higher, good uniformity; Realize big area easily; The more important thing is that its transmitter current is even, the device lifetime of processing is long, and is easy to other microelectronic device integrated.So the ZnO film field emission characteristic of research magnetron sputtering method preparation is significant.Moreover; The research of in the past launching for the semiconductor film field; More concern be of the influences of different thin-film materials for its field emission performance, and shorter mention membrane structure itself is for the influence of field emission performance, like film crystal particle scale, multi-layer film structure, film thickness etc.In fact, film thickness is very significant for the influence of field emission performance, finds the best film thickness value of field emission performance, can shorten the construction cycle of feds greatly, saves R&D costs, and tangible application prospect and potential economic benefit are arranged.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art; A kind of thickness modulation method of optimizing the ZnO film field emission characteristic is provided; Thereby this method is the thickness through the length control ZnO film of control sputtering time; Obtain the best film thickness value of field emission performance, this optimal design method helps to shorten the construction cycle of thin film field ballistic device, saves R&D costs.
The objective of the invention is to solve through following technical scheme:
The thickness modulation method of this optimization ZnO film field emission characteristic is characterized in that, comprises the steps:
1). select Si to do substrate, the metallic zinc target is done target;
2) boil substrate Si with ammoniacal liquor, ydrogen peroxide 50 and deionized mixed solution, boil 10～40min after, with deionized water substrate is rinsed well; Described mixeding liquid volume is than being ammoniacal liquor: ydrogen peroxide 50: deionized water=1: 2: 5;
3) use analytically pure toluene, acetone and ethanolic soln ultrasonic cleaning substrate Si successively, scavenging period is 10～20min, then with drying up with the HF acid of high pure nitrogen with substrate surface behind HF soak 2～10min again;
4). install the zinc target, and substrate Si is sent into the rf magnetron sputtering appearance;
5). vacuumize vacuum tightness, Ar and O at the bottom of the back of the body that configures
2Under ratio, operating air pressure, target-substrate distance, power and the underlayer temperature, the change sputtering time carries out plated film and obtains product of the present invention.
Wherein above-mentioned substrate is n type (100) Si, and zinc target purity is 99.9%.
Wherein above-mentioned mixeding liquid volume is than being ammoniacal liquor: ydrogen peroxide 50: deionized water=1: 2: 5, boiling time are 30min, then rinse well with deionized water.
The wherein above-mentioned ultrasonic cleaning time is 15min respectively, and the substrate use concentration after the cleaning is 3% HF soak 5min, dries up with the HF acid of high pure nitrogen with substrate surface then.
Vacuum is 8 * 10-2Pa～5 * 10-3Pa, Ar and O at the bottom of the wherein above-mentioned back of the body
2Volume ratio be 9: 5, operating air pressure is 0.2Pa, target-substrate distance is 40mm, sputtering power is 50W, underlayer temperature is 20 ℃, sputtering time is respectively 3,5,7,9,15 and 30min.
The thickness modulation method of optimization ZnO film field emission characteristic of the present invention; Thereby technical thought is the thickness through the length control ZnO film of control sputtering time; Obtain the best film thickness value of field emission performance, and this best field emission performance has reached the level of practical application.This optimization design helps to shorten the construction cycle of thin film field ballistic device, saves R&D costs, and tangible application prospect and potential economic benefit are arranged.
Description of drawings
Fig. 1 is the X ray diffracting spectrum (XRD) of different thickness ZnO film;
Fig. 2 is the atomic force micrograph (AFM) of different thickness ZnO film,
Wherein: Fig. 2 (a) is 20nm; Fig. 2 (b) is 30nm; Fig. 2 (c) is 40nm; Fig. 2 (d) is 55nm; Fig. 2 (e) is 85nm; Fig. 2 (f) is 140nm;
Fig. 3 is the field emission curve (J-E) of ZnO film;
Fig. 4 is the corresponding FN curve of ZnO film current density curve;
Fig. 5 opens the change curve of field intensity with thickness for ZnO film.
Embodiment
The preparation of ZnO cathode thin film is carried out according to following steps:
1) select n type (100) Si to do substrate, purity is that 99.9% metallic zinc target is done target;
2) use volume ratio to be ammoniacal liquor: ydrogen peroxide 50: after the mixed solution of de-ionized=1: 2: 5 boils substrate 30min, substrate to be rinsed well with deionized water;
3) use analytically pure toluene, acetone and ethanolic soln ultrasonic cleaning substrate successively, scavenging period is 15min, then with drying up with the HF acid of high pure nitrogen with substrate surface behind 3% the HF soak 5min again;
4) install the zinc target, and substrate Si is sent into the rf magnetron sputtering appearance;
5) vacuumize, back of the body end vacuum is 8 * 10-2Pa, Ar and O
2Volume ratio be 9: 5, operating air pressure is 0.2Pa, target-substrate distance is 40mm, sputtering power is 50W, underlayer temperature is 20 ℃, sputtering time is 3min, film thickness is 20nm.
1) select n type (100) Si to do substrate, purity is that 99.9% metallic zinc target is done target;
2) use volume ratio to be ammoniacal liquor: ydrogen peroxide 50: after the mixed solution of de-ionized=1: 2: 5 boils substrate 30min, substrate to be rinsed well with deionized water;
3) use analytically pure toluene, acetone and ethanolic soln ultrasonic cleaning substrate successively, scavenging period is 15min, then with drying up with the HF acid of high pure nitrogen with substrate surface behind 3% the HF soak 5min again;
4) install the zinc target, and substrate Si is sent into the rf magnetron sputtering appearance;
5) vacuumize, back of the body end vacuum is 3 * 10-3Pa, Ar and O
2Volume ratio be 9: 5, operating air pressure is 0.2Pa, target-substrate distance is 40mm, sputtering power is 50W, underlayer temperature is 20 ℃, sputtering time is 5min, film thickness is 30nm.
1) select n type (100) Si to do substrate, purity is that 99.9% metallic zinc target is done target;
2) use volume ratio to be ammoniacal liquor: ydrogen peroxide 50: after the mixed solution of de-ionized=1: 2: 5 boils substrate 30min, substrate to be rinsed well with deionized water;
3) use analytically pure toluene, acetone and ethanolic soln ultrasonic cleaning substrate successively, scavenging period is 15min, then with drying up with the HF acid of high pure nitrogen with substrate surface behind 3% the HF soak 5min again;
4) install the zinc target, and substrate Si is sent into the rf magnetron sputtering appearance;
5) vacuumize, back of the body end vacuum is 1 * 10-3Pa, Ar and O
2Volume ratio be 9: 5, operating air pressure is 0.2Pa, target-substrate distance is 40mm, sputtering power is 50W, underlayer temperature is 20 ℃, sputtering time is 7min, film thickness is 40nm.
1) select n type (100) Si to do substrate, purity is that 99.9% metallic zinc target is done target;
2) use volume ratio to be ammoniacal liquor: ydrogen peroxide 50: after the mixed solution of de-ionized=1: 2: 5 boils substrate 30min, substrate to be rinsed well with deionized water;
3) use analytically pure toluene, acetone and ethanolic soln ultrasonic cleaning substrate successively, scavenging period is 15min, then with drying up with the HF acid of high pure nitrogen with substrate surface behind 3% the HF soak 5min again;
4) install the zinc target, and substrate Si is sent into the rf magnetron sputtering appearance;
5) vacuumize, back of the body end vacuum is 3 * 10-3Pa, Ar and O
2Volume ratio be 9: 5, operating air pressure is 0.2Pa, target-substrate distance is 40mm, sputtering power is 50W, underlayer temperature is 20 ℃, sputtering time is 9min, film thickness is 55nm.
Embodiment 5
1) select n type (100) Si to do substrate, purity is that 99.9% metallic zinc target is done target;
2) use volume ratio to be ammoniacal liquor: ydrogen peroxide 50: after the mixed solution of de-ionized=1: 2: 5 boils substrate 30min, substrate to be rinsed well with deionized water;
3) use analytically pure toluene, acetone and ethanolic soln ultrasonic cleaning substrate successively, scavenging period is 15min, then with drying up with the HF acid of high pure nitrogen with substrate surface behind 3% the HF soak 5min again;
4) install the zinc target, and substrate Si is sent into the rf magnetron sputtering appearance;
5) vacuumize, back of the body end vacuum is 5 * 10-3Pa, Ar and O
2Volume ratio be 9: 5, operating air pressure is 0.2Pa, target-substrate distance is 40mm, sputtering power is 50W, underlayer temperature is 20 ℃, sputtering time is 15min, film thickness is 85nm.
1) select n type (100) Si to do substrate, purity is that 99.9% metallic zinc target is done target;
2) use volume ratio to be ammoniacal liquor: ydrogen peroxide 50: after the mixed solution of de-ionized=1: 2: 5 boils substrate 30min, substrate to be rinsed well with deionized water;
3) use toluene, acetone and ethanolic soln ultrasonic cleaning substrate successively, scavenging period is 15min, then with drying up with the HF acid of high pure nitrogen with substrate surface behind 3% the HF soak 5min again;
4) install the zinc target, and substrate Si is sent into the rf magnetron sputtering appearance;
5) vacuumize, back of the body end vacuum is 2 * 10-3Pa, Ar and O
2Volume ratio be 9: 5, operating air pressure is 0.2Pa, target-substrate distance is 40mm, sputtering power is 50W, underlayer temperature is 20 ℃, sputtering time is 30min, film thickness is 140nm.
Below in conjunction with accompanying drawing the present invention is done and to describe in further detail:
The optimization of ZnO film field emission characteristic (thickness modulation method):
Prepared film is (002) orientation among Fig. 1; The surfaceness RMS that surfaceness atomic force micrograph such as Fig. 2 show is respectively: 0.77nm, 0.5nm, 0.4nm, 0.82nm, 0.92nm and 1.6nm; The field emission is along with change curve such as Fig. 3 of field intensity show that thickness is that the sample field emitting performance of 40nm obviously is superior to other films, and it is minimum that it opens field intensity, is 0.4V/ μ m, and current density reached maximum 0.037A/cm when field intensity was 3.4V/ μ m
2, reached the level of practical application; FN curve such as Fig. 4 all are approximately straight line, show that all samples is electronics and wears emission then; When thickness changed from 20nm to 140nm, the unlatching field intensity of film increases afterwards earlier and reduces, and was as shown in Figure 5, and the thin film field emitting performance of 40nm is best.
Thereby, obtained the best film thickness value of field emission performance, and this best field emission performance has reached the level of practical application so pass through the thickness of the length control ZnO film of control sputtering time.This optimization design helps to shorten the construction cycle of thin film field ballistic device, saves R&D costs, and tangible application prospect and potential economic benefit are arranged.
Claims (2)
1. a thickness modulation method of optimizing the ZnO film field emission characteristic is characterized in that, this method comprises the steps:
1) select Si to do substrate, the metallic zinc target is done target, and said substrate is (100) Si of n type, and said zinc target purity is 99.9%;
2) boil substrate Si with ammoniacal liquor, ydrogen peroxide 50 and deionized mixed solution, boil 10 ~ 40min after, with deionized water substrate is rinsed well; Described mixeding liquid volume is than being ammoniacal liquor: ydrogen peroxide 50: deionized water=1:2:5;
3) use analytically pure toluene, acetone and ethanolic soln ultrasonic cleaning substrate Si successively, scavenging period is 10 ~ 20min, dries up with the HF acid of high pure nitrogen with substrate surface after using HF soak 2 ~ 10min then again;
4) install the zinc target, and substrate Si is sent into the rf magnetron sputtering appearance;
5) vacuumize, adjustment back of the body end vacuum tightness is 8 * 10
-2Pa ~ 5 * 10
-3Pa, Ar and O
2Volume ratio be 9:5, operating air pressure is 0.2 Pa, target-substrate distance is 40mm, sputtering power is 50W, underlayer temperature is 20 ℃, sputtering time is 7 min, obtains the ZnO film that thickness is 40 nm.
2. the thickness modulation method of optimization ZnO film field emission characteristic according to claim 1 is characterized in that: the time of said ultrasonic cleaning substrate Si is 15 min, and the volumetric concentration of described HF acid is 3%, and the described HF soak time is 5min.
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