CN117702260A - Device and method for rapidly preparing oxide epitaxial films in batches - Google Patents
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Abstract
The invention provides a device and a method for rapidly preparing oxide epitaxial films in batches. The method can ensure that the surface of the target, the plane of the mask plate and the plane of the substrate are always parallel, and ensure that the plume generated by pulse laser ablating the surface of the target, the center of the hole structure of the mask plate and the position of the substrate to be deposited are always on the same axis. Meanwhile, through the electric XYZ substrate base and the lens translation stage, the epitaxial film sample preparation with different cation defect concentrations under different laser energy densities can be realized by rapidly optimizing the epitaxial film growth conditions. By implementing the method, the high-flux preparation of the oxide epitaxial film with high uniformity, high reliability and high efficiency can be realized, and the method has important and wide application prospects in the aspects of advanced functional material production, basic physical research, semiconductor device manufacturing and the like.
Description
Technical Field
The invention relates to the field of material processing and preparation, in particular to rapid batch preparation of an oxide epitaxial film.
Background
The rapid development of modern information technology has changed the life of people, and the requirements of high integration and miniaturization of electronic components for realizing high-density and low-power-consumption modern electronic integrated equipment are also increasing. Film materials with thickness as low as several nanometers have achieved great economic benefits in the technical fields of modern storage, chips, display and the like. In the development process of such ultrathin film materials, a physical vapor deposition method such as a pulse laser deposition technique is generally adopted to prepare a target material sample. For the pulse laser deposition technology, the growth conditions of the film sample mainly comprise growth temperature, oxygen pressure, laser energy density and the like, and when the growth conditions are optimized, a certain growth condition needs to be changed in sequence until the sample meeting the design performance requirements can be obtained within a certain temperature, oxygen pressure and laser energy density range after multiple attempts. The time required for the high vacuum acquisition and the temperature rise and fall process is much longer than that required for the actual sample growth every time the sample is grown. Therefore, a long period is often required to obtain a new material after traversing all growth conditions, which is inefficient and costly, greatly limiting the development and application of the new material. On the other hand, although the current thin film growth technology has been capable of achieving atomic scale growth control, it has been actually shown that, when a sample is repeatedly grown a plurality of times, lattice defects, impurities, oxygen vacancies, etc. in the sample may fluctuate due to relative changes in growth conditions (e.g., laser energy, temperature, oxygen pressure, etc.), and systematic errors brought about may even confuse the intrinsic properties of the sample.
The method adopts a high-flux combined pulse laser film growth technology, and the existing method mainly bombards targets made of different materials in sequence through excimer pulse laser, so that target components are periodically deposited on a substrate, a thickness gradient is formed by combining with the movement of a mask plate, and hundreds or thousands of samples with different period thicknesses and different components can be prepared during one-time growth. Such a solution is described, for example, in chinese patent No. CN103469153A, CN103489750A, CN103871845a, etc. These techniques effectively accelerate the development of new materials such as superconductors, ferroelectrics, dielectrics, etc., but all of them realize the composition change of the whole sample by interdiffusion among the multiple components deposited on the substrate, have the disadvantages of uneven mixing, etc., and in order to ensure the complete diffusion among the components, the thickness of each period needs to be controlled not to exceed a certain critical value, and sometimes long-time post annealing is required.
Another high-flux combined pulse laser film growth technology (chinese patent No. CN112481586 a) synthesizes a superconducting combined film with sensitive parameters by combining laser energy densities, which realizes fine tuning of the chemical ratio of the film in a certain range by controlling the energy density ratio of two excimer pulse lasers bombarded to the target surface, thereby growing the film with specific components. The disadvantage of this approach is that it requires a complex optical path design and requires high demands on optical path control.
Disclosure of Invention
First, the technical problem to be solved
The invention aims to solve the problem of providing a simple and feasible high-flux film preparation method, which can realize the rapid batch preparation of the oxide epitaxial films with different cycle thicknesses and different components during one-time growth.
(II) technical solution
The invention provides a device for rapidly preparing oxide epitaxial films in batches, which is shown in figure 1 and comprises a multi-target base 1, a substrate base 2, a movable mask plate 3, an optical path system 4 and a monitoring system 5.
The multi-target base 1 is used for fixing targets, at least 4 targets can be loaded, the multi-target base is arranged in a vacuum cavity, each target can rotate and revolve, and a baffle plate with a round hole is arranged, so that other targets can be shielded when a film is deposited, and pollution among the targets is prevented.
The substrate holder 2 is described as being used for holding and heating a substrate, and is arranged opposite to the target holder 1. The substrate base 2 is fixed to the substrate 21 in a plane without projections, so that the mask plate can be moved closely without touching any parts. The substrate base 2 is rotatable to enable alignment of the edge of the substrate 21 with the aperture structure of the moving mask 3. In particular, the present invention proposes that the substrate base 2 is movable in three directions XYZ, wherein the movement in XY plane is used to grow high flux samples, ensuring that the target sample position remains in the plume axis all the time.
The movable mask plate 3 is a 304 or 316 stainless steel plate with a plurality of different hole-shaped structures, and the movable mask plate is detachably replaced by the mask plate with the different hole-shaped structures according to design requirements. The movable mask plate 3 needs to resist high temperature and does not release gas in vacuum. The movable mask plate 3 is arranged between the multi-target base 1 and the substrate base 2, and the displacement table controls the X, Y, Z to move in three dimensions. The target surface and the substrate surface are oppositely placed, and the movable mask plate is positioned between the target surface and the substrate surface and needs to be placed in parallel. The fact that the center position of the mask hole structure always keeps alignment with the axial direction of the plume and is combined with the substrate base 2 which can move in the three directions of XYZ is the key point of the invention, and each sample in the high-flux film grown can have uniform thickness and expected composition.
The optical path system 4 is composed of a plurality of 45-degree reflectors, a double-knife adjustable slit 41, a lens 42, an electric displacement table 43 for installing the lens and a manual absorption sheet 44, and is used for pulling pulse laser into a vacuum cavity to bombard the surface of a target material. The focal length of the lens is selected according to the actual requirement of the cavity, the lens is used for focusing the laser beam on the surface of the target, and the electric displacement table 43 is used for controlling the distance from the focal point of the lens to the target surface, so that the adjustment of the laser spot size is realized, which is unique to the invention.
The described monitoring system 5 comprises two high-definition cameras 51 and 52, a monitor 54, and an illumination LED lamp, and is mainly used for monitoring the relative positions of the movable mask plate 3 and the substrate 21, so as to control the distance between the mask plate 3 and the substrate 21 to be less than 0.2 mm, which is a feature of the present invention. Two high-definition cameras 51 and 52 are mounted on the flange at 90 degrees to each other, one of which is capable of observing whether the mask pattern edge is aligned with the substrate edge from the front surface of the substrate, and the other of which is capable of observing the space between the mask and the substrate from the side surface of the substrate.
The invention provides a method for rapidly optimizing epitaxial film growth conditions based on the device for rapidly preparing oxide epitaxial films in batches, which comprises the following steps:
the parameters influencing the growth of the epitaxial film mainly comprise temperature T, air pressure P and energy density F. The energy density is determined by the incident laser energy and the laser spot size, and the laser energy density bombarded on the target material can be adjusted by changing the laser spot size, so that the energy density F can be changed by setting the lens position in the invention.
The target is arranged at a position opposite to the substrate, the center of the hole-shaped structure of the movable mask plate 3 is controlled to be positioned at the center of a light spot of the laser on the surface of the target, so that the distance between the mask plate 3 and the substrate 21 is as close as possible, for example, less than 0.2 mm, and the distance between the mask plate 3 and the substrate 21 can be observed from the monitor 54 in real time. Setting the substrate temperature T n Pressure P of cavity m Energy density F i Bombarding the target material with laser to deposit the growth condition T on the substrate n P m F i Wherein T is n 、P m 、F i Respectively representing sequentially changing growth parameters. And moving the substrate to the next position, and repeating the film growth step.
According to the size of the hole-shaped structure of the movable mask plate 3 and the size of the substrate 21, epitaxial film samples with a plurality of different growth conditions can be grown at the same time, so that the optimization of the growth conditions of the epitaxial film can be quickened.
The invention provides a method for preparing epitaxial film samples with different cation defect concentrations based on the device for rapidly preparing oxide epitaxial films in batches, which comprises the following steps:
obtaining the optimal substrate temperature T on the basis of the rapid optimization of the growth conditions opt And cavity air pressure P opt And then the accurate control of different cation defects can be realized by changing the laser energy density. The target is arranged at a position opposite to the substrate, the center of the hole-shaped structure of the movable mask plate 3 is controlled to be positioned at the center of a light spot of laser on the surface of the target, the distance between the mask plate 3 and the substrate 21 is observed in real time through the monitor 54, and the distance between the mask plate 3 and the substrate 21 is controlled to be as close as possible, for example, less than 0.2 mm. Setting the temperature of the substrate to T opt The air pressure of the cavity is P opt And energy density F i Bombarding the target material with laser to deposit the growth condition T on the substrate opt P opt F i Is provided. Moving the substrate to the next position, setting the energy density F i+1 Bombarding the target material with laser to deposit the growth condition T on the substrate opt P opt F i+1 Is provided. Heavy weightThe film growth step is repeated n times, so that a plurality of epitaxial film samples with different cation defect concentrations can be obtained on the same substrate, namely, the control of the components of the epitaxial film is realized through simple lens position control.
(III) beneficial effects
(1) The substrate base 2 is movable in the XY plane for growing high flux samples, ensuring that the target sample position remains in the plume axis all the time.
The pulse laser deposition technology is to utilize the directional plasma plume ejected by the pulse laser bombarding the surface of the target material to deposit on the substrate to form a film, so that the plume has strong directivity. When the moving mask plate 3 deviates from the center of the plume, the film growth rate, composition, etc. are severely affected. Therefore, the invention proposes to move the center of the hole-like structure of the mask plate 3 to coincide with the center of the plume, and to realize high-throughput growth by moving the substrate base 2 in the XY plane, which enables more accurate and uniform growth control of each component point.
(2) The distance from the focal point of the lens 42 to the target surface is controlled by using the electric displacement table 43, so that the adjustment of the laser spot size and thus the laser energy density is realized.
The higher or lower laser energy density changes the composition of the film, e.g. for perovskite ABO 3 Oxide films are generally believed to have a higher laser energy density that causes vacancies in the a-site and a lower laser energy density that causes vacancies in the B-site. Therefore, the present invention proposes to pay attention to the important growth parameter of the laser energy density, and the electric displacement table 43 is used to realize the control of the laser spot size, so as to adjust the laser energy density within a certain range. The device can further accelerate the optimization of the growth conditions of the epitaxial film, and the research of the physical properties of the oxide epitaxial film by quantitatively researching the vacancy of A, B is possible.
(3) The monitoring system 5 is used to monitor the relative positions of the moving mask plate 3 and the substrate 21.
During film growth, the plume is blocked by obstacles to form uneven deposition at the edges to create shadow effects. Shadow effects not only affect the thickness and performance of the film, but also have a great negative effect on the accuracy of high-throughput growth. Therefore, it is necessary to bring the movable mask plate 3 close to the substrate 21 as much as possible. The invention adopts two high-definition cameras 51 and 52 which are vertically and orthogonally arranged to monitor the distance between the edge of the hole-shaped structure of the mask plate 3 and the edge of the substrate 21 and the distance between the mask plate 3 and the substrate 21 in real time. Through real-time monitoring, the invention can control the distance between the mask plate 3 and the substrate 21 to be less than 0.2 mm, which can effectively avoid serious shadow effect in the high-flux growth process.
Drawings
FIG. 1 is an overall schematic diagram of a high throughput thin film fabrication apparatus of the present invention.
FIG. 2 is a schematic diagram of a mask hole structure used in the present invention.
Fig. 3A is a schematic diagram of the fabrication of 10 epitaxial films with different growth conditions (or composition variations) on the same substrate using a moving mask hole pattern 311.
Fig. 3B is a schematic diagram of the fabrication of 20 epitaxial films with different growth conditions (or composition variations) on the same substrate using moving mask hole patterns 312 and 313.
Fig. 4A is a schematic diagram of the fabrication of a continuous graded epitaxial film on the same substrate using a moving reticle aperture structure 321.
Fig. 4B is a schematic diagram of the fabrication of a continuous graded epitaxial film on the same substrate using moving mask hole structures 322 and 323.
Fig. 5 is a flow chart for rapid optimization of epitaxial film growth conditions using a high throughput film preparation apparatus.
Fig. 6 is a flow chart of preparing epitaxial film samples of different cation defect concentrations using a high throughput film preparation apparatus.
Detailed Description
Detailed descriptionspecific embodiments of the invention are described (the accompanying drawings should be interpreted in light of the accompanying drawings, but the drawings are not to be substituted for the written description).
In the embodiments, not only the technical features related to the technical solution, but also relevant contents (such as a preparation process and equipment of a product, raw material sources, a molding state, an application range, a using method and the like, and implementation equipment and application range of the method and the like) which are helpful for understanding the invention are described in detail.
The number of embodiments will play a decisive role in defining the scope of protection of the inventive solution. If a broader scope is desired, a number of embodiments (e.g., the component structure may take many forms, names of various alternatives, structures, and alternatives thereof, the component content being regional, at least the two endpoints of the region and the specific formulation of the content of a point in the region with other components) should be given.
This example I describes the specific steps of using the hole structure 311 on the moving mask plate 31 in fig. 2 to grow epitaxial films with different growth conditions (or composition variations) on a size-matched substrate as shown in fig. 3A to achieve rapid optimization of the epitaxial film growth conditions:
(1) Installing a target and a substrate, and opening a valve to start vacuumizing after the target and the substrate 21 are placed oppositely;
(2) Adjusting the Z value of the movable mask plate 3, and observing in real time through a monitor 54 to enable the distance between the movable mask plate and the substrate 21 to be smaller than 0.2 millimeter;
(3) Adjusting X, Y value of the movable mask plate 3 to enable the center position of the hole-shaped structure to be consistent with the center position of the laser spot;
(4) Setting the substrate base 2 as X 1 、Y 1 A value that makes the center position of the first sample area to be grown on the substrate 21 consistent with the center position of the hole-shaped structure of the movable mask plate 3;
(5) Setting the substrate temperature T 1 Pressure P of cavity 1 Energy density F 1 Wait for T 1 、P 1 Reaching the set value;
(6) Using an energy density of F 1 The laser of (2) bombards the target material, the pulse number N 1 Frequency f, deposition growth conditions on substrate T 1 P 1 F 1 Epitaxial thin of (a)A membrane;
(7) Setting the substrate base 2 as X 2 、Y 2 The value is that the central position of the second sample area to be grown on the substrate 21 is consistent with the central position of the hole-shaped structure of the movable mask plate 3, and the steps (5) and (6) are repeated;
(8) And after a predetermined number of film samples are grown on the same substrate, cooling and annealing are carried out, sampling is carried out, and corresponding test characterization is carried out.
The embodiment I can be extended according to practical requirements, for example, by using the hole structures 312, 313 to implement multiple epitaxial thin film growth with different growth conditions (or composition changes) on a small-sized substrate, or to implement growth of more discrete samples with different growth conditions (or composition changes) on a single substrate (as shown in fig. 3B).
In this example I, a series of epitaxial thin film samples can be grown on a single substrate with a single growth condition as a variable, while keeping other growth conditions unchanged, to investigate the relationship of the physical properties of the thin film with the growth conditions such as temperature, air pressure, energy density, etc.
In the embodiment I, the laser energy density F can be used as a single growth condition variable to realize the growth of a plurality of discrete component epitaxial film samples on a single substrate, so as to study the influence of component variation on the physical properties of the film material.
This example II describes the specific steps of using the aperture structure 321 on the moving mask plate 32 of fig. 2 to grow a continuously compositionally varying epitaxial film on a size-matched substrate as shown in fig. 4 to achieve rapid optimization of epitaxial film growth conditions:
(1) Installing a target and a substrate, and opening a valve to start vacuumizing after the target and the substrate 21 are placed oppositely;
(2) Adjusting the Z value of the movable mask plate 3, and observing in real time through a monitor 54 to enable the distance between the movable mask plate and the substrate 21 to be smaller than 0.2 millimeter;
(3) Adjusting X, Y value of the movable mask plate 3 to enable the center position of the hole-shaped structure to be consistent with the center position of the laser spot;
(4) Setting the substrate base 2 as X 1 、Y 1 A value that makes the center position of the first sample area to be grown on the substrate 21 consistent with the center position of the hole-shaped structure of the movable mask plate 3;
(5) Setting the substrate temperature T 1 Pressure P of cavity 1 Energy density F 1 Wait for T 1 、P 1 Reaching the set value;
(6) Using an energy density of F 1 The laser of (2) bombards the target material, the pulse number N 1 Deposition growth conditions on the substrate were T 1 P 1 F 1 Is a thin epitaxial film of (a);
(7) Setting the substrate base 2 as X 2 、Y 2 The value is that the central position of the second sample area to be grown on the substrate 21 is consistent with the central position of the hole-shaped structure of the movable mask plate 3, and the steps (5) and (6) are repeated;
(8) And after a predetermined number of film samples are grown on the same substrate, cooling and annealing are carried out, sampling is carried out, and corresponding test characterization is carried out.
The embodiment II can be extended according to practical requirements, for example, by using the hole structures 312, 313 to realize epitaxial film growth with multiple discrete component variations on a small-sized substrate, or to realize growth with more discrete component samples on a single substrate.
Wherein T is n 、P m 、F i Respectively representing sequentially changing growth parameters. And moving the substrate to the next position, and repeating the film growth step.
According to the size of the hole-shaped structure of the movable mask plate 3 and the size of the substrate 21, epitaxial film samples with a plurality of different growth conditions can be grown at the same time, so that the optimization of the growth conditions of the epitaxial film can be quickened.
Claims (8)
1. The device for rapidly preparing the oxide epitaxial films in batches is characterized by comprising a multi-target base, a substrate base capable of being controlled in a three-dimensional and precise mode, a movable mask plate, an optical path system capable of being adjusted and focused electrically and a two-way monitoring system.
2. An apparatus for rapid batch fabrication of epitaxial thin films of oxides as set forth in claim 1 wherein the three-dimensional precision controllable substrate pedestal is adapted to hold a heated substrate without additional protrusions around a fixed substrate platform to ensure a mask plate is proximate to the substrate surface.
3. An apparatus for rapid mass production of epitaxial oxide films according to claim 1, wherein the three-dimensionally precisely controllable substrate base is movable in three directions XYZ, wherein in-XY movement is used to grow high throughput samples, ensuring that the target sample position remains always in the center of the plume axis.
4. The apparatus for rapid mass production of epitaxial thin films of claim 1, wherein the movable mask plate is composed of a plurality of 304 or 316 stainless steel plates with different hole structures, and the movable mask plate is detachably replaced by a mask plate with different hole structures, and the center position of the hole structures can be kept aligned with the axial direction of the plume when the movable mask plate moves in parallel.
5. The apparatus for rapid mass production of epitaxial thin films of oxide according to claim 1, wherein the electrically adjustable focusing optical path system comprises a plurality of 45 ° mirrors, double-knife adjustable slits, lenses, an electric displacement table for mounting lenses, and manual absorbing sheets, and the laser spot size is adjustable by changing the distance from the focal point of the lenses to the target surface, thereby realizing precise control of laser energy density.
6. An apparatus for rapid mass production of epitaxial thin films of oxides as set forth in claim 1, wherein the two-way monitoring system is composed of two high-definition cameras, a monitor and a lamp, the two high-definition cameras being mounted at 90 degrees to each other, one of which is capable of observing whether the mask pattern edge is aligned with the substrate edge from the front side of the substrate, and the other of which is capable of observing the spacing between the mask and the substrate from the side of the substrate.
7. A method for preparing oxide epitaxial films in batches rapidly is characterized in that three main parameters including a hole site of a mask plate and a position of a substrate are fixed, a temperature T, an air pressure P and an energy density F are set, the substrate is moved to the next position, and the film growth steps are repeated, so that the purpose of optimizing epitaxial film growth conditions rapidly is achieved.
8. A method for rapid batch preparation of oxide epitaxial films, characterized in that after optimizing the growth conditions of the epitaxial films according to claim 7, the precise control of different cationic defects can be achieved by changing the laser energy density by electrically adjusting the focusing optical path system.
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