WO2021022965A1

WO2021022965A1 - Apparatus and method for high-throughput preparation of multi-component uniform film material

Info

Publication number: WO2021022965A1
Application number: PCT/CN2020/100901
Authority: WO
Inventors: 高克玮; 宋有朋; 乔利杰; 庞晓露; 颜鲁春; 杨会生
Original assignee: 北京科技大学
Priority date: 2019-08-06
Filing date: 2020-07-08
Publication date: 2021-02-11
Also published as: CN110396671A; DE112020001782T5; CN110396671B

Abstract

The present invention provides an apparatus and method for high-throughput preparation of a multi-component uniform film material, and relates to the technical field of film preparation. According to the apparatus and method, uniform film samples of different material components can be prepared through an experiment, so that the preparation efficiency is greatly improved. The apparatus comprises a reaction chamber. A deposition station flat plate, a driving system, and a sputtering target are arranged in the reaction chamber. The sputtering target is hung at the top of the reaction chamber. A plurality of rotary deposition micro-region units are arranged on the deposition station flat plate, penetrate through the deposition station flat plate and are rotatably connected to the deposition station flat plate. The rotary deposition micro-region units are connected to the driving system and can realize synchronous rotation under power driving of the driving system. The technical solution provided by the present invention is suitable for the process of preparing films by sputtering.

Description

Device and method for high-throughput preparation of multi-component uniform film material

【Technical Field】

The invention relates to the technical field of thin film preparation, in particular to a device and method for high-throughput preparation of multi-component uniform thin film materials.

【Background technique】

The research and development of new materials is a complex process. Under normal circumstances, developers can only prepare one single-component material at a time and test its related properties. This traditional material research method characterized by trial and error is not only time-consuming and labor-intensive, severely restricts the speed of material research and development, but also requires high research and development costs.

In view of this, more efficient experimental methods must be explored. The proposed high-throughput experimental method can complete the preparation and characterization of a large number of samples in a short time, thereby greatly improving the speed of research and development of new materials. Generally, the preparation methods of composite material film samples in high-throughput experiments mainly include co-deposition film method, discrete template coating method, and continuous template coating method. As far as the co-deposition thin film method is concerned, although a large number of thin film materials with different compositions can be prepared by magnetron sputtering co-deposition technology through one experiment, for a thin film material with a specific composition, the composition of the thin film in the corresponding area Uneven. In addition, the prepared sample must be characterized by the high-throughput characterization method of the microdomain, which is not suitable for the traditional and relatively mature characterization method, and the applicability is poor.

In view of the above-mentioned problems, it is necessary to study a high-throughput device and method for preparing multi-component uniform thin film materials to deal with the deficiencies of the prior art, so as to solve or alleviate one or more of the above-mentioned problems.

[Content of the invention]

In view of this, the present invention provides a high-throughput device and method for preparing multi-component uniform thin film materials, which can prepare a variety of uniform thin film samples with different material components through one experiment, which greatly improves the preparation efficiency.

On the one hand, the present invention provides a device for high-throughput preparation of multi-component uniform thin film materials, characterized in that the device includes a reaction chamber, and the reaction chamber is provided with a deposition table, a driving system, and a sputtering target. , The sputtering target is suspended on the top of the reaction chamber;

A plurality of rotary deposition micro-domain units are provided on the deposition platform plate, and the bottom of the rotary deposition micro-domain unit passes through the deposition platform plate and is rotatably connected with the deposition platform plate;

The rotary deposition micro-zone unit is connected with the driving system, and realizes synchronous rotation under the power drive of the driving system.

According to the above aspect and any possible implementation manner, an implementation manner is further provided. A first transmission gear is fixedly sleeved on the bottom end of each of the rotary deposition micro-domain units, and two adjacent first transmission gears are fixedly sleeved. The gears mesh with each other; one of the rotary deposition micro-domain units is also provided with an extension shaft at the bottom end, and a second transmission gear is fixedly sleeved on the extension shaft, and the second transmission gear is connected to the drive system .

According to the above aspect and any possible implementation manner, an implementation manner is further provided. The rotary deposition micro-area unit includes a sample stage, a coarse rotating shaft and a fine rotating shaft; the sample stage is arranged horizontally, and the lower part of the sample stage The surface is fixedly connected with the top end of the coarse rotating shaft, and the bottom end of the coarse rotating shaft is fixedly connected with the top end of the thin rotating shaft; the fine rotating shaft passes through the deposition table plate and is rotatable with the deposition table plate connection.

In the above aspect and any possible implementation manner, an implementation manner is further provided. The rotatable connection is a bearing connection, specifically: a plurality of bearings corresponding to the thin rotating shaft are arranged in the deposition platform plate , The thin rotating shaft passes through the middle hole of the bearing to realize the bearing connection.

According to the above aspect and any possible implementation manner, an implementation manner is further provided, the drive system includes a drive motor and a drive gear, the drive gear is fixedly sleeved on the motor shaft of the drive motor; The driving gear is in meshing connection with the second transmission gear.

The above aspect and any possible implementation manner further provides an implementation manner in which the drive motor and the inner wall of the reaction chamber are insulated from each other.

According to the above aspect and any possible implementation manner, an implementation manner is further provided, and a plurality of support rods for supporting the deposition platform plate are provided under the deposition platform plate.

According to the above aspect and any possible implementation manner, an implementation manner is further provided. The first transmission gear, the second transmission gear, and the drive gear all have a downward boss, and the convex Taichung is equipped with a fixed top wire.

On the other hand, the present invention also provides a method for preparing thin film materials using any one of the above-mentioned high-throughput apparatus for preparing multi-component uniform thin film materials, characterized in that the steps include:

S1. Place the target material of the required material composition on the sputtering target, and adjust the angle and height of the sputtering target;

S2: Place and fix the substrate on the sample stage of each rotating deposition micro-area unit;

S3: Turn on the drive motor to make each rotating deposition micro-region unit rotate synchronously;

S4: Turn on the sputtering switch and start sputtering coating;

S5: After the coating is completed, turn off the equipment, take out the samples, and obtain multiple uniform thin film samples with different material compositions.

The foregoing aspects and any possible implementation manners further provide an implementation manner. Before sputtering is started, the vacuum degree, air pressure, temperature, and sputtering power in the reaction chamber are adjusted according to the specific conditions of the coating.

Compared with the prior art, the present invention can obtain the following technical effects: multiple materials can be simultaneously deposited on a sample stage that can rotate independently in each micro area, so that a variety of thin film samples with different material compositions can be prepared through one experiment , And can ensure that the surface of each sample is a film with uniform composition; the present invention applies the high-throughput idea and method to the preparation of a multi-component uniform film, which greatly improves the preparation efficiency and accelerates the development and screening of new materials.

Of course, any product implementing the present invention does not necessarily need to achieve all the above-mentioned technical effects at the same time.

【Explanation of drawings】

In order to explain the technical solutions of the embodiments of the present invention more clearly, the following will briefly introduce the drawings needed in the embodiments. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained from these drawings without creative work.

Fig. 1 is a schematic structural diagram of a device for high-throughput preparation of multi-component uniform thin film materials provided by an embodiment of the present invention;

2 is a schematic diagram of the structure of a sample stage and a rotating shaft in a micro area unit provided by an embodiment of the present invention;

3 is a schematic diagram of the structure of a transmission gear and a drive gear provided by an embodiment of the present invention;

4 is a distribution diagram of deposited micro-regions provided by an embodiment of the present invention;

Fig. 5 is a distribution diagram of deposited micro-regions according to another embodiment of the present invention.

Among them, in the figure:

1- Sample stage; 2- Coarse rotating shaft; 3- Fine rotating shaft; 4- Bearing; 5- Deposition stage plate; 6-First transmission gear; 7- Boss; 8- Extension shaft; 9- Second transmission gear; 10 -Drive gear; 11-drive motor; 12-support rod; 13-insulation member; 14-first sputtering target; 15-second sputtering target; 16-fixed top wire.

【Detailed ways】

In order to better understand the technical solutions of the present invention, the embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

It should be clear that the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work shall fall within the protection scope of the present invention.

The terms used in the embodiments of the present invention are only for the purpose of describing specific embodiments, and are not intended to limit the present invention. The singular forms of "a", "said" and "the" used in the embodiments of the present invention and the appended claims are also intended to include plural forms, unless the context clearly indicates other meanings.

A device for high-throughput preparation of multi-component uniform thin-film materials, as shown in Figure 1, includes a reaction chamber. The reaction chamber is equipped with a deposition table, a driving system and a sputtering target. The sputtering target is suspended in the reaction chamber Among them, the deposition platform includes a deposition platform plate 5, a number of independent rotary deposition micro-area units are provided on the deposition platform plate 5, and each rotary deposition micro-area unit can be detached separately. A bearing is used to connect the fine rotating shaft of the micro area unit and the plate of the deposition table. Specifically, the plate 5 of the deposition table is provided with a number of through holes, and bearings 4 are arranged in the through holes. connection. A first transmission gear 6 is provided at the bottom of each rotary deposition micro-zone unit. All the first transmission gears 6 are arranged at the same level, and two adjacent first transmission gears 6 are meshed and connected to ensure rotation. The other first transmission gears can be rotated at one time, so as to achieve the purpose of power transmission.

As shown in FIG. 2, the rotary deposition micro-zone unit includes a horizontally arranged sample stage 1, the lower surface of the sample stage 1 is fixedly connected to the top end of the coarse rotating shaft 2, and the bottom end of the coarse rotating shaft 2 is fixedly connected to the top end of the fine rotating shaft 3. The thin rotating shaft 3 passes through the deposition platform plate 5 and the corresponding bearing 4, and is connected to the bearing 4 in bearing. The bottom of the thin rotating shaft 3 is sleeved with a first transmission gear 6. The sample stage 1 of the micro-zone unit on the surface of the deposition stage has a circular, rectangular or other arbitrary shape, and the thick and thin rotating shafts are all circular. The micro-zone unit shaft is thicker and thinner on the lower part, and is placed in the bearing groove without other fixing methods, which ensures the smooth rotation between the thin shaft and the bearing and is easy to disassemble and assemble. The thin rotating shaft of a certain micro-zone unit is longer than that of other micro-zone units (that is, the extension shaft 8 is provided), and a first transmission gear and a second transmission gear are sleeved on it to transmit power from the driving motor. When the first transmission gear and the second transmission gear are connected to the thin rotating shaft or the extension shaft 8, both are fixedly connected.

The driving system includes a driving motor 11 and a driving gear 10. The driving gear 10 is set on the shaft of the driving motor 11. The driving motor provides power and is driven by gears to provide power and power for the synchronous rotation of all deposition micro-region units on the surface of the deposition table. transmission. The thin rotating shaft 3 of one of the rotary deposition micro-zone units is provided with an extension shaft, and the extension shaft is sleeved with a second transmission gear 9 which is fixedly connected to the extension shaft. The second transmission gear 9 is in meshing connection with the driving gear 10. When the drive motor 11 works, it drives the drive gear 10 to rotate, the drive gear 10 drives the second transmission gear 9 to rotate, and the second transmission gear 9 drives the extension shaft and the rotary deposition microdomain unit to rotate, and at the same time the rotary deposition microdomain unit rotates upward. The first transmission gear 6 rotates following the rotation of the thin rotating shaft 3, which in turn drives the rotation of other first transmission gears 6, so as to realize the synchronous rotation of all rotating deposition micro-region units. The drive motor and the wall of the reaction chamber are insulated from each other to meet the requirements for other process parameters in the actual coating process.

All transmission gears and drive gears are provided with downward bosses, as shown in Figure 3, and are equipped with fixed jacks 16 in the bosses, so that they can be easily disassembled while being fixed to the shaft.

The four corners of the deposition platform plate 5 are respectively provided with a support rod 12, the height of the four support rods 12 is matched with other components such as rotating shafts, gears, etc., while providing support for the deposition platform plate, it can provide a certain arrangement for the drive system space. The support rod can be divided into upper and lower parts, and the middle is blocked by an insulating member 13, which is made of insulating materials such as insulating ceramics; or the support rod is made of insulating materials as a whole to achieve electrical isolation between the deposition table and the chamber.

The vacuum, air pressure, and temperature adjustment devices continue the structure and working principle of the traditional thin-film preparation device, which will not be repeated here.

The method of using the above-mentioned device for high-throughput preparation of multi-component uniform thin film materials specifically includes the following steps:

Step 1: After placing the target material of the required specific material composition on the sputtering target, adjust the angle and height of the sputtering deposition target;

Step 2: Place and fix the substrate on the sample stage of each micro area unit;

Step 3: After adjusting the vacuum, air pressure, temperature, power (that is, the power of the sputtering target deposition power source) and other required coating parameters, before the formal coating, turn on the drive motor, so that each micro area is driven by gear The unit rotates synchronously;

Step 4: Turn on the sputtering switch to start sputtering coating, and simultaneously deposit a variety of materials on the deposition table;

Step 5: After the coating is completed, turn off the equipment and take out the samples to obtain multiple uniform thin film samples with different material compositions.

Example 1

As shown in Figure 1, take the preparation of Cu(100-x)Crx (x=3.2, 4.5, 5.7, 6.5, 7.9, 9.2, 10, 6at.%) Cu-Cr alloy films with 7 different alloy compositions as an example. The high-purity copper (99.9995%) target and the high-purity chromium (99.95%) target are placed on two target positions respectively, and the angles of the two targets are adjusted to make it 45° to the horizontal. Among them, the copper target is a DC power source, and the chromium target is a radio frequency power source. After placing 7 silicon wafers with a size of 10mm×10mm in an acetone solution ultrasonically cleaned for 20 minutes, they were placed on 7 micro-area sample stages parallel to the two targets. Adjust the magnetron sputtering process parameters, the process parameters are: Cu target power 100W, Cr target power 100W, sputtering time 30min, air pressure 0.5Pa, vacuum degree 8×10-4Pa. Turn on the drive motor to make each micro area unit rotate synchronously, and turn on the target power source for sputtering coating. After the coating was completed, the samples were taken out and analyzed for the content and distribution of copper and chromium in 7 thin film samples by EDS spectrometer. As shown in Figure 4, the different gray scales of each deposited micro-region represent different alloying element compositions. Among them, the closer the sample to the copper target, the greater the gray scale (that is, the darker the color), and the higher the copper content. Correspondingly, the closer the sample to the chromium target, the smaller the gray scale (that is, the lighter the color) and the higher the chromium content. In addition, the composition uniformity of a single sample was analyzed by an EDS spectrometer, and the results showed that the composition uniformity of the sample was less than 1% in the range of 10mm×10mm.

Example 2

As shown in Figure 1, taking the preparation of Cu(100-xy)CrxTiy (3≤x≤10, 2≤y≤8at.%) copper-chromium-titanium alloy films with 45 different alloy compositions as an example, the high-purity copper ( 99.9995%) target, high-purity chromium (99.95%) target and high-purity titanium (99.995%) target are placed on three target positions respectively, and the angles of the three targets are adjusted so that they are 45° with the horizontal. Among them, the copper target position and the titanium target position are DC power sources, and the chromium target position is a radio frequency power source. The three targets are triangularly distributed and the angle between them is 120°. After placing 45 silicon wafers with a size of 10mm×10mm in an acetone solution for 20 minutes after ultrasonic cleaning, they were placed on 45 micro-area sample stages. Adjust the magnetron sputtering process parameters. The process parameters are: Cu target power 100W, Cr target power 100W, Ti target power 100W, sputtering time 30min, air pressure 0.5Pa, vacuum degree 8×10-4Pa. Turn on the drive motor to make each micro area unit rotate synchronously, and turn on the target power source for sputtering coating. After the coating was completed, samples were taken out and analyzed for the content and distribution of copper and chromium in 45 thin film samples by EDS spectrometer. As shown in Figure 5, the different gray scales of each deposited micro-region represent different alloying element compositions. Among them, the closer the sample to the copper target, the greater the gray scale (that is, the darker the color), and the higher the copper content. Correspondingly, the closer the sample to the chromium target or titanium target, the smaller the gray scale (that is, the lighter the color), and the higher the chromium and titanium content is correspondingly. In addition, the uniformity of the composition of a single sample was analyzed by EDS spectrometer. The results show that the uniformity of the sample composition is less than 1% in the range of 10mm×10mm.

The device and method for high-throughput preparation of multi-component uniform thin film materials provided by the embodiments of the present application have been described in detail above. The description of the above embodiments is only used to help understand the method and core idea of this application; at the same time, for those of ordinary skill in the art, according to the idea of this application, there will be changes in the specific implementation and the scope of application. In summary, the content of this specification should not be construed as a limitation on this application.

For example, certain words are used in the specification and claims to refer to specific components. Those skilled in the art should understand that hardware manufacturers may use different terms to refer to the same component. This specification and claims do not use differences in names as a way to distinguish components, but use differences in functions of components as a criterion for distinguishing. As mentioned in the entire specification and claims, "including" and "including" are open-ended terms, so they should be interpreted as "including/including but not limited to". "Approximately" means that within an acceptable error range, those skilled in the art can solve the technical problem within a certain error range, and basically achieve the technical effect. The subsequent description of the specification is a preferred embodiment for implementing the application, but the description is for the purpose of explaining the general principles of the application and is not intended to limit the scope of the application. The protection scope of this application shall be subject to those defined by the appended claims.

It should also be noted that the terms "include", "include" or any other variants thereof are intended to cover non-exclusive inclusion, so that a commodity or system including a series of elements not only includes those elements, but also includes Other elements of, or also include elements inherent to this commodity or system. If there are no more restrictions, the element defined by the sentence "includes one..." does not exclude the existence of other identical elements in the commodity or system that includes the element.

It should be understood that the term "and/or" used herein is only an association relationship describing associated objects, indicating that there can be three types of relationships, for example, A and/or B can mean: A alone exists, and both A and A B, there are three cases of B alone. In addition, the character "/" in this text generally indicates that the associated objects before and after are in an "or" relationship.

The above description shows and describes several preferred embodiments of this application, but as mentioned above, it should be understood that this application is not limited to the form disclosed herein, and should not be regarded as an exclusion of other embodiments, but can be used for each Other combinations, modifications, and environments can be modified through the above teachings or technology or knowledge in related fields within the scope of the application concept described herein. The modifications and changes made by those skilled in the art do not depart from the spirit and scope of this application, and should fall within the protection scope of the appended claims of this application.

Claims

A device for high-throughput preparation of multi-component uniform thin-film materials is characterized in that the device comprises a reaction chamber in which a deposition platform plate, a driving system and a sputtering target are arranged, and the sputtering target Hung on the top of the reaction chamber;

A plurality of rotary deposition micro-domain units are provided on the deposition platform plate, and the bottom of the rotary deposition micro-domain unit passes through the deposition platform plate and is rotatably connected with the deposition platform plate;

The rotary deposition micro-zone unit is connected with the driving system, and realizes synchronous rotation under the power drive of the driving system.
The device for high-throughput preparation of multi-component uniform thin film materials according to claim 1, wherein the bottom end of each of the rotary deposition micro-domain units is fixedly sleeved with a first transmission gear, and two adjacent ones The first transmission gears mesh with each other; one of the rotary deposition micro-region units is also provided with an extension shaft at the bottom end, and a second transmission gear is fixedly sleeved on the extension shaft, and the second transmission gear is The drive system connection.
The device for high-throughput preparation of multi-component uniform thin film materials according to claim 1, wherein the rotary deposition micro-domain unit includes a sample stage, a coarse rotating shaft and a fine rotating shaft; the sample stage is arranged horizontally, the The lower surface of the sample stage is fixedly connected to the top end of the coarse rotating shaft, and the bottom end of the coarse rotating shaft is fixedly connected to the top end of the thin rotating shaft; the fine rotating shaft passes through the deposition table plate and is connected to the deposition table Rotatable connection of the plate.
The device for high-throughput preparation of multi-component uniform thin film materials according to claim 3, characterized in that the rotatable connection is a bearing connection, specifically: a plurality of thin films are arranged in the deposition platform plate. The bearing corresponding to the rotating shaft, the thin rotating shaft passes through the middle hole of the bearing to realize the bearing connection.
The device for high-throughput preparation of multi-component uniform thin film materials according to claim 2, wherein the drive system comprises a drive motor and a drive gear, and the drive gear is fixedly sleeved on the motor shaft of the drive motor On; the drive gear and the second transmission gear meshing connection.
The device for high-throughput preparation of multi-component uniform thin film materials according to claim 5, wherein the driving motor and the inner wall of the reaction chamber are insulated from each other.
The device for high-throughput preparation of multi-component uniform thin-film materials according to claim 1, wherein a plurality of support rods for supporting the deposition table are provided under the deposition table.
The device for high-throughput preparation of multi-component uniform thin film materials according to claim 5, wherein the first transmission gear, the second transmission gear and the drive gear all have downward bosses , The boss is equipped with a fixed top wire.
A method for preparing thin film materials using the high-throughput device for preparing multi-component uniform thin film materials according to any one of claims 1-8, characterized in that, the steps include:

S1. Place the target material of the required material composition on the sputtering target, and adjust the angle and height of the sputtering target;

S2: Place and fix the substrate on the sample stage of each rotating deposition micro-area unit;

S3: Turn on the drive motor to make each rotating deposition micro-region unit rotate synchronously;

S4: Turn on the sputtering switch and start sputtering coating;

S5: After the coating is completed, turn off the equipment, take out the samples, and obtain multiple uniform thin film samples with different material compositions.
The apparatus for high-throughput preparation of multi-component uniform thin film materials according to claim 9, characterized in that, before sputtering, the vacuum, air pressure, temperature and sputtering power in the reaction chamber are adjusted according to the specific conditions of the coating.