Experimental atomic layer deposition cavity and device integrated with four-probe tester

Abstract

The utility model discloses an experimental atomic layer deposition cavity and experimental atomic layer deposition equipment integrated with a four-probe tester, and belongs to the technical field of thin film deposition. According to the experimental atomic layer deposition cavity integrated with the four-probe tester, the cavity is formed, the four probes are arranged in the cavity, and the lifting mechanism and the gate valve are correspondingly arranged, so that in-situ detection of a deposited film can be realized in the deposition process, and the complicated operation process of repeatedly sampling in the deposition process is avoided; and moreover, the detection environment does not contain substances possibly causing oxidation of the deposited film, so that the detection result of the four probes can be ensured to be an accurate result of the deposited film. In addition, through the arrangement of the water cooling device, it is ensured that the four probes are not affected by the temperature as much as possible during detection, and the accuracy of the detection result is also ensured to a certain extent.

Description

Technical Field

[0001] The utility model relates to an experimental atomic layer deposition cavity and equipment integrating a four-probe tester, belonging to the technical field of thin film deposition. Background Art

[0002] Atomic Layer Deposition (ALD) technology is a special chemical vapor deposition technology. The process is to alternately introduce two different precursor sources into a heated vacuum cavity, so that the precursor sources alternately undergo saturated chemical adsorption on the substrate surface, thereby self-limiting the growth of a thin film with an atomic layer thickness. Compared with other thin film deposition technologies, atomic layer deposition has many incomparable advantages in the deposition of ultra-thin films, such as: precise controllability of the thin film thickness, high step coverage, low impurity content, excellent uniformity, etc. Therefore, in recent years, the types of thin films prepared by atomic layer deposition technology have increased rapidly, developing from only being able to deposit oxide thin films and sulfide thin films originally to being able to prepare nitride thin films and metal thin films nowadays.

[0003] For metal thin films, researchers usually focus on the electrical properties of the thin films. Therefore, the performance of the thin films is usually judged by measuring parameters such as the resistance, resistivity, and conductivity of the thin films after deposition. Currently, the four-probe method is usually used to measure parameters such as the resistance, resistivity, and conductivity of thin films; the four-probe method is to measure the current and voltage at the four ports of the thin film to be measured by using four equally spaced probes, so as to obtain parameters such as the resistance, resistivity, and conductivity of the measured thin film, which has the advantages of high measurement accuracy, good reliability, and simple operation, and is of great significance for the research, production, and quality control of semiconductor thin films. In addition, a four-probe tester is an electrical property test instrument with relatively simple operation. Only by making the metal probe in surface contact with the sample to be measured can test data be obtained. However, currently, usually after the thin film is deposited, the deposited sample is transferred out of the deposition equipment and then placed on the four-probe tester for detection. However, the metal thin film needs to be encapsulated during the transfer process, otherwise it is easy to oxidize and cause inaccurate measurement results; moreover, it is extremely inconvenient when measuring the thin film deposition parameters in the early experiments. If the four-probe tester can be integrated into the ALD equipment, the electrical properties of the conductive thin film can be measured in-situ, eliminating the cumbersome sample-taking steps and avoiding the influence of the oxide film generated by the contact of the sample with air on the test results.

[0004] However, if you want to integrate a four-probe tester into an experimental atomic layer deposition equipment to achieve in-situ monitoring, the following problems need to be overcome:

[0005] (1) The height of the vacuum cavity of the experimental atomic layer deposition equipment is usually relatively low, and the existing four-probe testers on the market cannot be directly integrated on the side of the vacuum cavity.

[0006] (2) The vacuum chamber of the experimental atomic layer deposition equipment usually has a flip-top design, and it is impossible to directly integrate the existing four-probe tester on the market above the vacuum chamber;

[0007] (3) If the four-probe tester is directly integrated with the vacuum chamber, during the experiment, the probe part of the four-probe tester will also be coated with a thin film, thus affecting the measurement results;

[0008] (4) The working temperature of the existing four-probe testers on the market is usually room temperature. If the four-probe tester is directly integrated with the vacuum chamber, the high temperature generated by the vacuum chamber during the experiment will affect the four-probe tester; Utility Model Content

[0009] In view of the above problems, the present utility model provides an experimental atomic layer deposition chamber and equipment integrated with a four-probe tester. Overcoming the deficiencies of the prior art, by using the experimental atomic layer deposition chamber integrated with the four-probe tester, in-situ electrical property testing of the deposited thin film can be carried out during the experiment, and test data such as resistance, resistivity, and conductivity can be obtained.

[0010] The above technical objectives of the present utility model are achieved through the following technical solutions:

[0011] An experimental atomic layer deposition chamber integrated with a four-probe tester, the experimental atomic layer deposition chamber integrated with the four-probe tester includes: a vacuum chamber base 1, a chamber cover 2, a four-probe 13, a cavity 12, and a lifting mechanism 5; wherein, the cavity 12 is located above the vacuum chamber base 1, a chamber cover 2 is arranged between the cavity 12 and the vacuum chamber base 1, the four-probe 13 is placed in the cavity 12, and a deposition chamber 17 is arranged inside the vacuum chamber base 1.

[0012] In an embodiment, a flap valve 15 is arranged on the chamber cover 2. When the chamber cover 2 is in a closed state, the connection and isolation between the deposition chamber 17 and the cavity 12 are realized through the opening and closing of the flap valve 15.

[0013] In an embodiment, a sample stage 4 for placing deposition samples is arranged in the deposition chamber 17, and the sample stage 4 is connected to the lifting mechanism 5.

[0014] In an embodiment, the experimental atomic layer deposition chamber integrated with the four-probe tester further includes an upper connecting rod 8 and a lower connecting rod 9. The vacuum chamber base 1 and the chamber cover 2 are connected through the upper connecting rod 8 and the lower connecting rod 9, and the upper connecting rod 8 and the lower connecting rod 9 are rotatably connected to realize the rotation of the chamber cover 2 in the horizontal direction.

[0015] In one embodiment, a threaded rod 10 is provided inside the upper connecting rod 8 and the lower connecting rod 9. A knob 11 is provided above the threaded rod. By rotating the knob 11, the length of the threaded rod 10 in the connecting rod is changed, so as to control the closing and separation of the upper connecting rod 8 and the lower connecting rod 9, and realize the up and down movement of the cavity cover 2.

[0016] In one embodiment, a water cooling device is provided inside the cavity 12 for cooling the cavity 12.

[0017] In one embodiment, the size of the flap valve 15 is larger than the size of the sample stage 4, so that the sample stage 4 can rise into the cavity 12 under the action of the lifting mechanism 5.

[0018] In one embodiment, the experimental atomic layer deposition cavity of the integrated four-probe tester further includes a heating device, and the heating device is arranged inside the vacuum cavity base 1 and below the deposition cavity 17.

[0019] In one embodiment, the deposition cavity 17 is provided with an air inlet 6 and an air outlet 7, and the deposition cavity 17 is communicated with the precursor source delivery pipeline and the vacuum pipeline through the air inlet 6 and the air outlet 7.

[0020] The present invention also provides an experimental atomic layer deposition device of an integrated four-probe tester, and the cavity of the experimental atomic layer deposition device of the integrated four-probe tester adopts the above-mentioned experimental atomic layer deposition cavity of the integrated four-probe tester.

[0021] Advantages of the present invention:

[0022] (1) In the present invention, a rotatable connecting rod is designed, and a threaded rod is arranged inside it, so that the cavity cover can move up and down and rotate around the connecting rod, which is convenient for opening the cavity to take samples and can conveniently integrate the four-probe tester above the cavity cover;

[0023] (2) In the present invention, a flap valve is designed. During the experiment, the flap valve is closed, and the probe and the vacuum cavity can be isolated. When in-situ testing is required, the flap valve is opened again. In this way, the influence on the test data after the probe is coated with film is avoided, and in-situ detection can be realized;

[0024] (3) In the present invention, a lifting mechanism is designed. During the test, the lifting mechanism can be adjusted to make the sample stage rise or fall, so as to realize the contact and separation between the four-probe and the sample surface;

[0025] (4) In the present invention, water cooling joints are arranged on both sides of the cavity, and a water cooling device can be connected, so that the metal probe is maintained at the working temperature, and the influence of the high temperature of the vacuum cavity on the test data is avoided. Description of the drawings

[0026] Figure 1 Schematic diagram of the internal structure of an experimental atomic layer deposition chamber integrated with a four-probe tester;

[0027] Figure 2 Schematic diagram of the back structure of an experimental atomic layer deposition chamber integrated with a four-probe tester;

[0028] Wherein, 1 - vacuum chamber base, 2 - chamber cover, 3 - heater, 4 - sample stage, 5 - lifting mechanism, 6 - inlet, 7 - outlet, 8 - upper connecting rod, 9 - lower connecting rod, 10 - threaded rod, 11 - knob, 12 - cavity, 13 - four-probe, 14 - flange, 15 - gate valve, 16 - water-cooling joint, 17 - deposition chamber. Detailed implementation manners

[0029] The following is a detailed description of the present utility model.

[0030] Embodiment 1

[0031] Referring to the attached Figure 1 , this embodiment provides an experimental atomic layer deposition chamber integrated with a four-probe tester, including a vacuum chamber base 1, a chamber cover 2, a four-probe 13, a cavity 12 and a lifting mechanism 5; wherein the cavity 12 is located above the vacuum chamber base 1, a chamber cover 2 is arranged between the cavity 12 and the vacuum chamber base 1, the four-probe 13 is placed in the cavity 12, and a deposition chamber 17 is arranged inside the vacuum chamber base 1.

[0032] A gate valve 15 is arranged on the chamber cover 2. When the chamber cover 2 is in a closed state, the communication and isolation between the deposition chamber 17 and the cavity 12 can be realized through the opening and closing of the gate valve 15.

[0033] A sample stage 4 for placing deposition samples is arranged in the deposition chamber 17, and the sample stage 4 can be lifted in position through the lifting mechanism 5. Thus, when it is necessary to detect the deposition samples with the four-probe 13, the sample stage 4 is raised to a position where it can contact the four-probe 13. When detection is not required, the sample stage 4 is lowered to the deposition position. Moreover, the communication and isolation between the deposition chamber 17 and the cavity 12 are realized through the opening and closing of the gate valve 15 to prevent the four-probe 13 from being coated during deposition.

[0034] It should be noted that the size of the gate valve 15 is larger than the size of the sample stage 4, so that the sample stage 4 can be raised into the cavity 12 under the action of the lifting mechanism 5.

[0035] To facilitate the integration of the four-probe tester and the atomic layer deposition chamber, and at the same time facilitate the loading and unloading of deposition samples, the chamber cover 2 of the present utility model is set to be rotatable and open. Specifically, as Figure 2As shown in the figure, an upper connecting rod 8 and a lower connecting rod 9 are provided on the back of the entire vacuum chamber base. The base 1 and the chamber cover 2 are connected by the upper connecting rod 8 and the lower connecting rod 9 at the back. The upper connecting rod 8 and the lower connecting rod 9 are rotatably connected. A threaded rod 10 is provided inside the upper connecting rod 8 and the lower connecting rod 9, and a knob 11 is provided above the threaded rod. By rotating the knob 11, the length of the threaded rod 10 in the connecting rod can be changed, so as to control the closing and separation of the upper connecting rod 8 and the lower connecting rod 9, and realize the up and down movement of the chamber cover 2. The rotatable connection between the upper connecting rod 8 and the lower connecting rod 9 enables the chamber cover 2 to rotate around the connecting rod, so as to facilitate the opening of the chamber cover 2 during the sampling process.

[0036] During the deposition process, a precursor source is usually introduced into the heated deposition chamber 17 to deposit a film on the deposited sample. Therefore, a heater 3 is also provided inside the vacuum chamber base 1 and below the deposition chamber 17 to heat the deposition chamber 17. Inlets 6 and outlets 7 are respectively provided on both sides of the deposition chamber 17, and the deposition chamber 17 is connected to the precursor source delivery pipeline and the vacuum pipeline through the inlets 6 and outlets 7.

[0037] It should be noted that this solution does not improve the external computer, analyzer, and the external precursor source delivery pipeline and vacuum pipeline. Therefore, the above parts are not shown in the drawings of this application.

[0038] Considering the possible influence of the high-temperature environment in the deposition chamber 17 on the four-probe 13, two water-cooling joints 16 are provided on the side wall of the cavity 12 in the solution of the present utility model to reduce the temperature of the cavity 12 by water-cooling.

[0039] The experimental atomic layer deposition chamber of this integrated four-probe tester can realize in-situ monitoring of the deposited thin film. Especially when determining the optimal deposition parameters of the thin film in the preliminary experiment, the specific use steps are as follows:

[0040] Step 1, rotate the knob 11 to raise the chamber cover 2, and rotate the upper connecting rod 8 and the lower connecting rod 9 to rotate the chamber cover 2 from directly above the chamber to the upper side of the chamber, so as to facilitate the placement of the deposited sample.

[0041] Step 2, place the deposited sample on the sample stage 4.

[0042] Step 3, rotate the upper connecting rod 8 and the lower connecting rod 9 to rotate the chamber cover 2 from the upper side of the chamber to directly above the chamber, and rotate the knob 11 to lower it to close the chamber cover 2.

[0043] Step 4, open the gate valve 15 to connect the cavity 12 with the vacuum chamber base 1.

[0044] Step 5, evacuate the entire chamber to vacuum.

[0045] Step 6: Close the gate valve 15 to separate the cavity 12 from the vacuum chamber base 1, preventing the four-probe from being coated with a film during the experiment;

[0046] Step 7: Connect to the water cooling system through the water cooling joint 16 to lower the temperature of the cavity 12 part, maintaining the four-probe at the working temperature and avoiding the influence of excessive temperature on subsequent tests;

[0047] Step 8: Maintain the reaction temperature of the vacuum chamber through the heater 3;

[0048] Step 9: The precursor source delivery pipeline allows the precursor source participating in the reaction to enter the deposition chamber 17 through the air inlet 6;

[0049] Step 10: The vacuum pipeline evacuates the by-products of the side reaction and the precursors that did not participate in the reaction through the air outlet 7;

[0050] Step 11: Conduct n-cycle ALD experiments;

[0051] Step 12: After the experiment, evacuate the vacuum chamber to a vacuum;

[0052] Step 13: Open the gate valve 15 and adjust the lifting mechanism 5 to raise the sample stage 4 until the sample can come into contact with the four-probe 13. Since the cavity 12 was in communication with the vacuum chamber base 1 during the vacuum pumping operation in step 5, when the gate valve 15 is opened, the cavity 12 does not contain substances that may cause oxidation of the deposited film, thus ensuring that the detection result of the four-probe 13 is the accurate result of the deposited film;

[0053] Step 14: Analyze the information collected by the four-probe through an external computer, analyzer and other four-probe test data analysis systems to obtain data;

[0054] Step 15: Adjust the lifting mechanism 5 to lower the sample stage 4 to the lowest point;

[0055] Step 16: If the data obtained from the test does not meet the requirements, steps 5 to 15 can be repeated until the electrical properties meet the requirements.

[0056] Step 17: Only one sampling is required for the whole process, and there is no need for repeated sampling.

[0057] The working principle of the present utility model:

[0058] The experimental atomic layer deposition cavity of the integrated four-probe tester is provided with a cavity 12, and the four probes are arranged in the cavity 12. The lifting mechanism 5 and the gate valve 15 are correspondingly arranged, so that in-situ detection of the deposited thin film can be realized during the deposition process, avoiding the complicated operation process of repeatedly taking samples during the deposition process. Moreover, since it is ensured that the detection environment does not contain substances that may cause oxidation of the deposited thin film, the detection result of the four probes 13 can be guaranteed to be the accurate result of the deposited thin film. In addition, through the setting of the water cooling device, it is ensured that the four probes are not affected by temperature as much as possible during detection, and to a certain extent, the accuracy of the detection result is also guaranteed.

[0059] Although the present utility model has been disclosed above with a preferred embodiment, it is not intended to limit the present utility model. Any person familiar with this technology can make various modifications and decorations without departing from the spirit and scope of the present utility model. Therefore, the protection scope of the present utility model should be defined by the claims.

Claims

1. An experimental atomic layer deposition chamber integrated with a four-probe tester, characterized in that: The experimental atomic layer deposition chamber of the integrated four-probe tester comprises: a vacuum chamber base (1), a chamber cover (2), four probes (13), a cavity (12) and a lifting mechanism (5); wherein the cavity (12) is located above the vacuum chamber base (1), a chamber cover (2) is arranged between the cavity (12) and the vacuum chamber base (1), the four probes (13) are placed in the cavity (12), and a deposition chamber (17) is arranged inside the vacuum chamber base (1).

2. The experimental atomic layer deposition chamber integrated with a four-probe tester according to claim 1, characterized in that: The chamber cover (2) is provided with a gate valve (15), and when the chamber cover (2) is in a closed state, the deposition chamber (17) and the cavity (12) are connected and isolated by opening and closing the gate valve (15).

3. The experimental atomic layer deposition chamber integrated with a four-probe tester according to claim 2, characterized in that: A sample stage (4) for placing a deposition sample is provided in the deposition chamber (17), and the sample stage (4) is connected to the lifting mechanism (5).

4. The experimental atomic layer deposition chamber integrated with a four-probe tester according to claim 3, characterized in that: The experimental atomic layer deposition chamber of the integrated four-probe tester also includes an upper connecting rod (8) and a lower connecting rod (9), the vacuum chamber base (1) and the chamber cover (2) are connected via the upper connecting rod (8) and the lower connecting rod (9), and the upper connecting rod (8) and the lower connecting rod (9) are rotatably connected to realize the rotation of the chamber cover (2) in the horizontal direction.

5. The experimental atomic layer deposition chamber integrated with a four-probe tester according to claim 4, characterized in that: The upper connecting rod (8) and the lower connecting rod (9) are provided with a threaded rod (10) inside, and a knob (11) is provided above the threaded rod. By rotating the knob (11), the length of the threaded rod (10) in the connecting rod is changed, thereby controlling the closing and separation of the upper connecting rod (8) and the lower connecting rod (9), thereby realizing the up and down movement of the cavity cover (2).

6. The experimental atomic layer deposition chamber integrated with a four-probe tester according to claim 1, characterized in that: A water cooling device is provided in the cavity (12) for cooling the cavity (12).

7. The experimental atomic layer deposition chamber integrated with a four-probe tester according to claim 5, characterized in that: The size of the gate valve (15) is larger than the size of the sample stage (4), so that the sample stage (4) can be lifted into the cavity (12) under the action of the lifting mechanism (5).

8. The experimental atomic layer deposition chamber integrated with a four-probe tester according to claim 1, characterized in that: The experimental atomic layer deposition chamber integrated with a four-probe tester further comprises a heating device, which is arranged inside the vacuum chamber base (1) and below the deposition chamber (17).

9. The experimental atomic layer deposition chamber integrated with a four-probe tester according to claim 1, characterized in that: The deposition chamber (17) is provided with an air inlet (6) and an air outlet (7), and the deposition chamber (17) is connected with a precursor source delivery pipeline and a vacuum pipeline through the air inlet (6) and the air outlet (7).

10. An experimental atomic layer deposition device integrated with a four-probe tester, characterized in that: The chamber of the experimental atomic layer deposition device integrated with a four-probe tester adopts the experimental atomic layer deposition chamber of the integrated four-probe tester according to any one of claims 1-9.

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