A high-throughput in-situ X-ray diffraction test device

Abstract

The present invention provides a high-throughput in-situ X-ray diffraction testing device, which is suitable for testing integrated circuit thin film materials grown on a disk to be tested, and comprises an upper cover, a main frame and a movable adjustment component arranged in sequence from top to bottom, and a heating ceramic disk is arranged in a cavity formed between the upper cover, the main frame and the movable adjustment component. The high-throughput in-situ X-ray diffraction testing device of the present invention arranges a heating ceramic disk in the cavity of the device, and heats the disk to be tested to a maximum of 300 degrees Celsius by heating the ceramic disk, so that a variable temperature in-situ X-ray diffraction experiment can be performed.

Description

Technical Field

[0001] The invention relates to the field of in-situ testing, in particular to a high-throughput in-situ X-ray diffraction testing device, which is suitable for integrated circuit thin film materials grown on 8-inch silicon wafers. Background Art

[0002] With the development of high-throughput preparation technology, in-situ research platforms for high-throughput testing methods of semiconductor materials are becoming increasingly important.

[0003] Traditional offline characterization makes it difficult to study the multi-dimensional parameter effects of materials such as nucleation, growth, and orientation evolution. Synchrotron radiation sources have the characteristics of high brightness, wide band, narrow pulses, and high temporal and spatial resolution, which are conducive to the realization of high-throughput in-situ characterization of microstructures. For high-throughput prepared composite material samples, corresponding in-situ characterization equipment based on synchrotron radiation sources and related data processing methods are developed. Summary of the invention

[0004] The purpose of the present invention is to provide a high-throughput in-situ X-ray diffraction testing device to realize a variable-temperature in-situ X-ray diffraction experiment.

[0005] In order to achieve the above-mentioned purpose, the present invention provides a high-throughput in-situ X-ray diffraction testing device, which is suitable for testing integrated circuit thin film materials grown on a disk to be tested, comprising an upper cover, a main frame and a movable adjustment component arranged in sequence from top to bottom, and a heating ceramic disk is provided in the cavity formed among the upper cover, the main frame and the movable adjustment component.

[0006] The upper cover comprises a bottom support frame, a plurality of side structures respectively mounted on a plurality of edges of the bottom support frame, and a top structure, wherein the side structures are composed of the side support frame and the side panels.

[0007] A ventilation interface is installed on at least one side panel.

[0008] The support frame of the bottom surface is rectangular, and the side structure includes two trapezoidal side structures and two rectangular side structures. The side panels and top surface structures of the rectangular side structures are made of polymer materials.

[0009] The bottom surface and the side support frames of the upper cover are made of metal material, and the side panels of the trapezoidal side structure are made of metal sheets.

[0010] The movable adjustment component includes a rotation adjustment mechanism located below the main frame and a translation adjustment mechanism located below the rotation adjustment mechanism. The main frame, the upper cover and the rotation adjustment mechanism form a sealed cavity, and the heating ceramic plate is directly fixed on the rotating shaft of the rotation adjustment mechanism.

[0011] The rotation adjustment mechanism includes a base and a rotation shaft, the rotation adjustment mechanism and the base of the main frame are fastened by a first fastening screw group, the upper cover and the main frame are fastened by a second fastening screw group, and the rotation adjustment mechanism and the sliding block of the translation adjustment mechanism are fastened by a third fastening screw group; a screw-driven slider is provided on the translation adjustment mechanism, and the rotation adjustment mechanism is fixed to the slider of the translation adjustment mechanism; sealing rubber rings are provided between the upper cover and the main frame, and between the base of the rotation adjustment mechanism and the main frame.

[0012] The main frame is connected to a circulating cooling mechanism; a sinking platform which is recessed downward relative to the outer periphery is provided at the center of the main frame, and the circulating cooling mechanism includes a surrounding water pipe arranged in the sinking platform, and the water pipe is composed of a base with a water pipe groove and a top cover of the water pipe, and the two ends of the water pipe are respectively connected to two coolant interfaces on the outside of the main frame, and are connected to at least one water inlet pipe and at least one water outlet pipe through the coolant interface.

[0013] The heating ceramic disk is connected to a temperature sensor; a heating interface and a temperature measuring interface are provided on both sides of the rotation adjustment mechanism, the heating interface is connected to the heating power line of the heating ceramic disk, the temperature measuring interface is connected to the wire of the temperature sensor, and both the heating interface and the temperature measuring interface are connected to an external power supply.

[0014] A metal clamp is provided at the outer edge of the heating ceramic disk, and a plurality of metal pressing plates are evenly fixed on the metal clamp; during testing, the disk to be tested is directly placed on the heating ceramic disk and fixed on the heating ceramic disk by the metal pressing plates.

[0015] The high-throughput in-situ X-ray diffraction testing device of the present invention is provided with a heating ceramic disk in the cavity of the device, and the disk to be tested is heated to a maximum of 300 degrees Celsius by the heating ceramic disk, so that a variable temperature in-situ X-ray diffraction experiment can be performed.

[0016] In addition, the high-throughput in-situ X-ray diffraction testing device of the present invention uses PMMA material with excellent chemical stability, processability, light transmittance and insulation as the upper cover, and does not need to set up an additional observation window, thereby reducing the absorption of X-rays by the device.

[0017] Furthermore, the high-throughput in-situ X-ray diffraction testing device of the present invention realizes one translational degree of freedom and one rotational degree of freedom by setting a rotation adjustment mechanism and a rotation adjustment mechanism, and has excellent compatibility. By using the high-throughput in-situ X-ray diffraction testing device of the present invention, real-time online characterization of three experimental methods: X-ray diffraction, reflectivity, and grazing incidence can be achieved. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic diagram of the disassembled structure of the high-throughput in-situ X-ray diffraction testing device of the present invention. DETAILED DESCRIPTION

[0019] The present invention provides a high-throughput in-situ X-ray diffraction test device, which is suitable for testing integrated circuit thin film materials grown on a disk to be tested (the disk to be tested is usually an 8-inch silicon wafer), and can be used to perform in-situ high-throughput synchrotron radiation X-ray diffraction characterization. Using the high-throughput in-situ X-ray diffraction test device of the present invention, in-situ measurements of X-ray diffraction, reflectivity, grazing incidence and other methods under high temperature and electric field can be performed, and by moving the disk to be tested, X-ray diffraction data of samples at different positions of the silicon wafer to be tested can be collected, that is, the point crystal structure of the thin film material at different positions of the disk to be tested can be tested to change with temperature.

[0020] like Figure 1 As shown, the high-throughput in-situ X-ray diffraction test device includes an upper cover 1, a main frame 2 and a movable adjustment component 3 which are arranged in sequence from top to bottom. Among them, a heating ceramic disk 4 is provided in the cavity formed between the upper cover 1, the main frame 2 and the movable adjustment component 3. The movable adjustment component 3 includes a rotation adjustment mechanism 31 located below the main frame 2 and a translation adjustment mechanism 32 located below the rotation adjustment mechanism 31. Therefore, the high-throughput in-situ X-ray diffraction test device of the present invention realizes one translational degree of freedom and one rotational degree of freedom by setting a rotation adjustment mechanism and a rotation adjustment mechanism. According to the test requirements, the diffraction at different positions on the same radius on the disk to be tested or the diffraction at different positions in the radial direction can be tested. Therefore, the compatibility performance is excellent. The high-throughput in-situ X-ray diffraction test device of the present invention can realize the real-time online characterization of the three experimental methods of X-ray diffraction, reflectivity and grazing incidence.

[0021] The upper cover 1 has a support frame on the bottom surface, a plurality of side structures respectively installed on the multiple edges of the support frame on the bottom surface, and a top surface structure, and the side structures are composed of the side support frame and the side panels. A ventilation interface 11 is installed on at least one side panel. In this embodiment, the number of ventilation interfaces 11 is 2, one ventilation interface 11 is used to introduce inert protective gas or experimental reaction gas in high temperature experiments, and the other ventilation interface 11 is used to exhaust to maintain a fixed internal air pressure. In this embodiment, the support frame on the bottom surface of the upper cover 1 is rectangular, and the side structure includes two trapezoidal side structures and two rectangular side structures. The support frames on the bottom and sides of the upper cover 1 are made of metal materials. In this embodiment, the support frames are formed by welding stainless steel bars. The side panels of the trapezoidal side structure are made of metal sheets such as stainless steel sheets, and the side panels are connected to the support frame on the side of the upper cover 1 by welding. The side panels and top surface structures of the rectangular side structures are made of PMMA materials, so that the rectangular side structures and top surface structures constitute the input, output and experimental observation windows of X-rays. The high-throughput in-situ X-ray diffraction testing device of the present invention uses PMMA material with excellent chemical stability, processability, light transmittance and insulation as the upper cover, and does not need to set up an additional observation window, thereby reducing the absorption of X-rays by the device.

[0022] The main frame 2 is used to connect the upper cover 1 and the rotation adjustment mechanism 31 of the movable adjustment assembly 3, and the main frame 2, the upper cover 1 and the rotation adjustment mechanism 31 form a sealed cavity.

[0023] Specifically, the rotation adjustment mechanism 31 and the main frame 2 are fastened by a first fastening screw group 61, the support frame on the bottom surface of the upper cover 1 and the main frame 2 are fastened by a second fastening screw group 62, and the rotation adjustment mechanism 31 and the sliding block of the translation adjustment mechanism 32 are fastened by a third fastening screw group 63. The support frame on the bottom surface of the upper cover 1 is provided with a uniform number of upper cover threaded holes. In this embodiment, the number of upper cover threaded holes is 16. The main frame 2 is provided with through holes corresponding to the upper cover threaded holes, and the main frame 2 and the upper cover threaded holes are fastened by the second fastening screw group 62. The rotation adjustment mechanism 31 includes a base and a rotation shaft, and the main frame 2 is fixed to the base of the rotation adjustment mechanism 31. The translation adjustment mechanism 32 is provided with a slider driven by a screw, and the rotation adjustment mechanism 31 is fixed to the slider of the translation adjustment mechanism 32.

[0024] Sealing rubber rings are provided between the support frame on the bottom surface of the upper cover 1 and the main frame 2, and between the base of the rotating adjustment mechanism 31 and the main frame 2. The sealing rubber rings are compressed by tightening the support frame on the bottom surface of the upper cover 1 and the main frame 2, and by tightening the base of the rotating adjustment mechanism 31 and the main frame 2, so that the cavity formed by the main frame 2, the upper cover 1 and the rotating adjustment mechanism 31 is more tightly sealed, thereby improving the airtightness of the entire system.

[0025] The main frame 2 is connected to a circulating cooling mechanism. Specifically, a sink that is recessed downward relative to the periphery is provided at the center of the main frame 2. The circulating cooling mechanism includes a surrounding water pipe arranged in the sink, and the water pipe is composed of a base with a water pipe groove and a top cover of the water pipe, thereby forming a cooling cavity for the coolant to pass through the two; the two ends of the water pipe are respectively connected to the two coolant interfaces 7 on the outside of the main frame 2, and are connected to at least one water inlet pipe and at least one water outlet pipe through the coolant interface 7. In this embodiment, the two ends of the water pipe are connected to the water inlet pipe and the water outlet pipe of the circulating water pump of the circulating cooling mechanism through the coolant interface 7, so as to cool the entire system. In this embodiment, the circulating water pump is a circulating water pump with scattering, which takes away the heat on the main frame through water circulation.

[0026] The heating ceramic disk 4 is connected to a temperature sensor for measuring the temperature in the main frame 2. In this embodiment, the temperature sensor is a temperature measuring thermocouple. Specifically, a heating interface 8 and a temperature measuring interface 9 are provided on both sides of the rotation adjustment mechanism 31, the heating interface 8 is connected to the heating power line of the heating ceramic disk 4, the temperature measuring interface 9 is connected to the wire of the temperature sensor, and the heating interface 8 and the temperature measuring interface 9 are both connected to an external power supply.

[0027] The heating ceramic disc 4 is directly fixed on the rotating shaft of the rotation adjustment mechanism 31, and can make circular motion along with the rotating shaft of the rotating mechanism. Specifically, the heating ceramic disc 4 is connected and fastened with the mounting hole on the rotating shaft through a fastening mechanism (such as a screw).

[0028] A metal clamp is provided at the outer edge of the heating ceramic disk 4, and a plurality of metal pressing plates are evenly fixed on the metal clamp, that is, a clamping device is provided at the outer edge of the heating ceramic disk 4. The function of the heating ceramic disk 4 is to heat the test disk 5. During the test, the disk 5 to be tested is directly placed on the heating ceramic disk 4 and is fixed on the heating ceramic disk 4 by the metal pressing plate. The disk 5 to be tested is a silicon wafer on which integrated circuit thin film materials are grown. The heating temperature of the heating ceramic disk 4 is from room temperature to 300 degrees Celsius. Therefore, the high-throughput in-situ X-ray diffraction test device of the present invention heats the 8-inch disk 5 to be tested to a maximum of 300 degrees Celsius by the heating ceramic disk 4 to conduct a variable temperature in-situ X-ray diffraction experiment.

[0029] The X-ray diffractometer has a three-dimensional adjustment device (i.e., a sample circle). The high-throughput in-situ X-ray diffraction test device of the present invention is fixed on the sample circle of the X-ray diffractometer, so that the device of the present invention can rotate with the sample circle of the diffractometer, support the symmetrical scanning mode in the X-ray diffraction experiment, and perform an online variable temperature test of the disk 5 to be tested.

[0030] The above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. The above embodiments of the present invention can also be modified in various ways. All simple, equivalent changes and modifications made according to the claims and the description of the present invention fall within the scope of protection of the claims of the present invention. The contents not described in detail in the present invention are all conventional technical contents.

Claims

1. A high-throughput in-situ X-ray diffraction testing device, which is suitable for testing integrated circuit thin film materials grown on a disk to be tested, characterized in that: It comprises an upper cover (1), a main frame (2) and a movable adjustment component (3) which are arranged in sequence from top to bottom, and a heating ceramic plate (4) is provided in a cavity formed between the upper cover (1), the main frame (2) and the movable adjustment component (3); The upper cover (1) comprises a bottom support frame, a plurality of side structures respectively mounted on a plurality of edges of the bottom support frame, and a top structure, wherein the side structures are each composed of a side support frame and a side panel; The movable adjustment component (3) comprises a rotation adjustment mechanism (31) located below the main frame (2) and a translation adjustment mechanism (32) located below the rotation adjustment mechanism (31); the main frame (2), the upper cover (1) and the rotation adjustment mechanism (31) form a sealed cavity; the heating ceramic plate (4) is directly fixed on the rotation shaft of the rotation adjustment mechanism (31); The rotation adjustment mechanism (31) comprises a base and a rotation shaft; the rotation adjustment mechanism (31) and the base of the main frame (2) are fastened by a first fastening screw group (61); the upper cover (1) and the main frame (2) are fastened by a second fastening screw group (62); and the rotation adjustment mechanism (31) and the sliding block of the translation adjustment mechanism (32) are fastened by a third fastening screw group (63); a slider driven by a screw is provided on the translation adjustment mechanism (32); the rotation adjustment mechanism (31) is fixed to the slider of the translation adjustment mechanism (32); sealing rubber rings are provided between the upper cover (1) and the main frame (2), and between the base of the rotation adjustment mechanism (31) and the main frame (2); A metal clamp is provided at the outer edge of the heating ceramic disk (4), and a plurality of metal pressing plates are evenly fixed on the metal clamp; during testing, the disk (5) to be tested is directly placed on the heating ceramic disk (4) and fixed to the heating ceramic disk (4) via the metal pressing plates.

2. The high-throughput in-situ X-ray diffraction testing device according to claim 1, characterized in that: A ventilation interface (11) is installed on at least one side panel.

3. The high-throughput in-situ X-ray diffraction testing device according to claim 1, characterized in that: The support frame of the bottom surface is rectangular, and the side structure includes two trapezoidal side structures and two rectangular side structures. The side panels and top surface structures of the rectangular side structures are made of PMMA material.

4. The high-throughput in-situ X-ray diffraction testing device according to claim 3, characterized in that: The bottom surface and side support frames of the upper cover (1) are made of metal material, and the side panels of the trapezoidal side structure are made of metal sheets.

5. The high-throughput in-situ X-ray diffraction testing device according to claim 1, characterized in that: The main frame (2) is connected to a circulating cooling mechanism; a sink is provided at the center of the main frame (2) and is recessed downward relative to the outer periphery; the circulating cooling mechanism comprises a surrounding water pipe provided in the sink, the water pipe comprising a base having a water pipe groove and a top cover of the water pipe, the two ends of the water pipe are respectively connected to two cooling liquid interfaces (7) on the outside of the main frame (2), and are connected to at least one water inlet pipe and at least one water outlet pipe via the cooling liquid interface (7).

6. The high-throughput in-situ X-ray diffraction testing device according to claim 1, characterized in that: The heating ceramic disk (4) is connected to a temperature sensor; a heating interface (8) and a temperature measuring interface (9) are provided on both sides of the rotation adjustment mechanism (31); the heating interface (8) is connected to a heating power line of the heating ceramic disk (4), and the temperature measuring interface (9) is connected to a wire of the temperature sensor; and both the heating interface (8) and the temperature measuring interface (9) are connected to an external power source.

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