CN103922798B - A kind of preparation method of Cu doped zirconia Memister film - Google Patents
A kind of preparation method of Cu doped zirconia Memister film Download PDFInfo
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- CN103922798B CN103922798B CN201410123046.2A CN201410123046A CN103922798B CN 103922798 B CN103922798 B CN 103922798B CN 201410123046 A CN201410123046 A CN 201410123046A CN 103922798 B CN103922798 B CN 103922798B
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Abstract
A preparation method for Cu doped zirconia Memister film, stirs the glove box in vacuum after zirconia sol and Cu Ar ion mixing, obtains Cu doped zirconia colloidal sol; At room temperature, with Cu doped zirconia colloidal sol for precursor liquid, with SnO 2 thin film substrate for substrate lift Cu doped zirconia film, adopt dip-coating method obtained Cu doped zirconia gel film on SnO 2 thin film electrode again, carry out after drying in atmosphere naturally cooling in atmosphere after annealing in process, then put it into the sputtering of carrying out top electrode in sputter and get final product.The preparation method of Cu doped zirconia Memister film of the present invention, can effectively reduce set voltage and electric current after carrying out Cu doping; Compared with the technology of preparing of conventional semiconductive thin film, this sol-gel process is easy, device simple, and technological parameter is easy to control, and reduces production cost widely; When carrying out the doping of zirconia film, doping process simply, quantitatively accurate.
Description
Technical field
The invention belongs to microelectronic material preparing technical field, be specifically related to a kind of preparation method of Cu doped zirconia Memister film.
Background technology
Zirconia is a kind of important transition metal oxide material, and its chemical formula is ZrO2, has good optics and electrology characteristic, is widely used in antiferromagnetic materials, electrochromic display device, in numerous microelectronics such as chemical co-ordination device.Zirconia film Memister material have ultralow stable operating voltage, with traditional cmos process completely compatibility, extremely low power dissipation, ultrafast switching speed, high-density multi-value stores, Residuated Lattice energy by force, heat budget and the plurality of advantages such as tolerance is better and radiation resistance is good, become one of most important material in nonvolatile memory of future generation as the new device based on new physics mechanism.
But impurity doping is an important research means in solid research, is the 4th kind of perturbation scheme outside electricity, magnetic, thermal agitation.Cu doped zirconia Memister of the present invention film preparation have employed the research means of impurity doping, is also an important research in the research of electric resistance changing material.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Cu doped zirconia Memister film, its method technique is simple, cost is low.
The technical solution adopted in the present invention is, a kind of preparation method of Cu doped zirconia Memister film, specifically implements according to following steps:
Step 1, is not more than in the glove box of 40%RH in relative humidity, clarifying, then sealing stirring 1 ~ 2h after the mixing of zirconium-n-butylate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol ageing 20 ~ 24h and obtaining zirconia sol to solution; Being stirred to solution clarification by dripping acrylic acid after Schweinfurt green and methyl alcohol mix and blend 2h, obtaining the Cu ion needed for adulterating; Then by the Cu Ar ion mixing needed for zirconia sol and doping, and stir 8h at the glove box of vacuum, obtain Cu doped zirconia colloidal sol;
Step 2, at room temperature, with Cu doped zirconia colloidal sol for precursor liquid, with SnO 2 thin film substrate for substrate lift Cu doped zirconia film, adopt dip-coating method obtained Cu doped zirconia gel film on SnO 2 thin film electrode again, be then positioned over natural drying 5 ~ 10min in air;
Step 3, the Cu doped zirconia gel film obtained step 2 cools after carrying out annealing in process in atmosphere naturally, then puts it into the sputtering carrying out top electrode in sputter, namely obtains Cu doped zirconia Memister film.
Feature of the present invention is also,
In step 1, the mol ratio of zirconium-n-butylate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol is 1:1:40 ~ 45.
In step 1, the mol ratio of Schweinfurt green, acrylic acid and methyl alcohol is 1:1:20 ~ 25.
In step 1, the mol ratio of zirconia sol and the Cu ion needed for doping is 1:0.005 ~ 0.02.
In step 3, the temperature of annealing in process is 500 DEG C, and the time is 15 ~ 20min.
The specific operation process of the sputtering of top electrode in step 3 is: the Cu doped zirconia gel film after annealing in process is put into sputter, the mask plate with periodic diameter being 2mm micropore is fixed on sputter, open switch and carry out forvacuum, when vacuum degree reaches 1 × 10
-3after Pa, Cu doped zirconia gel film is carried out to the sputtering of top electrode, in sputter, sputtering target material is Cu, and sputtering time is 10 ~ 15min.
The invention has the beneficial effects as follows, the preparation method of Cu doped zirconia Memister film of the present invention, technique is simple, equipment is cheap, cost is low, and any surface finish of the Cu doped zirconia Memister film prepared is fine and close, and film quality is better.
Accompanying drawing explanation
Fig. 1 is the afm scan figure of the Cu doped zirconia gel film that embodiment 1 annealing in process obtains;
Fig. 2 is the afm scan figure of the Cu doped zirconia gel film that embodiment 2 annealing in process obtains;
Fig. 3 is the afm scan figure of the Cu doped zirconia gel film that embodiment 3 annealing in process obtains;
Fig. 4 is the transmittance curve figure of the Cu doped zirconia gel film that embodiment 1 ~ 3 annealing in process obtains;
Fig. 5 is the absorption constant curve chart of the Cu doped zirconia gel film that embodiment 1 ~ 3 annealing in process obtains;
Fig. 6 is the optical energy gap figure of the Cu doped zirconia gel film that embodiment 1 ~ 3 annealing in process obtains;
Fig. 7 is the I-V characteristic curve of the Cu doped zirconia Memister film that embodiment 1 prepares;
Fig. 8 is the Cu/ZrO of the Resistance of Zirconia memory film of the non-doped with Cu that embodiment 4 prepares
2/ ATO heterojunction I-V curve chart.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The preparation method of Cu doped zirconia Memister film of the present invention, specifically implements according to following steps:
Step 1, is not more than in the glove box of 40%RH in relative humidity, zirconium-n-butylate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol is clarified to solution for 1:1:40 ~ 45 mix the rear 1 ~ 2h that stirs in molar ratio, then seals ageing 20 ~ 24h and obtain zirconia sol; Be stirred to solution clarification by dripping acrylic acid after Schweinfurt green and methyl alcohol mix and blend 2h, wherein the mol ratio of Schweinfurt green, acrylic acid and methyl alcohol is 1:1:20 ~ 25, obtains the Cu ion needed for adulterating; Then by zirconia sol and doping needed for Cu ion be in molar ratio 1:0.005 ~ 0.02 mix, and vacuum glove box stirring 8h, obtain Cu doped zirconia colloidal sol;
Step 2, at room temperature, with Cu doped zirconia colloidal sol for precursor liquid, with SnO 2 thin film substrate for substrate lift Cu doped zirconia film, adopt dip-coating method obtained Cu doped zirconia gel film on SnO 2 thin film electrode again, be then positioned over natural drying 5 ~ 10min in air;
Step 3, the Cu doped zirconia gel film obtained step 2 cools carry out annealing in process 15 ~ 20min in the annealing furnace of 500 DEG C after in atmosphere naturally, then the Cu doped zirconia gel film just after annealing in process puts into sputter, the mask plate with periodic diameter being 2mm micropore is fixed on sputter, open switch and carry out forvacuum, when vacuum degree reaches 1 × 10
-3after Pa, Cu doped zirconia gel film is carried out to the sputtering of top electrode, in sputter, sputtering target material is Cu, and sputtering time is 10 ~ 15min, namely obtains Cu doped zirconia Memister film.
Embodiment 1
Step 1, in the glove box of relative humidity 38%RH, clarifying zirconium-n-butylate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol to solution for stirring 1.5h after 1:1:40 mixing in molar ratio, then sealing ageing 22h and obtaining zirconia sol; Be stirred to solution clarification by dripping acrylic acid after Schweinfurt green and methyl alcohol mix and blend 2h, wherein the mol ratio of Schweinfurt green, acrylic acid and methyl alcohol is 1:1:20, obtains the Cu ion needed for adulterating; Then by zirconia sol and doping needed for Cu ion in molar ratio for 1:0.005 mixing, and vacuum glove box stirring 8h, obtain Cu doped zirconia colloidal sol;
Step 2, at room temperature, with Cu doped zirconia colloidal sol for precursor liquid, with SnO 2 thin film substrate for substrate lift Cu doped zirconia film, adopt dip-coating method obtained Cu doped zirconia gel film on SnO 2 thin film electrode again, be then positioned over natural drying 8min in air;
Step 3, the Cu doped zirconia gel film obtained step 2 cools carry out annealing in process 15min in the annealing furnace of 500 DEG C after in atmosphere naturally, then the Cu doped zirconia gel film just after annealing in process puts into sputter, the mask plate with periodic diameter being 2mm micropore is fixed on sputter, open switch and carry out forvacuum, when vacuum degree reaches 1 × 10
-3after Pa, Cu doped zirconia gel film is carried out to the sputtering of top electrode, in sputter, sputtering target material is Cu, and sputtering time is 15min, namely obtains Cu doped zirconia Memister film.
Embodiment 2
Step 1, in the glove box of relative humidity 35%RH, clarifying zirconium-n-butylate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol to solution for stirring 2h after 1:1:45 mixing in molar ratio, then sealing ageing 20h and obtaining zirconia sol; Be stirred to solution clarification by dripping acrylic acid after Schweinfurt green and methyl alcohol mix and blend 2h, wherein the mol ratio of Schweinfurt green, acrylic acid and methyl alcohol is 1:1:22, obtains the Cu ion needed for adulterating; Then by zirconia sol and doping needed for Cu ion in molar ratio for 1:0.01 mixing, and vacuum glove box stirring 8h, obtain Cu doped zirconia colloidal sol;
Step 2, at room temperature, with Cu doped zirconia colloidal sol for precursor liquid, with SnO 2 thin film substrate for substrate lift Cu doped zirconia film, adopt dip-coating method obtained Cu doped zirconia gel film on SnO 2 thin film electrode again, be then positioned over natural drying 10min in air;
Step 3, the Cu doped zirconia gel film obtained step 2 cools carry out annealing in process 18min in the annealing furnace of 500 DEG C after in atmosphere naturally, then the Cu doped zirconia gel film just after annealing in process puts into sputter, the mask plate with periodic diameter being 2mm micropore is fixed on sputter, open switch and carry out forvacuum, when vacuum degree reaches 1 × 10
-3after Pa, Cu doped zirconia gel film is carried out to the sputtering of top electrode, in sputter, sputtering target material is Cu, and sputtering time is 10min, namely obtains Cu doped zirconia Memister film.
Embodiment 3
Step 1, in the glove box of relative humidity 40%RH, clarifying zirconium-n-butylate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol to solution for stirring 1h after 1:1:42 mixing in molar ratio, then sealing ageing 24h and obtaining zirconia sol; Be stirred to solution clarification by dripping acrylic acid after Schweinfurt green and methyl alcohol mix and blend 2h, wherein the mol ratio of Schweinfurt green, acrylic acid and methyl alcohol is 1:1:25, obtains the Cu ion needed for adulterating; Then by zirconia sol and doping needed for Cu ion in molar ratio for 1:0.02 mixing, and vacuum glove box stirring 8h, obtain Cu doped zirconia colloidal sol;
Step 2, at room temperature, with Cu doped zirconia colloidal sol for precursor liquid, with SnO 2 thin film substrate for substrate lift Cu doped zirconia film, adopt dip-coating method obtained Cu doped zirconia gel film on SnO 2 thin film electrode again, be then positioned over natural drying 8min in air;
Step 3, the Cu doped zirconia gel film obtained step 2 cools carry out annealing in process 20min in the annealing furnace of 500 DEG C after in atmosphere naturally, then the Cu doped zirconia gel film just after annealing in process puts into sputter, the mask plate with periodic diameter being 2mm micropore is fixed on sputter, open switch and carry out forvacuum, when vacuum degree reaches 1 × 10
-3after Pa, Cu doped zirconia gel film is carried out to the sputtering of top electrode, in sputter, sputtering target material is Cu, and sputtering time is 12min, namely obtains Cu doped zirconia Memister film.
Embodiment 4
Step 1, in the glove box of relative humidity 38%RH, clarifying zirconium-n-butylate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol to solution for stirring 1.5h after 1:1:40 mixing in molar ratio, then sealing ageing 22h and obtaining zirconia sol;
Step 2, at room temperature, take zirconia sol as precursor liquid, with SnO 2 thin film substrate for substrate lifts zirconia film, adopt dip-coating method obtained zirconia gel film on SnO 2 thin film electrode again, be then positioned over natural drying 8min in air;
Step 3, the zirconia gel film obtained step 2 cools carry out annealing in process 15min in the annealing furnace of 500 DEG C after in atmosphere naturally, then the zirconia gel film just after annealing in process puts into sputter, the mask plate with periodic diameter being 2mm micropore is fixed on sputter, open switch and carry out forvacuum, when vacuum degree reaches 1 × 10
-3after Pa, zirconia gel film is carried out to the sputtering of top electrode, in sputter, sputtering target material is Cu, and sputtering time is 15min, namely obtains Resistance of Zirconia memory film.
Cu doped zirconia gel film after utilizing atomic force microscope (AFM) to observe embodiment 1 ~ 3 annealing in process, as shown in Figures 1 to 3, Fig. 1,2,3 uses atomic force microscope (AFM) to carry out the flat scanning figure of microexamination to the Cu doped zirconia gel film surface after embodiment 1,2,3 annealing in process, and scanning area is 5 × 5um
2.As can be seen from Fig. 1 ~ 3, Cu doping be 0.005 zirconia film face in root mean square (RMS) value be 11.21nm; Cu doping be 0.01 zirconia film face in root-mean-square value be 6.39nm; Cu doping be 0.02 zirconia film face in root mean square be 11.9nm.All relatively more even, fine and close smooth by the zirconia film surface of the surface topography known three kinds of variable concentrations doping observing microcell, mean roughness is also all lower, and define the more uniform particle of size, crystal grain is high-visible.
In order to study the change of doping to the energy gap of film further, the basic concept of band theory thinks that the energy level of all electronics not distributes by energy even in any solid, but in a certain energy range close integrated belt, and high and low two energy ranges be adjacent are energy forbidden zones of electronics, by being called that the energy forbidden zone of forbidden band or energy gap separates between being with.The energy difference of high and low two energy becomes energy gap.Therefore We conducted the test of some optical properties, i.e. the test of reflectivity (R) and transmissivity (T).The energy gap of film can be calculated by reflectivity, thickness and transmitance, and concrete computing formula is:
α=(1/d)×㏑[(1-R)/T]（1）
αhν=C(hν-Eg)
1/2（2）
In formula: α-absorption constant;
D-thickness;
R-reflectivity;
T-transmissivity;
H ν-incident light energy;
C-light velocity, 3 × 10
8m/s.
Fig. 4 is the transmittance curve figure of the Cu doped zirconia gel film that embodiment 1 ~ 3 annealing in process obtains; Fig. 5 is the absorption constant curve chart of the Cu doped zirconia gel film that embodiment 1 ~ 3 annealing in process obtains; The optical transmission spectra figure of the Cu doped zirconia Memister film that embodiment 1 ~ 3 prepares as shown in Figure 4, as seen from Figure 4, sample has strong ABSORPTION EDGE at 350nm wavelength place, Cu doped zirconia Memister film prepared by embodiment 1 has the highest transmitance, can reach 91.0%; As shown in Figure 5, as seen from Figure 5, sample prepared by embodiment 1 ~ 3 all has obvious light interference phenomena to reflectance spectrum figure, shows that film surface is smooth and even.
Fig. 6 is the optical energy gap figure of the Cu doped zirconia gel film that embodiment 1 ~ 3 annealing in process obtains; With (α h ν)
2map to h ν, carrying out linearly outer delaying to curve, is exactly the optical energy gap of sample with the intersection point of transverse axis (X-axis).The energy gap of zirconia film of 0.005Cu, doping 0.01Cu and doping 0.02Cu of adulterating as shown in Figure 6 is respectively 5.80eV, 5.73eV and 5.67eV, and along with the increase of doping content, energy gap presents the trend of reduction.
(Keithley company produces to use Keithley; model 2400) the table Cu doped zirconia Memister film for preparing embodiment 1 in current/voltage source carries out the research of I-V resistance reverse speed characterisstic; when current protection line is 10mA, the I-V resistance reverse speed characterisstic curve of Cu doped zirconia Memister film prepared by embodiment 1 as shown in Figure 7.Scanning pattern is as shown by the arrows in Figure 7: 0V → 3.0V → 0 →-6.0V → 0V.First, when voltage reaches by 0V arrival 3.0V, increased by the electric current of film, device is transformed into low resistive state; Secondly, when voltage reaches-0.6V, electric current reduces suddenly, and device turns back to high-impedance state.This conversion between high-impedance state and low resistance state can repeat to realize, and the number of times of reversion is apparently higher than unadulterated zirconium dioxide membrane.
The zirconia film being illustrated in figure 8 non-doped with Cu prepared by embodiment 4 has typical bipolar I-V curve.Forward voltage scanning from 0, when set voltage reaches 4.1V, electric current increases suddenly, resistance decreasing.Now memory cell becomes low resistance state from high-impedance state, and this process is called set process.Compared with the I-V resistance reverse speed characterisstic of the zirconia film of non-doped with Cu, as a mole doping ZrO
2: during Cu=1:0.005, the set voltage required for zirconia film of Cu doping is only 3.0V, and be less than the 4.1V of unadulterated zirconia film, electric current is also down to 1mA from 10mA.Therefore, carry out Cu doping and can effectively reduce set voltage and electric current, thus effectively reduce the power of Memister work.Result of study according to various existing various resistance inversion mechanism compares can find out with experimental data, and the resistance reverse speed characterisstic of the zirconium dioxide membrane of doping 0.005Cu meets conductive filament theory.
Claims (3)
1. a preparation method for Cu doped zirconia Memister film, is characterized in that, specifically implements according to following steps:
Step 1, is not more than in the glove box of 40%RH in relative humidity, clarifying, then sealing stirring 1 ~ 2h after the mixing of zirconium-n-butylate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol ageing 20 ~ 24h and obtaining zirconia sol to solution; Being stirred to solution clarification by dripping acrylic acid after Schweinfurt green and methyl alcohol mix and blend 2h, obtaining the Cu ion needed for adulterating; Then by the Cu Ar ion mixing needed for zirconia sol and doping, and stir 8h at the glove box of vacuum, obtain Cu doped zirconia colloidal sol;
The mol ratio of described Schweinfurt green, acrylic acid and methyl alcohol is 1:1:20 ~ 25;
The mol ratio of described zirconia sol and the Cu ion needed for doping is 1:0.005 ~ 0.02;
The mol ratio of described zirconium-n-butylate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol is 1:1:40 ~ 45;
Step 2, at room temperature, with Cu doped zirconia colloidal sol for precursor liquid, with SnO 2 thin film substrate for substrate lift Cu doped zirconia film, adopt dip-coating method obtained Cu doped zirconia gel film on SnO 2 thin film electrode again, be then positioned over natural drying 5 ~ 10min in air;
Step 3, the Cu doped zirconia gel film obtained step 2 cools after carrying out annealing in process in atmosphere naturally, then puts it into the sputtering carrying out top electrode in sputter, namely obtains Cu doped zirconia Memister film.
2. the preparation method of Cu doped zirconia Memister film according to claim 1, it is characterized in that, in step 3, the temperature of annealing in process is 500 DEG C, and the time is 15 ~ 20min.
3. the preparation method of Cu doped zirconia Memister film according to claim 1, it is characterized in that, the specific operation process of the sputtering of top electrode in step 3 is: the Cu doped zirconia gel film after annealing in process is put into sputter, the mask plate with periodic diameter being 2mm micropore is fixed on sputter, open switch and carry out forvacuum, when vacuum degree reaches 1 × 10
-3after Pa, Cu doped zirconia gel film is carried out to the sputtering of top electrode, in sputter, sputtering target material is Cu, and sputtering time is 10 ~ 15min.
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| CN107155374A (en) | 2014-09-30 | 2017-09-12 | 惠普发展公司，有限责任合伙企业 | Memristor with oxide switchable layer |
| CN105137216A (en) * | 2015-07-09 | 2015-12-09 | 西安理工大学 | Zirconia film resistance conversion characteristic detection device and detection method thereof |
| CN105714250A (en) * | 2016-02-19 | 2016-06-29 | 西安理工大学 | Preparation method of N-doped amorphous carbon film resistive random access memory |
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