CN116171095B - Controllable alternating-current polarization nano domain regulation and control method based on lithium niobate single crystal film - Google Patents
Controllable alternating-current polarization nano domain regulation and control method based on lithium niobate single crystal film Download PDFInfo
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Abstract
The invention belongs to the technical field of semiconductors and relates to a MEMS (micro electro mechanical system) preparation process, in particular to a controllable alternating current polarization nano domain regulation method based on a lithium niobate single crystal film. The invention is based on the single characteristic of the inclination angle of the lithium niobate domain wall, and utilizes the PFM output alternating voltage to regulate and control the nano-scale domain structure design method, thereby effectively solving the problems that the traditional nano-scale electric domain is difficult to regulate and control, difficult to keep, and the high-density domain wall cannot be accurately regulated and controlled during preparation.
Description
Technical Field
The invention belongs to the technical field of semiconductors, relates to a MEMS (micro electro mechanical systems) preparation process, and particularly relates to a controllable alternating-current polarization nano domain regulation and control method based on a lithium niobate single crystal film.
Background
The preparation of domain wall elements has grown to a great extent as domain wall currents are discovered. The prior domain wall device has the problems of low device response, large noise influence and the like, and has limited application in various occasions. Currently, increasing the domain density to achieve a high density of charged domain walls is one of the main methods to increase the piezoelectric response of domain wall elements.
The PFM probe polarization is a mainstream electric domain regulating and controlling means, and the technology can accurately regulate and control polarization inversion of an electric domain at a designated position, and is a reliable and stable technical means. By utilizing the traditional means of PFM output direct current voltage to regulate and control electric domains, it is difficult to efficiently regulate and control stable nano domain structures which can be maintained for a long time. Therefore, development of nano domain structures with high density, high efficiency, high stability and long retention has become an object of current researchers. Furthermore, li Fei et al achieve electric domain modulation of the entire material by applying an alternating voltage across the face of the ferroelectric film. The technical means proves that the size of the electric domain cannot be reduced, and a large number of charged domain walls can be prepared only by means of alternating voltage so as to enhance the piezoelectric response output of the device. The alternating current polarization means has obvious defects, long polarization time, high polarization voltage and high energy consumption, can not realize the regulation and control of electric domains in a designated area, and is extremely dangerous because uncontrollable variables exist in MEMS sensing devices which are pursued to have high precision and high quality.
The lithium niobate is a lead-free ferroelectric monocrystal, has high Curie temperature, single domain wall inclination angle, wider forbidden bandwidth and high research value in external domain formation of an external field control surface. In the preparation of nano-domain structures, the traditional method for regulating domain inversion by applying direct-current voltage to the PFM needle tip needs to reduce the polarization range and obviously increases the number of stripes of gray level patterns, but the regulated domain structure is still difficult to maintain and has low density.
At present, the MEMS sensing device based on the ferroelectric material becomes a bottleneck for further breaking through the ferroelectric material due to the problems of small output, large noise and the like. For this reason, many scholars have proposed solutions such as polarization rotation and domain wall enhanced piezoelectric response.
Disclosure of Invention
Based on the research background, the invention aims to provide a controllable alternating-current polarization nano domain regulating method based on a lithium niobate single crystal film according to the capability of enhancing the output of a piezoelectric response device of a high-density charged domain wall, so that the problems that the traditional external field regulating high-density nano domain can not be regulated and controlled stably, is difficult to keep and the like during the overturning process of the nano domain can be solved.
The invention is realized by adopting the following technical scheme:
a controllable alternating-current polarization nano domain regulation method based on a lithium niobate single crystal film comprises the following steps:
step S1, in a lithium niobate single crystal (LiNbO) 3 LN) surface is subjected to ion implantation to form a damaged layer, and then a metal layer is sputtered; growing a silicon dioxide insulating layer on another lithium niobate monocrystal substrate;
directly bonding lithium niobate monocrystal with lithium niobate monocrystal substrate, annealing, stripping damaged layer to obtain monocrystal lithium niobate film, thinning and polishing to prepare optical grade lithium niobate film with LN/SiO successively from bottom to top 2 /Cr/LN。
Step S2, the PFM equipment is opened to a Single Frequency PFM mode, and the output voltage of the needle point is adjusted from direct current voltage to alternating current voltage.
And S3, selecting a region needing polarization by using a PFM equipment microscope, and setting a proper voltage frequency.
Step S4, selecting a proper gray scale map and voltage amplitude in the Litho mode.
And S5, completing alternating-current polarization regulation and control of nano domain formation, and scanning an electric domain phase diagram.
The method comprises the steps of performing ion implantation on the surface of a lithium niobate monocrystal, sputtering a layer of metal, directly bonding the metal with a lithium niobate substrate with a silicon dioxide insulating layer, then stripping a damaged layer after annealing to obtain a monocrystal lithium niobate film, preparing an optical-grade lithium niobate film by utilizing processes such as thinning and polishing, and finally realizing accurate regulation and control of a nano electric domain in a Litho mode after changing the output voltage of a needle point into an alternating voltage by utilizing Single Frequency PFM mode on the surface of the prepared monocrystal lithium niobate film.
Further preferably, in step S1, the implanted ions are helium ions. He (He) + The ion implantation energy range is 35 KeV-400 KeV, and the implantation dosage is more than 1X 10 13 ions/cm 2 。
In the step S1, the metal layer is a Cr layer with the thickness of 100nm, cr is used as a bottom electrode in the bonding sheet, and the bonding sheet is connected to the ground end of the equipment after being adhered with the metal gasket by utilizing conductive silver paste.
In step S1, a silicon dioxide insulating layer having a thickness of 2 μm was formed on another lithium niobate single crystal substrate by vapor deposition (PECVD).
Further preferably, in step S2, the tip output voltage is an ac voltage of a sinusoidal signal; in the step S3, the voltage frequency is 1-50 Hz; in step S4, the gray level map is in a shape of a Chinese character 'hui' or a stripe, or may be in other shapes; the voltage amplitude is 80-130V.
Alternating polarization can be accomplished at any given location, with polarized regions being square regions of no more than 120 μm.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention relates to a controllable alternating-current polarization nano domain regulating method based on a lithium niobate single crystal film, which prepares LN/SiO 2 The PFM needle point is used to apply frequency and amplitude controllable alternating voltage on the/Cr/LN bonding sheet, and the high-density nano domain regulation and control is realized in a specified range of a specified position.
2. The controllable high-density nano domain structure is successfully prepared by adopting a method combining a micro-nano processing technology and external field regulation and control and utilizing PFM output alternating voltage to regulate and control the nano domain structure based on the characteristic of single inclination angle of the lithium niobate single crystal domain wall.
3. Unlike direct current regulated nanometer domain turning, the invention proposes to realize high density nanometer electric domain preparation based on PFM. The preparation of the lithium niobate single crystal film high-density nano domain is realized based on the PFM external field domain regulation technology by changing the output voltage of the nano probe tip.
The invention has reasonable design and has important scientific significance and application value for breaking through the size effect promotion limitation and developing, applying and popularizing domain wall elements with high response.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described, and it will be obvious to those skilled in the art that other drawings can be obtained according to these drawings without inventive effort.
FIG. 1 shows a flow chart of a controllable alternating-current polarization nano-domain regulating method based on a lithium niobate single crystal film.
FIG. 2 shows a schematic diagram of the process for preparing a lithium niobate single crystal thin film according to the step S1 of the present invention.
FIG. 3 is a graph showing the nano domain structure regulated by the gray scale pattern of the Chinese character 'Hui' shape in the embodiment 1 of the present invention at the frequency of 20Hz.
FIG. 4 is a graph showing the nano domain structure regulated by the striped gray pattern of example 2 of the present invention at a frequency of 30Hz.
FIG. 5 shows the result of 70V voltage regulation for the striped domains.
FIG. 6 shows the result of 75V voltage regulation for the striped domains.
FIG. 7 shows the result of the voltage regulation of the striped domains 80V.
FIG. 8 shows the result of voltage regulation of the stripe-type electric domains 85V.
FIG. 9 shows the result of 90V voltage regulation for the striped domains.
Fig. 10 shows the test result of domain wall current at day 0 after the preparation of the stripe type electric domain.
Fig. 11 shows the result of maintaining the domain wall current at 100 days after the preparation of the stripe-type electric domain.
FIG. 12 shows the domain results for 10Hz voltage frequency modulation of the back-word type domains.
FIG. 13 shows the domain results for a 20Hz voltage frequency modulation of the back-word type domains.
FIG. 14 shows the domain results for a frequency modulation of the 30Hz voltage for the inverted-V-shaped domains.
FIG. 15 shows the domain results for 10Hz voltage frequency modulation of striped domains.
FIG. 16 shows the domain results for a striped domain 20Hz voltage frequency modulation.
FIG. 17 shows the domain results for a striped domain 30Hz voltage frequency modulation.
Fig. 18 shows a graph of dc polarized hundred nanometer electric domains.
FIG. 19 shows the result of PFM probe control return-type domain inversion under DC voltage.
FIG. 20 shows the PFM probe-controlled striped domain inversion results under DC voltage.
Detailed Description
Referring to fig. 1 to 2, the method for controlling the controllable alternating current polarization nano domain based on the lithium niobate single crystal film according to the embodiment of the invention comprises the steps of implanting a damage layer into lithium niobate single crystal ions, sputtering a metal film by magnetron sputtering, directly bonding with a lithium niobate substrate with a silicon dioxide insulating layer, stripping the damage layer after annealing, and obtaining the optical-grade lithium niobate film by utilizing thinning and polishing processes. And adjusting the output voltage of the needle point in the Single Frequency PFM mode into alternating voltage, selecting a region needing polarization, setting proper voltage frequency, opening the Litho mode, selecting proper gray level diagram and proper voltage amplitude, completing polarization, and scanning an electric domain phase diagram.
Wherein He is + The ion implantation energy range is 35 KeV-400 KeV, and the implantation dosage is more than 1X 10 13 ions/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The implantation energy of helium ion determines the position of the damaged layer, the larger the implantation energy is, the closer the damaged layer is to the bottom of LN single crystal (the thicker the film is), the smaller the implantation energy is, the closer the damaged layer is to the upper surface of LN single crystal (the thinner the film is), the implantation depth of the ion implantation on the surface of lithium niobate single crystal is controlled by the implantation energy of helium ion (the implantation depth, namely the thickness of the film is determined by the implantation energy, the easiness of stripping after annealing is determined by the implantation dose, the stripping is not good enough due to the dose, and the damaged layer is easily stripped due to the fact that bubbles are relatively easy to be generated due to the large dose).
It should be noted that the ac polarization controlling nano domain structure is a domain structure under the control of an external field, which integrates a gray scale map, frequency, polarization region, and polarization voltage. As the preparation process of the lithium niobate monocrystal film is mature and the inclination angle of the domain wall is single, the material is suitable for researching the formation of the external field regulation high-density nano domain structure, has wide application range and is beneficial to the preparation of a later-stage high-output response device.
The embodiment of the invention is oriented to the application requirements of electric domain regulation and piezoelectric enhanced output response devices on high-precision and high-stability high-density nano electric domain preparation, and explores the feasibility of being compatible with MEMS (micro electro mechanical systems) nanometer processing technology and outfield regulation technology, namely, the high-density nano domain structure is prepared by utilizing the characteristics of PFM outfield precise regulation and control of electric domain turnover and controllable alternating voltage frequency and amplitude. The invention selects the lithium niobate single crystal film, the lithium niobate is used as an artificial synthetic single crystal, has the characteristics of high Curie temperature, wide forbidden band, single domain wall angle and the like, and is an ideal material for researching the controllable alternating current polarization nano domain regulation.
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions of the embodiments of the present invention are clearly and completely described, and it is apparent that the embodiments described below are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, one of ordinary skill in the art could obtain all other embodiments without undue burden. The reagents and raw materials used in the examples of the invention are all commercially available or self-made.
Example 1
A controllable alternating-current polarization nano domain regulation method based on a lithium niobate single crystal film comprises the following steps:
step S1, forming a damaged layer by helium ion implanted on the surface of the lithium niobate single crystal (implantation depth is controlled by helium ion energy, wherein the helium ion implantation energy is 35KeV, and the implantation dosage is 1×10) 13 ions/cm 2 ) And sputtering a layer of metal Cr with the thickness of 100nm by utilizing the magnetron sputtering technology. And simultaneously, a silicon dioxide insulating layer with the thickness of 2 mu m is grown on the other lithium niobate single crystal substrate by using a vapor deposition method.
The lithium niobate substrate and the lithium niobate monocrystal are directly bonded together, and the thickness of the required lithium niobate monocrystal film is achieved through a polishing and thinning process, as shown in figure 2. As a result of the test, the roughness reaches the pm level in the region of 10 μm×10 μm.
And S2, opening the PFM equipment to a Single Frequency PFM mode, and adjusting the output voltage of the nanometer needle point to the alternating voltage of a sine signal.
And S3, selecting a region needing polarization by using a PFM equipment microscope, setting a square region with a side length of 20 mu m as a polarization range, and setting the voltage frequency to be 20Hz.
And S4, selecting a gray scale image in a shape like a Chinese character 'Hui' for polarization in a Litho mode, and adjusting the voltage amplitude to be 90V.
And S5, completing alternating-current polarization regulation and control of nano domain formation, and scanning an electric domain phase diagram.
The controllable ac polarization nano-domain control method based on the lithium niobate single crystal thin film applied in this embodiment 1, the phase diagram of the reverse-square gray scale map and the electric domain polarization inversion under the ac voltage of 20Hz are shown in fig. 3, the gray scale map is reverse-square (wherein the outer ring is the inversion region and the inner ring is the holding region), if the inversion is controlled by using the dc voltage, the electric domain control result is shown in fig. 19, which is the reverse-square domain structure realizing the inversion completely according to the gray scale map. The alternating voltage has alternating voltage amplitude, so that a certain area exists in each period, the voltage is insufficient to turn over the electric domains, corresponding blank is left in the final result, a striped domain of one track appears, and the position of domain turning over is controlled by the gray image. Therefore, the domain regulating method is determined by the gray level diagram and the voltage frequency.
Example 2
A controllable alternating-current polarization nano domain regulation method based on a lithium niobate single crystal film comprises the following steps:
step S1, helium ions are injected on the surface of the lithium niobate single crystal to form a damage layer (the injection depth is controlled by the energy of the helium ions, wherein the injection energy of the helium ions is 200KeV, and the injection dosage is 1 multiplied by 10) 13 ions/cm 2 ) And sputtering a layer of gold with the thickness of 100nm by using the magnetron sputtering technologyBelongs to Cr. And simultaneously, a silicon dioxide insulating layer with the thickness of 2 mu m is grown on the other lithium niobate single crystal substrate by using a vapor deposition method.
The lithium niobate substrate and the lithium niobate monocrystal are directly bonded together, and the thickness of the required lithium niobate monocrystal film is achieved through a polishing and thinning process, as shown in figure 2. As a result of the test, the roughness reaches the pm level in the region of 10 μm×10 μm.
And S2, opening the PFM equipment to a Single Frequency PFM mode, and adjusting the output voltage of the nanometer needle point to the alternating voltage of a sine signal.
And S3, selecting a required polarization region by utilizing a PFM equipment microscope, setting a square region with the side length of 20 mu m as a polarization range, and setting the voltage frequency to be 30Hz.
And S4, selecting a stripe gray scale map for polarization in a Litho mode, and adjusting the voltage amplitude to be 100V.
And S5, completing alternating-current polarization regulation and control of nano domain formation, and scanning an electric domain phase diagram.
The controllable ac polarization nano-domain control method based on the lithium niobate single crystal thin film applied in this embodiment 2, the stripe type gray scale map and the phase map of the electric domain polarization inversion under the ac voltage of 30Hz are shown in fig. 4, the gray scale map is stripe type (five stripes to be inverted and four stripes to be maintained), if the inversion is controlled by using the dc voltage, the electric domain control result is shown in fig. 20, and this is the stripe type domain structure realizing the inversion completely according to the gray scale map. The alternating voltage has alternating voltage amplitude, so that a certain area exists in each period, the voltage is insufficient to turn over the electric domains, corresponding blank is left in the final result, a striped domain of one track appears, and the position of domain turning over is controlled by the gray image. Therefore, the domain regulating method is determined by the gray level diagram and the voltage frequency.
The technical method for outputting controllable alternating voltage by the PFM needle tip in the embodiment 1 and the embodiment 2 is applied to the preparation of a high-density nano domain structure, so that the high-density nano electric domain which is efficient, simple and stable to prepare is obtained.
Example 3
A controllable alternating-current polarization nano domain regulation method based on a lithium niobate single crystal film comprises the following steps:
step S1, forming a damaged layer by helium ion implanted on the surface of the lithium niobate single crystal (implantation depth is controlled by helium ion energy of 300KeV with implantation dose of 1×10) 13 ions/cm 2 ) And sputtering a layer of metal Cr with the thickness of 100nm by utilizing the magnetron sputtering technology. And simultaneously, a silicon dioxide insulating layer with the thickness of 2 mu m is grown on the other lithium niobate single crystal substrate by using a vapor deposition method.
The lithium niobate substrate and the lithium niobate monocrystal are directly bonded together, and the thickness of the required lithium niobate monocrystal film is achieved through a polishing and thinning process, as shown in figure 2. As a result of the test, the roughness reaches the pm level in the region of 10 μm×10 μm.
And S2, opening the PFM equipment to a Single Frequency PFM mode, and adjusting the output voltage of the nanometer needle point to the alternating voltage of a sine signal.
And S3, selecting a region needing polarization by using a PFM equipment microscope, setting a square region with a side length of 100 mu m as a polarization range, and setting the voltage frequency to be 30Hz.
And S4, selecting a stripe gray scale map for polarization in a Litho mode, and adjusting the voltage amplitude to be 120V.
And S5, completing alternating-current polarization regulation and control of nano domain formation, and scanning an electric domain phase diagram.
In this example 3, experimental results of stable maintenance of alternating current domains of domain structures at 30Hz voltage in the region of 100 μm were applied based on the lithium niobate single crystal thin film controllable alternating current polarization nano domain regulation method, and as shown in fig. 10 and 11, the maintenance time of domain wall current was tested, since the existence of domain wall current demonstrated the existence of electric domains, i.e., the maintenance of electric domains was verified. 10 is the domain wall current at day 0 after domain preparation, and 11 is the result of the holding test of domain wall current at day 100 after domain preparation. It can be seen that the method of the present invention produces complete electrical domains with very pronounced retention characteristics and good retention. The alternating current polarization regulation nano domain structure has good domain wall current retention performance, and is suitable for manufacturing various sensing devices.
The invention aims at integrating the advantages of high precision and low power consumption of PFM needle point regulation and control, simultaneously plays the advantages of the response capability of the compact charged domain wall lifting device prepared by alternating voltage in the polarization process, changes the output voltage of the PFM probe into alternating voltage, can realize the precise regulation and control of domain walls with different densities by controlling the voltage frequency, can accurately meet various requirements, and provides more possibility for the preparation of domain wall enhanced piezoelectric response devices.
For this purpose, the properties of the prepared device were specifically tested in experiments for domain wall enhancement piezoelectric response and by longitudinal piezoelectric coefficientd 33 To react (since the lithium niobate material used is a Z-cut material, only the Z-axis direction is verified when verifying the force electrical coupling performance). The specific data are shown in Table 1:
TABLE 1
As known from the prior art, the longitudinal piezoelectric coefficient of lithium niobate materialsd 33 Typically less than 40pc/N. The point positions 1 to 7 are direct current voltage regulation and the point positions 8 and 9 are alternating current voltage regulation, and the output enhancement effect can be obviously seen by comparing the piezoelectric coefficient of the direct current regulation with the piezoelectric coefficient of the alternating current. As shown in Table 1, the piezoelectric coefficient was 69.89pc/N when only a single DC domain (five squares) was written, and there was a significant change in piezoelectric coefficient (as shown by points 2-7, up to 100 more) when a plurality of domain structures were written using the electric domain nesting technique, as compared to a single domain structure. However, when the direct current regulates and controls a plurality of domain structures, the direct current domain can regulate and control only 3-4 domain structures under a certain electrode due to the limitation of the size and the domain writing range, which means that under the same condition, the piezoelectric coefficient of the film under direct current polarization is about 100, but the gain of domain wall enhanced piezoelectric response caused by alternating current polarization is obviously larger (a single alternating current domain can increase the piezoelectric coefficient of the device to 240.98 pc)N is 3.4 times the piezoelectric coefficient of a single dc domain). This remarkable gain effect results from the preparation of high density, small size nano-domain structures, which is also where the invention provides more possibilities for domain wall element preparation. It can be verified that the force electric coupling device prepared by the embodiment of the invention has domain wall boosting electric response.
The invention has the greatest advantages that accurate electric domain regulation and control can be completed in any appointed area, and meanwhile, the output enhancement of the device is realized by utilizing the advantages of controllable alternating voltage frequency and the like.
Fig. 19 shows the result of gray scale pattern control of the shape of the return character under direct current voltage, and according to the gray scale pattern, the domain structure can keep the original domain in the internal return character, the original domain between the inner ring and the outer ring is turned over to obtain a reversed domain structure, and the phase difference generated between the inner ring and the outer ring after the inversion can be used for verifying domain inversion. However, ac polarization is also characterized by the alternating nature of the voltage, which is a variable quantity, resulting in a large fraction of the voltage being insufficient to complete the polarization during the polarization process. This would result in the absence of inversion of the electric domains, and in the presence of gaps in the region where the inversion should have been polarized, which gaps would otherwise fail to invert, further verifying the authenticity of the alternating signal applied to the PFM probe. Such gaps exist in both the back-shaped and striped domains patterns, primarily because the ac voltage is too small in this region to polarize the switching domains. In addition to the effect of the gray pattern on the ac polarization, the frequency change can also have an effect. Fig. 12 to 14 show the electric domain control results under different voltage frequencies of the gray scale pattern of the ac voltage in the shape of a Chinese character 'hui', and it is clear that the above-mentioned non-inverted gap will decrease with increasing voltage frequency, which is related to the short polarization time and the decrease of the non-inverted region caused by the decrease of the ac voltage period after the frequency increase. Fig. 15 to 17 show the results of electric domain control prepared under different voltage frequencies of the stripe-type electric domains under the alternating voltage, and the stripe-type electric domains have the conditions of increasing frequency and decreasing gap as the electric domains controlled by the gray scale pattern in the shape of a Chinese character 'hui'. However, because the preset turning areas are different, the control results of the gray level images are obviously different from those of the gray level images in the shape of a Chinese character 'hui', namely, the whole image distribution accords with the preset gray level image, and the influence of the gray level image and the frequency in the whole polarization process can be intuitively seen. Because of the influence of frequency on the electric domain structure, electric domains with different densities can be prepared by only changing the voltage frequency in a fixed range, and the method has good guiding significance for the preparation of high-density domain walls and the enhancement of piezoelectric response of the domain walls.
FIGS. 5 to 9 show the influence of different AC voltages on the formation of AC domains, and the invention performs a polarization experiment of 70V to 90V and verifies that the 20 μm region can be regulated by a voltage of more than or equal to 90V. Compared with direct current voltage regulation, alternating current polarization requires higher voltage to complete polarization inversion, which is mainly related to the fact that the effective value of alternating current voltage is 0.707 times of the amplitude, so that the current polarization requires higher voltage to realize inversion of electric domains.
In addition, as shown in FIG. 18, a DC polarization hundred nanometer electric domain picture is shown, and in the figure, a 300nm electric domain regulation and control picture is shown. As can be seen from fig. 18, dc polarization needs to control more stripes in a smaller area to achieve the requirement of hundred nanometers, but it is difficult to control stable and reliable high-density electric domains in this way, so dc voltage does not have obvious advantages in the preparation of high-density electric domains, and the preparation of the domain structure is completed under the polarization voltage which needs a new needle, is well dried in weather and has a voltage greater than the original size, so that the harsh condition required when dc voltage is controlled in hundred nanometer-scale electric domains can be seen. Meanwhile, the illustrated 300nm domain structure still cannot be perfectly prepared even under such severe conditions, which further proves the difficulty of direct-current voltage regulation of hundred-nanometer-scale electric domains. The same electric domain density can be easily achieved by modulating the 30Hz electric domain in the 20 μm region (example 2 shown in FIG. 4).
In summary, the invention researches the nano-scale high-density electric domain regulation of the ferroelectric single crystal film, adopts a method combining a micro-nano processing technology and external field regulation, is based on the characteristic of single domain wall inclination angle of the lithium niobate single crystal, and utilizes the design method of regulating the nano-scale domain structure by using the PFM needle point to output alternating voltage, thereby effectively solving the problems that the traditional nano-scale electric domain is difficult to regulate and control, is difficult to maintain, and the high-density domain wall cannot be accurately regulated and controlled during preparation, and the like.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; while the invention has been described in detail with reference to the foregoing embodiments, it will be appreciated by those skilled in the art that variations may be made in the techniques described in the foregoing embodiments, or equivalents may be substituted for elements thereof; such modifications and substitutions do not depart from the spirit and scope of the various embodiments of the invention, which should be construed to cover all aspects of the invention as set forth in the following claims.
Claims (10)
1. A controllable alternating-current polarization nano domain regulation method based on a lithium niobate single crystal film is characterized by comprising the following steps of: the method comprises the following steps:
s1, forming a damaged layer after ion implantation on the surface of a lithium niobate single crystal, and then sputtering a metal layer; growing a silicon dioxide insulating layer on another lithium niobate monocrystal substrate;
directly bonding the lithium niobate monocrystal with a lithium niobate monocrystal substrate, stripping a damaged layer after annealing to obtain a monocrystal lithium niobate film, and preparing an optical-grade lithium niobate film by utilizing thinning and polishing processes;
step S2, the PFM equipment is opened to a Single Frequency PFM mode, and the output voltage of the needle tip is adjusted from direct current voltage to alternating current voltage;
step S3, selecting a region needing polarization by utilizing a PFM equipment microscope, and setting proper voltage frequency;
step S4, selecting a proper gray scale map and a proper voltage amplitude in a Litho mode;
and S5, completing alternating-current polarization regulation and control of nano domain formation, and scanning an electric domain phase diagram.
2. The method for controlling the controllable alternating-current polarization nano-domain based on the lithium niobate single crystal film according to claim 1, which is characterized by comprising the following steps: in step S1, the implanted ions are helium ions.
3. The method for controlling the controllable alternating-current polarization nano-domain based on the lithium niobate single crystal film according to claim 2, which is characterized by comprising the following steps: in step S1, the metal layer is a Cr layer with a thickness of 100 nm.
4. The method for controlling the controllable alternating-current polarization nano-domain based on the lithium niobate single crystal film according to claim 3, which is characterized by comprising the following steps: in step S1, a silicon dioxide insulating layer having a thickness of 2 μm was formed on another lithium niobate single crystal substrate by vapor deposition.
5. The method for controlling the controllable alternating-current polarization nano-domain based on the lithium niobate single crystal film according to claim 4, which is characterized by comprising the following steps: in step S2, the tip output voltage is an ac voltage of a sinusoidal signal.
6. The method for controlling the controllable alternating-current polarization nano-domain based on the lithium niobate single crystal film according to claim 5, which is characterized by comprising the following steps: in step S3, the voltage frequency is 1-50 Hz.
7. The method for controlling the controllable alternating-current polarization nano-domain based on the lithium niobate single crystal film according to claim 6, which is characterized by comprising the following steps: in step S3, the voltage frequency is 10-30 Hz.
8. The method for controlling the controllable alternating-current polarization nano-domain based on the lithium niobate single crystal film according to claim 7, which is characterized by comprising the following steps: in step S4, the gray level diagram is in a shape of a Chinese character 'Hui' or a stripe; the voltage amplitude is 80-130V.
9. The method for controlling the nanometer domain based on controllable alternating current polarization of the lithium niobate single crystal film according to claim 8, which is characterized in that: in the step S4, the voltage amplitude is 90-120V.
10. According to claim2, a controllable alternating-current polarization nano domain regulating method based on a lithium niobate single crystal film is characterized in that: he (He) + The ion implantation energy range is 35 KeV-400 KeV, and the implantation dosage is more than 1X 10 13 ions/cm 2 。
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| JP2014187362A (en) * | 2013-02-25 | 2014-10-02 | National Institute Of Advanced Industrial & Technology | Piezoelectric mems device and manufacturing method therefor |
| CN108560060A (en) * | 2018-04-18 | 2018-09-21 | 重庆科技学院 | Lithium niobate nanometer farmland processing based on PFM and imaging method |
| CN113801412A (en) * | 2021-10-14 | 2021-12-17 | 之江实验室 | Flexible transparent piezoelectric composite film, transparent stretchable ultrasonic transducer and preparation method thereof |
| WO2022089959A1 (en) * | 2020-10-26 | 2022-05-05 | Université de Franche-Comté | Piezoelectric device comprising flexible single crystalline piezoelectric linbo3 and/or litao3 films integrated on flexible substrate and methods for producing the same |
| CN115116829A (en) * | 2022-08-29 | 2022-09-27 | 中北大学 | Method for preparing lithium niobate single crystal film domain wall enhanced force electric coupling response device |
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| JP2014187362A (en) * | 2013-02-25 | 2014-10-02 | National Institute Of Advanced Industrial & Technology | Piezoelectric mems device and manufacturing method therefor |
| CN108560060A (en) * | 2018-04-18 | 2018-09-21 | 重庆科技学院 | Lithium niobate nanometer farmland processing based on PFM and imaging method |
| WO2022089959A1 (en) * | 2020-10-26 | 2022-05-05 | Université de Franche-Comté | Piezoelectric device comprising flexible single crystalline piezoelectric linbo3 and/or litao3 films integrated on flexible substrate and methods for producing the same |
| CN113801412A (en) * | 2021-10-14 | 2021-12-17 | 之江实验室 | Flexible transparent piezoelectric composite film, transparent stretchable ultrasonic transducer and preparation method thereof |
| CN115116829A (en) * | 2022-08-29 | 2022-09-27 | 中北大学 | Method for preparing lithium niobate single crystal film domain wall enhanced force electric coupling response device |
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