CN102653863A - Preparation method of Ru-Li codoped nickel oxide film - Google Patents
Preparation method of Ru-Li codoped nickel oxide film Download PDFInfo
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- CN102653863A CN102653863A CN201210143328XA CN201210143328A CN102653863A CN 102653863 A CN102653863 A CN 102653863A CN 201210143328X A CN201210143328X A CN 201210143328XA CN 201210143328 A CN201210143328 A CN 201210143328A CN 102653863 A CN102653863 A CN 102653863A
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Abstract
The invention belongs to the field of semiconductors and devices, and particularly relates to a preparation method of an Ru-Li codoped nickel oxide film, which comprises the following steps: preparing an Ru-Li codoped nickel sol, carrying out spin coating on the Ru-Li codoped nickel oxide sol on the substrate, and carrying out heat treatment on the film at 300-600 DEG C in air for 1-2 hours, thereby obtaining the Ru-Li codoped nickel oxide film. The Ru-Li codoped nickel oxide film has favorable repeatable resistance switch characteristic, and the switch phenomenon can be observed after continuously sweeping 9 times. Compared with the doped NiO film and the intrinsic NiO film, the Ru-Li codoped nickel oxide film has higher switch ratio, and improves the signal to noise ratio of the resistor memory device.
Description
Technical field
The invention belongs to semi-conductor and devices field, be specifically related to a kind of preparation method of Ru-Li co-doped nickel oxide film.
Backgroundfield
The storer that uses at present mainly contains volatile random access memory and non-volatility memorizer; Fast but the data storage of outage back of former data storage speed can disappear; Still can continue to preserve data after latter's outage, it is particularly important therefore to develop novel non-volatility memorizer.The more non-volatility memorizer of development in recent years mainly contains ferroelectric memory, magneticstorage, phase transition storage and resistance-variable storing device, and wherein resistance-variable storing device is simple to prepare, storage density is high, data hold time is long, receive much concern with the compatible advantage such as get well of traditional cmos process.NiO is a kind of transition metal binary oxide of the 3d of having electronic structure, and the energy gap under the room temperature is 3.6-4.0eV, has insulating property, but film can produce Ni in the actual fabrication process
2+The room makes film present broad stopband P-type semiconductor characteristic.The NiO film is a vitreous state in the visible range, has good optical and electrology characteristic, has been widely used in fields such as catalysis, air-sensitive sensing, photoelectricity conversion and battery electrode.The NiO film also has the resistance switch characteristic, in the resistance-variable storing device field, good application prospects is arranged, and is considered to replace the novel nonvolatile memory of traditional flash storer, therefore obtains investigator's extensive concern.
In order to make nickel oxide material obtain practical application in the resistance-variable storing device field, people once attempted with different element doping nickel oxide films to improve its resistance switch characteristic, like switch stability, anelasticity and the thermostability of Li, Na doping can raising film; Al mixes can increase the persistence of thin film switch action; Nb mixes can reduce V
SETThe distribution of voltage; W mixes can change thin film switch polarity.Wherein high valence elements such as doped with Al, Ti, Nb are to make film by the conduction of P-type conduction becoming N-type, increase Ni in the film
0Promote the formation of conductive wire, thereby improve the switching characteristic of film.In recent years, occur two or more element codopeds again and improve the nickel oxide The Characteristic Study, prepare nickel oxide film like the Li-Ti codoped.Though the above-mentioned various doping of studying have advantages such as thin film switch high stability and anelasticity; But alloying element is not improved the switching threshold voltage and the on-off ratio of NiO film; And threshold voltage and on-off ratio are the significant parameters that the resistance of reflection storer becomes characteristic: threshold voltage is the embodiment of power consumption; Thereby the purpose that the threshold voltage that reduces resistance change device reaches the reduction power consumption is all being sought by each study group; On-off ratio then is the external manifestation of memory property, also is being the effort of raising on-off ratio both at home and abroad.Though the research report that improves NiO thin film switch ratio through the preparation heterojunction structure is arranged, and its preparation method is complicated, complex steps.
Summary of the invention
To the problem that existing NiO film exists, the present invention provides a kind of preparation method of Ru-Li co-doped nickel oxide film,
Through preparation Ru-Li codoped nickel sol, process steps such as cleaning substrate, spin coating plated film and thermal treatment, preparation has the good NiO film of high on-off ratio.
The technical scheme of realization the object of the invention is carried out according to following steps:
(1) takes by weighing 1.24-1.25gNi (CH
3COO)
24H
2O is dissolved in the 25mL EGME, adds and Ni (CH
3COO)
24H
2The equimolar thanomin of O, after stirring 30-40 min under 60-70 ℃ the water bath condition, adding mass ratio is 3: RuCl (1-5)
33H
2O and CH
3COOLi continues to stir 90-100 min, obtains the nickel oxide colloidal sol of Ru-Li codoped, with its still aging 24-48h in air;
(2) substrate is cleaned 10-15min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple successively, with the absolute ethyl alcohol flushing, on heating platform, dry afterwards again;
(3) with sol evenning machine the Ru-Li co-doped nickel oxide colloidal sol that obtains after still aging is carried out spin-coating on substrate; Under the rotating speed of 800-1000r/min, drip colloidal sol 5-10s earlier to substrate; Then substrate is rotated 30-40 s under the rotating speed of 3000-3500r/min; Substrate surface forms wet film, and substrate is placed on the heating platform heating, drying under 100-120 ℃ of temperature, repeats above-mentionedly to be coated with membrane process twice;
(4) at last with the temperature rise rate of 6 ℃/min, under 300-600 ℃ of condition in air to film thermal treatment 1-2 h, obtain Ru-Li co-doped nickel oxide film.
Described substrate is Si substrate, ITO conductive glass substrate or glass substrate.
Ultimate principle of the present invention is: Ru is good memory metal and extinction metallic element; Can make the film high-resistance resistors bigger; Thereby reach the effect that improves on-off ratio; And Li has advantages such as improving switch stability, so Ru-Li co-doped nickel oxide film has good repeated resistance switch characteristic, has effectively improved the on-off ratio of nickel oxide film.
Compared with prior art, the technical scheme of the present invention's proposition has following beneficial effect:
1. preparation method of the present invention adopts sol-gel method, and depositing device is simple, cost is low, film composition easy to control;
2. the film surface of the present invention's preparation is smooth, compactness good, and a little crackle is only arranged on the edge of;
3. the Ru-Li codoped NiO film of the present invention's preparation has good repeated resistance switch characteristic, and continuous sweep is all observed on-off phenomenon 9 times;
4. the present invention only compares on-off ratio through the NiO film of the preparation of mixing with intrinsic NiO film and increases, and has improved the SNR of resistance memory.
Description of drawings
Fig. 1 is a process flow diagram of the present invention;
Fig. 2 is the volt-ampere characteristic test set figure of the Ru-Li codoped NiO film of the embodiment of the invention 1 preparation;
Fig. 3 is the I-V rational curve of the Ru-Li codoped NiO film of the embodiment of the invention 1 preparation, and wherein illustration is 9 corresponding threshold voltages of continuous sweep;
Fig. 4 is threshold voltage and the on-off ratio of Ru-Li codoped NiO thin-film device under different annealing temperature that the present invention prepares;
Fig. 5 is the transmittance spectrum of the Ru-Li codoped NiO film for preparing of the present invention;
Fig. 6 is the absorbance spectrum of the Ru-Li codoped NiO film for preparing of the present invention;
Fig. 7 is the scanning electron microscope diagram sheet of the Ru-Li codoped NiO film for preparing of the present invention;
Fig. 8 is the scanning electron microscope diagram sheet of the Ru-Li codoped NiO film edge for preparing of the present invention.
Embodiment
Chemical reagent used in the embodiment of the invention is analytical pure;
The embodiment of the invention is used X ' Pert Pro type X-ray diffractometer (Cu
K α) sample is carried out XRD analysis; Characterize the surface topography of sample through SSX-550 type sem; Optical characteristics through UV759S type ultra-violet and visible spectrophotometer specimen; Through liquid gallium indium microdrop technique sample is carried out volt-ampere (I-V) characteristic test, obtain the electrology characteristic of codoped NiO film.
Further illustrate embodiment of the present invention through embodiment, but be not only to be confined to embodiment at present.
(1) takes by weighing 1.24g Ni (CH
3COO)
24H
2O is dissolved in the 25mL EGME, adds and Ni (CH
3COO)
24H
2The equimolar thanomin of O after stirring 40 min under 60 ℃ the water bath condition, adds the RuCl of mass ratio 3:5
33H
2O and CH
3COOLi continues to stir 100 min, obtains the nickel oxide colloidal sol of Ru-Li codoped, Ni in the colloidal sol
2+Concentration is 0.2 mol/L, with colloidal sol still aging 24h in air;
(2) select the ito glass conductive substrate for use, substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, with the absolute ethyl alcohol flushing, on heating platform, dry afterwards again;
(3) with sol evenning machine the Ru-Li co-doped nickel oxide colloidal sol that obtains is carried out spin-coating on substrate; Under the rotating speed of 800r/min, drip colloidal sol 5s earlier to substrate; Then substrate is rotated 40 s under the rotating speed of 3000r/min; Form wet film on the substrate, substrate is placed on the heating platform in 120 ℃ of heating, dryings, the above-mentioned membrane process that is coated with repeats twice;
(4) at last with the temperature rise rate of 6 ℃/min, under 500 ℃ of conditions in air to film thermal treatment 1.5h, obtain Ru-Li co-doped nickel oxide film.
Adopt volt-ampere characteristic test set shown in Figure 2 that film is carried out the volt-ampere characteristic test; Its current-voltage curve is as shown in Figure 3; Can find out that by figure Ru-Li codoped NiO film has good bipolar resistance switch characteristic, and the film same point has been carried out 9 continuous sweep; In scanning process, all observe on-off phenomenon, illustration is 9 pairing threshold voltages of on-off phenomenon among Fig. 3;
To the Ru-Li co-doped nickel oxide thin film switch specificity analysis that makes, can find out by Fig. 4,500 ℃ of film resistance change switching characteristic the bests that annealing obtains, its threshold voltage less (about 1V), on-off ratio be big (about 400);
Ru-Li co-doped nickel oxide film to making carries out Optical characteristics, and its transmittance spectrum is as shown in Figure 5, from figure can find out that annealing temperature is 500 ℃ the time codoped NiO film transmittance up to more than 85%.
(1) takes by weighing 1.25gNi (CH
3COO)
24H
2O is dissolved in the 25mL EGME, adds and Ni (CH
3COO)
24H
2The equimolar thanomin of O after stirring 30 min under 70 ℃ the water bath condition, adds the RuCl of mass ratio 3:4
33H
2O and CH
3COOLi continues to stir 90 min, obtains the nickel oxide colloidal sol of Ru-Li codoped, Ni in the colloidal sol
2+Concentration is 0.2 mol/L, with colloidal sol still aging 48h in air;
(2) select glass substrate for use, substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, with the absolute ethyl alcohol flushing, on heating platform, dry afterwards again;
(3) with sol evenning machine the Ru-Li co-doped nickel oxide colloidal sol that obtains is carried out spin-coating on substrate; Under the rotating speed of 800r/min, drip colloidal sol 5s earlier to substrate; Then substrate is rotated 30s under the rotating speed of 3500r/min; Form wet film on the substrate, the wet film that forms is placed on the heating platform in 120 ℃ of heating, dryings, the above-mentioned membrane process that is coated with repeats twice;
(4) at last with the temperature rise rate of 6 ℃/min, under 400 ℃ of conditions in air to film thermal treatment 1.5h, obtain Ru-Li co-doped nickel oxide film.
Ru-Li co-doped nickel oxide film to making carries out Optical characteristics, and its absorbancy collection of illustrative plates is as shown in Figure 6, can be known by figure, and the film absorbancy is maximum during 400 ℃ of annealing.
(1) takes by weighing 1.24gNi (CH
3COO)
24H
2O is dissolved in the 25mL EGME, adds and Ni (CH
3COO)
24H
2The equimolar thanomin of O after stirring 35 min under 65 ℃ the water bath condition, adds the RuCl of mass ratio 3:4
33H
2O and CH
3COOLi continues to stir 95 min, obtains the nickel oxide colloidal sol of Ru-Li codoped, Ni in the colloidal sol
2+Concentration is 0.2 mol/L, with colloidal sol still aging 24h in air;
(2) select the Si substrate for use, substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, with the absolute ethyl alcohol flushing, on heating platform, dry afterwards again;
(3) with sol evenning machine the Ru-Li co-doped nickel oxide colloidal sol that obtains is carried out spin-coating on substrate; Under the rotating speed of 900r/min, drip colloidal sol 8s earlier to substrate; Then substrate is rotated 35s under the rotating speed of 3250r/min; The wet film that forms is placed on the heating platform in 110 ℃ of heating, dryings, and the above-mentioned membrane process that is coated with repeats twice;
(4) at last with the temperature rise rate of 6 ℃/min, under 300 ℃ of conditions in air to film thermal treatment 2h, obtain Ru-Li co-doped nickel oxide film.
Ru-Li co-doped nickel oxide film to making carries out electron microscope scanning; The picture that obtains is like Fig. 7, shown in 8; By the visible film surface compact structure of figure, the size of particles size evenly, only the edge owing to centrifugation make its film thicker in heat treatment process unbalance stress ftracture.
(1) takes by weighing 1.25gNi (CH
3COO)
24H
2O is dissolved in the 25mL EGME, adds and Ni (CH
3COO)
24H
2The equimolar thanomin of O after stirring 30 min under 70 ℃ the water bath condition, adds the RuCl of mass ratio 3:4
33H
2O and CH
3COOLi continues to stir 90min, obtains the nickel oxide colloidal sol of Ru-Li codoped, Ni in the colloidal sol
2+Concentration is 0.2 mol/L, with colloidal sol still aging 24h in air;
(2) select the Si substrate for use, substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, with the absolute ethyl alcohol flushing, on heating platform, dry afterwards again;
(3) with sol evenning machine the Ru-Li co-doped nickel oxide colloidal sol that obtains is carried out spin-coating on substrate; Under the rotating speed of 800r/min, drip colloidal sol 10s earlier to substrate; Then substrate is rotated 30 s under the rotating speed of 3000r/min; Form wet film on the substrate, the wet film that forms is placed on the heating platform in 120 ℃ of heating, dryings, the above-mentioned membrane process that is coated with repeats twice;
(4) at last with the temperature rise rate of 6 ℃/min, under 600 ℃ of conditions in air to film thermal treatment 1h, obtain Ru-Li co-doped nickel oxide film.
Embodiment 5
(1) takes by weighing 1.25gNi (CH
3COO)
24H
2O is dissolved in the 25mL EGME, adds and Ni (CH
3COO)
24H
2The equimolar thanomin of O after stirring 40 min under 60 ℃ the water bath condition, adds the RuCl of mass ratio 3:1
33H
2O and CH
3COOLi continues to stir 100 min, obtains the nickel oxide colloidal sol of Ru-Li codoped, Ni in the colloidal sol
2+Concentration is 0.2 mol/L, with colloidal sol still aging 36h in air;
(2) select ITO conductive glass substrate for use, substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, with the absolute ethyl alcohol flushing, on heating platform, dry afterwards again;
(3) with sol evenning machine the Ru-Li co-doped nickel oxide colloidal sol that obtains is carried out spin-coating on substrate; Under the rotating speed of 800r/min, drip colloidal sol 10s earlier to substrate; Under the rotating speed of 3000r/min, rotate 30 s then; The wet film that forms is placed on the heating platform in 120 ℃ of heating, dryings, have certain thickness for making film, the above-mentioned membrane process that is coated with repeats twice;
(4) at last with the temperature rise rate of 6 ℃/min, under 500 ℃ of conditions in air to film thermal treatment 1h, obtain Ru-Li co-doped nickel oxide film.
Embodiment 6
(1) takes by weighing 1.24gNi (CH
3COO)
24H
2O is dissolved in the 25mL EGME, adds and Ni (CH
3COO)
24H
2The equimolar thanomin of O after stirring 30-40 min under 60-70 ℃ the water bath condition, adds the RuCl of mass ratio 1:1
33H
2O and CH
3COOLi continues to stir 90 min, obtains the nickel oxide colloidal sol of Ru-Li codoped, Ni in the colloidal sol
2+Concentration is 0.2 mol/L, with colloidal sol still aging 24h in air;
(2) select glass substrate for use, substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, with the absolute ethyl alcohol flushing, on heating platform, dry afterwards again;
(3) with sol evenning machine the Ru-Li co-doped nickel oxide colloidal sol that obtains is carried out spin-coating on substrate; Under the rotating speed of 1000r/min, drip colloidal sol 5s earlier to substrate; Then substrate is rotated 30 s under the rotating speed of 3000r/min; Form wet film on the substrate, the wet film that forms is placed on the heating platform in 120 ℃ of heating, dryings, the above-mentioned membrane process that is coated with repeats twice;
(4) at last with the temperature rise rate of 6 ℃/min, under 500 ℃ of conditions in air to film thermal treatment 1.5h, obtain Ru-Li co-doped nickel oxide film.
Embodiment 7
(1) takes by weighing 1.25gNi (CH
3COO)
24H
2O is dissolved in the 25mL EGME, adds and Ni (CH
3COO)
24H
2The equimolar thanomin of O after stirring 30 min under 70 ℃ the water bath condition, adds the RuCl of mass ratio 3:4
33H
2O and CH
3COOLi continues to stir 100 min, obtains the nickel oxide colloidal sol of Ru-Li codoped, Ni in the colloidal sol
2+Concentration is 0.2 mol/L, with colloidal sol still aging 24h in air;
(2) select the Si substrate for use, substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, with the absolute ethyl alcohol flushing, on heating platform, dry afterwards again;
(3) with sol evenning machine the Ru-Li co-doped nickel oxide colloidal sol that obtains is carried out spin-coating on substrate; Under the rotating speed of 800r/min, drip colloidal sol 5s earlier to substrate; Then substrate is rotated 40 s under the rotating speed of 3500r/min; The wet film that forms is placed on the heating platform in 120 ℃ of heating, dryings, and the above-mentioned membrane process that is coated with repeats twice;
(4) at last with the temperature rise rate of 6 ℃/min, under 500 ℃ of conditions in air to film thermal treatment 1h, obtain Ru-Li co-doped nickel oxide film.
Claims (2)
1. the preparation method of a Ru-Li co-doped nickel oxide film is characterized in that carrying out according to following steps:
(1) takes by weighing 1.24-1.25gNi (CH
3COO)
24H
2O is dissolved in the 25mL EGME, adds and Ni (CH
3COO)
24H
2The equimolar thanomin of O, after stirring 30-40 min under 60-70 ℃ the water bath condition, adding mass ratio is 3: RuCl (1-5)
33H
2O and CH
3COOLi continues to stir 90-100 min, obtains the nickel oxide colloidal sol of Ru-Li codoped, with its still aging 24-48h in air;
(2) substrate is cleaned 10-15min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple successively, with the absolute ethyl alcohol flushing, on heating platform, dry afterwards again;
(3) with sol evenning machine the Ru-Li co-doped nickel oxide colloidal sol that obtains after still aging is carried out spin-coating on substrate; Under the rotating speed of 800-1000r/min, drip colloidal sol 5-10s earlier to substrate; Then substrate is rotated 30-40 s under the rotating speed of 3000-3500r/min; Substrate surface forms wet film, and substrate is placed on the heating platform heating, drying under 100-120 ℃ of temperature, repeats above-mentionedly to be coated with membrane process twice;
(4) at last with the temperature rise rate of 6 ℃/min, under 300-600 ℃ of condition in air to film thermal treatment 1-2 h, obtain Ru-Li co-doped nickel oxide film.
2. the preparation method of a kind of Ru-Li co-doped nickel oxide film according to claim 1 is characterized in that described substrate is Si substrate, ITO conductive glass substrate or glass substrate.
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Cited By (3)
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| CN103904216A (en) * | 2014-03-21 | 2014-07-02 | 西安理工大学 | Method for preparing titanium-doped nickel oxide resistance memorizer thin film |
| CN104834033A (en) * | 2015-04-10 | 2015-08-12 | 北京空间机电研究所 | Spin coating preparation method for transparent diffraction film used for optical element |
| CN116332623A (en) * | 2023-03-27 | 2023-06-27 | 深圳市众诚达应用材料科技有限公司 | NMO oxide semiconductor material, and preparation method and application thereof |
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| CN103904216A (en) * | 2014-03-21 | 2014-07-02 | 西安理工大学 | Method for preparing titanium-doped nickel oxide resistance memorizer thin film |
| CN104834033A (en) * | 2015-04-10 | 2015-08-12 | 北京空间机电研究所 | Spin coating preparation method for transparent diffraction film used for optical element |
| CN104834033B (en) * | 2015-04-10 | 2017-05-10 | 北京空间机电研究所 | Spin coating preparation method for transparent diffraction film used for optical element |
| CN116332623A (en) * | 2023-03-27 | 2023-06-27 | 深圳市众诚达应用材料科技有限公司 | NMO oxide semiconductor material, and preparation method and application thereof |
| CN116332623B (en) * | 2023-03-27 | 2024-06-11 | 深圳众诚达应用材料股份有限公司 | NMO oxide semiconductor material, and preparation method and application thereof |
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Application publication date: 20120905 |