CN111307872A - Method for measuring surface work function of ferroelectric film - Google Patents
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- CN111307872A CN111307872A CN202010108083.1A CN202010108083A CN111307872A CN 111307872 A CN111307872 A CN 111307872A CN 202010108083 A CN202010108083 A CN 202010108083A CN 111307872 A CN111307872 A CN 111307872A
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 63
- 239000002184 metal Substances 0.000 claims abstract description 63
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000005036 potential barrier Methods 0.000 claims abstract description 13
- 239000010408 film Substances 0.000 claims description 44
- 239000010409 thin film Substances 0.000 claims description 40
- 230000007547 defect Effects 0.000 claims description 12
- 239000000523 sample Substances 0.000 claims description 9
- 238000001453 impedance spectrum Methods 0.000 claims description 8
- 230000004888 barrier function Effects 0.000 claims description 7
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 5
- 238000001259 photo etching Methods 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 238000005530 etching Methods 0.000 claims description 3
- 238000004544 sputter deposition Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052737 gold Inorganic materials 0.000 description 10
- 229910052697 platinum Inorganic materials 0.000 description 10
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 9
- 230000004913 activation Effects 0.000 description 7
- 229910002115 bismuth titanate Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- -1 Pt and Au Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- ZDOOFQHNSWDMES-UHFFFAOYSA-N [Nd].[Mn] Chemical compound [Nd].[Mn] ZDOOFQHNSWDMES-UHFFFAOYSA-N 0.000 description 1
- VNSWULZVUKFJHK-UHFFFAOYSA-N [Sr].[Bi] Chemical compound [Sr].[Bi] VNSWULZVUKFJHK-UHFFFAOYSA-N 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/002—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the work function voltage
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The invention discloses a method for measuring the surface work function of a ferroelectric film, which comprises the following steps: s1, preparing metal top electrodes with different work functions on the surface of the ferroelectric film to be tested; s2, measuring potential barrier differences between different metal top electrodes and the ferroelectric film to be measured; and S3, generating the surface work function of the ferroelectric film to be tested based on the potential barrier difference and the work function of the metal top electrode. Compared with the prior art, the method can conveniently obtain the work function value of the surface of the film under the condition of lacking a large work function detection instrument, further deepens people's understanding of the surface characteristics of the oxide ferroelectric film and effectively obtains the concentration value of the oxygen vacancy, and in addition, the method can also greatly improve the performance regulation and control of the surface properties of the oxide ferroelectric film, so that the optimal film preparation parameters are obtained.
Description
Technical Field
The invention relates to the technical field of functional films, in particular to a method for measuring the surface work function of a ferroelectric film.
Background
In the field of engineering and scientific research, researchers urgently want to know the defect concentration and the Fermi level state of the surface of the thin film, but the method is not available, and only a great deal of time is spent on microscopic detection.
In the prior art, the following two methods are generally adopted for detection: one method is to use kelvin probe and kelvin probe force microscope to make measurements; another method is based on the principle of light emission, in which Ultraviolet (UV) light is used to excite electrons on the surface of a solid sample, and the energy spectrum of the emitted electrons is measured to analyze information such as density of states, occupation states, and work functions of the sample. However, the above methods are all for measuring a minute area, it is difficult to obtain the work function of a film sample in a large area, and the measured result is further processed and cannot be used as it is.
Therefore, how to rapidly measure the work function of a film in a large area becomes a problem that needs to be solved by those skilled in the art.
Disclosure of Invention
Aiming at the defects in the prior art, the problems to be solved by the invention are as follows: how to quickly measure the work function of a film in a large area.
The invention adopts the following technical scheme:
a method for measuring the surface work function of a ferroelectric film comprises the following steps:
s1, preparing metal top electrodes with different work functions on the surface of the ferroelectric film to be tested;
s2, measuring potential barrier differences between different metal top electrodes and the ferroelectric film to be measured;
and S3, generating the surface work function of the ferroelectric film to be tested based on the potential barrier difference and the work function of the metal top electrode.
Preferably, step S1 includes:
s101, aligning holes to a target preparation area and shielding a non-preparation area by using a mask plate with the holes;
s102, etching a target electrode pattern in a target preparation area in a photoetching, exposing and developing mode;
s103, sputtering a target metal electrode in a magnetron sputtering mode;
s104, repeating the steps S101 to S103 to complete the preparation of a plurality of metal top electrodes with different work functions.
Preferably, step S2 includes:
s201, obtaining equivalent grain resistances Rg corresponding to different metal top electrodes at different temperatures through temperature impedance spectrum curves;
s202, obtaining the barrier difference of the current carrier defect at the metal top electrode by utilizing a fitting curve of linear relation between Ln (Rg) and 1000/T, wherein Ln (Rg) represents that the equivalent crystal grain resistance Rg takes a logarithmic value, and T represents the temperature.
Preferably, step S201 includes:
s2011, measuring complex impedance data under different frequencies at different temperatures;
s2012, fitting the complex impedance circle to obtain a complex impedance map;
s2013, calculating the radius of the impedance circle based on the complex impedance map so as to obtain equivalent grain resistance at different temperatures.
Preferably, when the metal top electrode is in a probe structure, the barrier difference of the carrier defects at the metal top electrode is obtained by measuring the temperature impedance spectrum curves of a plurality of adjacent regions.
Preferably, the work function of the surface of the ferroelectric film to be measured is equal to the work function of the metal top electrode plus the corresponding potential barrier difference.
Preferably, the ferroelectric thin film is a doped oxide ferroelectric thin film, an undoped oxide ferroelectric thin film, or an organic ferroelectric thin film.
Preferably, the different metal top electrodes include at least one metal top electrode having a work function larger than a work function of a surface of the ferroelectric thin film and one metal top electrode having a work function smaller than a work function of a surface of the ferroelectric thin film.
In summary, the technical scheme adopted by the invention is as follows: the temperature complex impedance diagram under the metal top electrode with different work functions is obtained through the measurement of the impedance spectrum technology, the activation energy value of the defect under a specific area is obtained through fitting, the work function value of the thin film oxide is obtained through comparing the difference value of the temperature complex impedance diagram and the activation energy value of the defect under the specific area, and the work function value of the thin film oxide is obtained through adding the difference value according to the work function value of the known metal.
Compared with the existing film work function technology, the method has the advantages of simplicity and easy operability, and can quickly find the specific work function value of the film surface by the method especially for laboratories or enterprises which lack large-scale film work function detection instruments and devices, thereby effectively improving the film preparation efficiency and being more beneficial to establishing a corresponding theoretical physical model to improve the film preparation quality.
Drawings
FIG. 1 is a flow chart of an embodiment of the method for determining the surface work function of a ferroelectric thin film according to the present invention;
FIG. 2 is a schematic diagram illustrating the structure of a ferroelectric thin film prepared on Pt or metal oxide as a bottom electrode according to the present invention;
FIG. 3 is a schematic structural diagram of the top electrode of the present invention with different top electrodes such as Pt, Au, NiFe and Al prepared in four different areas of the thin film by a mask;
FIG. 4 is a temperature impedance spectrum plot of various metal top electrodes of the present invention: (a) pt; (b) au; (c) NiFe; (d) al;
FIG. 5 is a graph of the curves of different metal top electrodes Ln (Rg) -1000/T in the present invention, and the slope of the corresponding segment is the activation energy value under defect.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
As shown in fig. 1, the invention discloses a method for measuring the surface work function of a ferroelectric thin film, which comprises the following steps:
s1, preparing metal top electrodes with different work functions on the surface of the ferroelectric film to be tested;
s2, measuring potential barrier differences between different metal top electrodes and the ferroelectric film to be measured;
and S3, generating the surface work function of the ferroelectric film to be tested based on the potential barrier difference and the work function of the metal top electrode.
The invention obtains the work function of the film according to the potential barrier difference value of different metal top electrodes and the known metal work function value by utilizing the principle that the metal top electrodes with different work functions can form the potential barrier difference of carrier defects with the oxide ferroelectric film. Compared with the existing film work function technology, the method has the advantages of simplicity and easy operability, and can quickly find the specific work function value of the film surface by the method especially for laboratories or enterprises which lack large-scale film work function detection instruments and devices, thereby effectively improving the film preparation efficiency and being more beneficial to establishing a corresponding theoretical physical model to improve the film preparation quality.
In specific implementation, step S1 includes:
s101, aligning holes to a target preparation area and shielding a non-preparation area by using a mask plate with the holes;
s102, etching a target electrode pattern in a target preparation area in a photoetching, exposing and developing mode;
s103, sputtering a target metal electrode in a magnetron sputtering mode;
s104, repeating the steps S101 to S103 to complete the preparation of a plurality of metal top electrodes with different work functions.
In the present invention, the film can be prepared by the following method:
the preparation of ferroelectric thin films (zirconium doped lead titanate (PZT) or neodymium doped bismuth titanate thin film (BNT)) on the same bottom electrode (Pt, Au or metal oxide electrode) requires that the leakage current of the thin film not be too large. The structure is shown in fig. 2.
After the preparation of the thin film is completed, the preparation of the metal top electrode is carried out, and the specific structure can be shown in fig. 3. In fig. 3, an 1/4 area of the film is selected through a mask plate with circular holes, and other areas are covered, or a corresponding electrode pattern is engraved in a 1/4 area of the film through photoetching, exposure and developing technologies, a metal electrode is sputtered through a magnetron sputtering method, a metal target is replaced in magnetron sputtering, and metal top electrodes are sputtered in the other three areas of the film respectively. In the preparation process of the electrode, three or two types of metals can be sputtered according to actual conditions, but the work function of the metal is ensured to meet a group of gradients, such as Pt, Au, NiFe and Al electrodes; pt, Au, NiFe and Ta electrodes or Pt, Au, NiFe and Zn electrodes.
In specific implementation, step S2 includes:
s201, obtaining equivalent grain resistances Rg corresponding to different metal top electrodes at different temperatures through temperature impedance spectrum curves;
s202, obtaining the barrier difference of the current carrier defect at the metal top electrode by utilizing a fitting curve of linear relation between Ln (Rg) and 1000/T, wherein Ln (Rg) represents that the equivalent crystal grain resistance Rg takes a logarithmic value, and T represents the temperature.
In specific implementation, step S201 includes:
s2011, measuring complex impedance data under different frequencies at different temperatures;
s2012, fitting the complex impedance circle to obtain a complex impedance map;
s2013, calculating the radius of the impedance circle based on the complex impedance map so as to obtain equivalent grain resistance at different temperatures.
The test sample can be placed on a test bench with variable temperature, and the test from high temperature to low temperature is recommended to ensure the stability of the test temperature. Complex impedance data under different frequencies from normal temperature (300K) to 150 ℃ (425K) are obtained, and a specific model can be selected through Z-View commercial fitting software to fit a complex impedance circle. The associated fitted curves are shown in FIG. 4, which shows the complex impedance plots at different temperatures. The equivalent grain resistance at different temperatures can be obtained by calculating the radius of the resistance circle.
RgSatisfy the Arrhenius formula in different temperature rangesg∝exp(-Ea/kBT) in which EaAverage activation energy of ions, k, for participating in electrical conductionBBoltzmann coefficients. Ln (R) is thus based on the principle of the above formulag) There is a linear relationship with 1000/T. And drawing a corresponding fitting curve of Ln (Rg) and 1000/T, wherein the slope of each curve is the activation energy value at the metal top electrode. Specifically, a neodymium-manganese co-doped bismuth titanate ferroelectric film (BNTM) can be selected as an example, ln (rg) and 1000/T linear curves of the film with Pt as a bottom electrode and Pt, Au, NiFe and Al as top electrodes are respectively used, and the slopes of the ln (rg) and the 1000/T linear curves are calculated by fitting, so that the corresponding activation energy value can be obtained, as shown in fig. 5. The activation energy for Pt, Au, NiFe top electrodes is 0.19eV, which is reported in the relevant literature as the energy of the first ionization migration of oxygen vacancies. And Al powerThe work function of the electrode in this region is 0.55eV, which is largely due to the fact that the work function of the Al electrode is lower than that of the ferroelectric film, and a hole blocking layer from the ferroelectric film to the Al electrode of 0.36eV is formed, and taking the metal work function of the Al electrode as 4.3eV as an example, the work function of the BNTM film can be calculated to be 4.66 eV. I.e. Wfilm＝Wal+WdiffWherein W isfilmIs the work function of the film, WalIs the work function of the Al electrode, WdiffIs the potential barrier difference between the Al top electrode and the Pt, Au and NiFe top electrodes.
In specific implementation, when the metal top electrode is in a probe structure, the barrier difference of the carrier defects at the metal top electrode is obtained by measuring temperature impedance spectrum curves of a plurality of adjacent regions (regions containing the metal top electrode).
In specific implementation, the work function of the surface of the ferroelectric film to be measured is equal to the work function of the metal top electrode plus the corresponding potential barrier difference.
In specific implementation, the ferroelectric thin film is a doped oxide ferroelectric thin film, an undoped oxide ferroelectric thin film or an organic ferroelectric thin film.
The ferroelectric thin film in the present invention includes not only the conventional oxide ferroelectric thin film (lead zirconate titanate (PZT), Bismuth Titanate (BTO), Bismuth Ferrite (BFO), Barium Titanate (BTO), hafnium oxide (HfO2), Strontium Bismuth Titanate (SBT), etc.), but also all doped forms of the oxide ferroelectric thin film of the type and partially organic ferroelectric thin films (e.g., PVDF, etc.).
In a specific implementation, the different metal top electrodes at least include a metal top electrode with a work function larger than the work function of the surface of the ferroelectric film, and a metal top electrode with a work function smaller than the work function of the surface of the ferroelectric film.
In the present invention, the metal top electrode is not limited to combinations of Pt, Au and NiFe with Al, Ta or Zn, according to actual measurement requirements, as long as several types of top electrode metals satisfy the work function above or below the work function of the ferroelectric thin film. Meanwhile, the types of the metal top electrode can also be three metals (such as Pt and Au, Al, Ta or Zn and the like) or two metals (such as Pt and Al, Ta or Zn and the like).
Finally, it is noted that the above-mentioned embodiments illustrate rather than limit the invention, and that, while the invention has been described with reference to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A method for measuring the surface work function of a ferroelectric thin film is characterized by comprising the following steps:
s1, preparing metal top electrodes with different work functions on the surface of the ferroelectric film to be tested;
s2, measuring potential barrier differences between different metal top electrodes and the ferroelectric film to be measured;
and S3, generating the surface work function of the ferroelectric film to be tested based on the potential barrier difference and the work function of the metal top electrode.
2. The method for measuring a surface work function of a ferroelectric thin film as set forth in claim 1, wherein the step S1 includes:
s101, aligning holes to a target preparation area and shielding a non-preparation area by using a mask plate with the holes;
s102, etching a target electrode pattern in a target preparation area in a photoetching, exposing and developing mode;
s103, sputtering a target metal electrode in a magnetron sputtering mode;
s104, repeating the steps S101 to S103 to complete the preparation of a plurality of metal top electrodes with different work functions.
3. The method for measuring a surface work function of a ferroelectric thin film as set forth in claim 1, wherein the step S2 includes:
s201, obtaining equivalent grain resistances Rg corresponding to different metal top electrodes at different temperatures through temperature impedance spectrum curves;
s202, obtaining the barrier difference of the current carrier defect at the metal top electrode by utilizing a fitting curve of linear relation between Ln (Rg) and 1000/T, wherein Ln (Rg) represents that the equivalent crystal grain resistance Rg takes a logarithmic value, and T represents the temperature.
4. A method for measuring a surface work function of a ferroelectric thin film as set forth in claim 3, wherein the step S201 comprises:
s2011, measuring complex impedance data under different frequencies at different temperatures;
s2012, fitting the complex impedance circle to obtain a complex impedance map;
s2013, calculating the radius of the impedance circle based on the complex impedance map so as to obtain equivalent grain resistance at different temperatures.
5. The method for determining a surface work function of a ferroelectric thin film as set forth in claim 1, wherein the barrier difference of the carrier defect at the metal top electrode is obtained by measuring temperature impedance spectrum curves of a plurality of adjacent regions when the metal top electrode has a probe structure.
6. The method of claim 1, wherein the work function of the surface of the ferroelectric thin film to be measured is equal to the work function of the metal top electrode plus the corresponding barrier difference.
7. The method for measuring the surface work function of a ferroelectric thin film as claimed in any one of claims 1 to 6, wherein the ferroelectric thin film is a doped oxide ferroelectric thin film, an undoped oxide ferroelectric thin film or an organic ferroelectric thin film.
8. The method for measuring a work function of a surface of a ferroelectric thin film as set forth in any one of claims 1 to 6, wherein the different metal top electrodes include at least one metal top electrode having a work function larger than a work function of a surface of the ferroelectric thin film and one metal top electrode having a work function smaller than the work function of a surface of the ferroelectric thin film.
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