Apparatus for testing the rate of corrosion of metal films and method of using same

Abstract

The application provides a device for testing the corrosion rate of a metal film, comprising a constant-temperature container. A first partition plate and a second partition plate are arranged in the constant-temperature container in the height direction of the constant-temperature container, and the first partition plate and the second partition plate divide the inner cavity of the constant-temperature container into a first cavity, a second cavity and a third cavity which are sequentially arranged. The first partition plate comprises a first movable part and a first fixed part connected with the first movable part, and the first movable part is used for controlling the communication between the first cavity and the second cavity. The second partition plate comprises a second movable part and a second fixed part connected with the second movable part, and the second movable part is used for controlling the communication between the second cavity and the third cavity. The application can avoid the influence of temperature on the corrosion rate and has high measurement accuracy. The application further provides a method for testing the corrosion rate of a metal film by using the device.

Description

Technical Field

[0001] This invention relates to the field of metal thin film corrosion rate testing technology, and in particular to a metal thin film corrosion rate testing device and its usage method. Background Technology

[0002] In semiconductor devices, metals are often used as conductors or barrier layers. Chemical mechanical polishing (CMP), as an effective planarization method in semiconductor device manufacturing, is frequently used to remove excess metal to achieve planarization. As the requirements for semiconductor devices become increasingly stringent, the number of patterned layers is also constantly increasing. During metal polishing, it is desirable to achieve a high metal removal rate while effectively controlling defects in the polished metal conductors, such as corrosion. Even minute corrosion in each layer can significantly reduce or even destroy the performance of the semiconductor device; therefore, controlling the corrosion rate of the polishing slurry on the metal is crucial.

[0003] Since the static corrosion rate of metal is entirely determined by the rate of chemical reaction between the polishing slurry and the metal film on the surface of the test piece, and this rate is closely related to the reaction temperature and reaction time, controlling these factors is crucial. However, existing testing devices cannot avoid the influence of temperature on the corrosion rate when measuring the corrosion rate of metal films, and the measurement accuracy is relatively poor. Summary of the Invention

[0004] Therefore, it is necessary to provide a testing device for the corrosion rate of metal thin films that can avoid the influence of temperature on the corrosion rate and has high measurement accuracy.

[0005] Furthermore, it is necessary to provide a method for testing the corrosion rate of metal thin films using the aforementioned testing apparatus.

[0006] At least one embodiment of the present invention provides a testing device for the corrosion rate of a metal thin film, comprising:

[0007] A thermostatic container, along the height direction of the thermostatic container, has a first partition and a second partition arranged in sequence, the first partition and the second partition dividing the inner cavity of the thermostatic container into a first cavity, a second cavity and a third cavity arranged in sequence;

[0008] The first partition includes a first movable part and a first fixed part connected to the first movable part. The first movable part is used to control the communication between the first cavity and the second cavity. The second partition includes a second movable part and a second fixed part connected to the second movable part. The second movable part is used to control the communication between the second cavity and the third cavity.

[0009] In some embodiments, the thermostatic container includes a sidewall, a bottom located at one end of the sidewall, and a cover located at the other end of the sidewall. The bottom and the cover are both connected to the sidewall and are disposed opposite to each other. The sidewall is a heating layer.

[0010] In some embodiments, the testing apparatus further includes a first timing device and a second timing device, wherein the first timing device is located on the outer surface of the sidewall corresponding to the first cavity, and the second timing device is located on the outer surface of the sidewall corresponding to the second cavity.

[0011] In some embodiments, the testing apparatus further includes a first driving device and a second driving device, wherein the first driving device is connected to the first movable part, and the second driving device is connected to the second movable part.

[0012] At least one embodiment of the present invention provides a method for testing the corrosion rate of a metal thin film using the aforementioned testing device, comprising the following steps:

[0013] A test piece with a metal thin film is provided, and the thickness of the metal thin film is measured to obtain a first thickness value;

[0014] The test piece is placed in the second cavity;

[0015] The polishing slurry is added to the first cavity, and the polishing slurry added to the first cavity is subjected to constant temperature treatment for a first predetermined time so that the temperature of the polishing slurry in the first cavity is a predetermined temperature.

[0016] The first movable part is opened to allow the polishing liquid in the first cavity to flow into the second cavity and immerse the test piece, so that the polishing liquid in the second cavity corrodes the metal film in the test piece, and the corrosion time is set to a second preset time;

[0017] Open the second movable part to allow the polishing liquid in the second cavity to flow into the third cavity;

[0018] The thickness of the metal film in the test piece after corrosion is measured to obtain a second thickness value, and the corrosion rate of the metal film is calculated based on the first thickness value, the second thickness value, and the second preset time; and

[0019] The metal ion content in the polishing fluid in the third cavity is tested, and the corrosion rate of the metal film is calculated based on the metal ion content.

[0020] In some embodiments, measuring the thickness of the metal thin film specifically includes the following steps:

[0021] A first measurement point is selected on the surface of the metal thin film;

[0022] The resistance of the metal thin film at the first measurement point was measured using a four-probe resistance meter to obtain a first resistance value; and

[0023] The thickness of the metal film at the first measurement point is calculated based on the first resistance value;

[0024] Measuring the thickness of the metal film in the corroded test piece specifically includes the following steps:

[0025] A second measurement point is selected on the surface of the corroded metal film, and the position of the second measurement point corresponds to the position of the first measurement point;

[0026] The resistance of the corroded metal film at the second measurement point was measured using a four-probe resistance meter to obtain a second resistance value; and

[0027] The thickness of the metal film at the second measurement point is calculated based on the second resistance value.

[0028] In some embodiments, the first predetermined time is 10 min to 60 min; and / or

[0029] The predetermined temperature is 25℃~75℃; and / or

[0030] The second preset time is 10 min to 60 min.

[0031] In some embodiments, testing the metal ion content in the polishing fluid in the third chamber specifically includes the following steps:

[0032] The content of metal ions in the polishing fluid in the third chamber was measured using inductively coupled plasma mass spectrometry.

[0033] In some embodiments, the polishing fluid is a chemical mechanical polishing fluid.

[0034] In some embodiments, the material of the metal thin film is selected from at least one of aluminum, copper, tantalum, titanium, tungsten, cobalt, ruthenium, and copper.

[0035] The testing apparatus provided by this invention includes a constant-temperature container, which maintains the temperature of the polishing solution and avoids the influence of polishing solution temperature, ambient temperature, and changes in ambient temperature on the corrosion rate of the metal film, thus improving measurement accuracy. Furthermore, the testing apparatus provided by this invention can test the corrosion rate of the metal film using two methods: one method measures the corrosion rate by measuring the thickness difference of the metal film; the other method measures the corrosion rate by testing the metal ion content in the polishing solution. Compared to using only one method, this invention employs two methods, resulting in more accurate measurement results and a wider range of applications. Attached Figure Description

[0036] Figure 1 A cross-sectional view of the testing apparatus provided by the present invention;

[0037] Figure 2 for Figure 1 Top view of the test apparatus shown;

[0038] Figure 3 for Figure 1 A schematic diagram of the structure of the first partition in the test device shown;

[0039] Figure 4 for Figure 1 A schematic diagram of the structure of the second partition in the test device shown;

[0040] Figure 5 For use Figure 1 The flowchart shown is a method for testing the corrosion rate of metal thin films using the test apparatus shown.

[0041] Reference numerals: 100-Testing device; 10-Thermostatic container; 101-Side wall; 102-Bottom; 103-Lid; 11-First cavity; 12-Second cavity; 13-Third cavity; 20-First partition; 201-First movable part; 202-First fixed part; 30-Second partition; 301-Second movable part; 302-Second fixed part; 40-First timing device; 50-Second timing device; 200-Test piece. Detailed Implementation

[0042] To facilitate understanding of the present invention, a more complete description will be given below with reference to the accompanying drawings. Preferred embodiments of the invention are shown in the drawings. However, the invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of the invention.

[0043] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the specification of this invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0044] Please see Figure 1 At least one embodiment of the present invention provides a testing device 100 for the corrosion rate of a metal thin film. The testing device 100 includes a constant temperature container 10, a first driving device (not shown), a second driving device (not shown), a first timing device 40, and a second timing device 50.

[0045] Please refer to the following: Figure 2 In one embodiment, the thermostatic container 10 is generally cylindrical. In another embodiment, the thermostatic container 10 includes a sidewall 101, a bottom 102 located at one end of the sidewall 101, and a lid 103 located at the other end of the sidewall 101. Both the bottom 102 and the lid 103 are connected to the sidewall 101, and the bottom 102 and the lid 103 are disposed opposite to each other. In one embodiment, the bottom 102 and the sidewall 101 are fixedly connected, and the lid 103 and the sidewall 101 are movably connected.

[0046] In one embodiment, the sidewall 101 is a heating layer. That is, the sidewall 101 can control the temperature inside the thermostatic container 10, thereby controlling the temperature of the substance placed inside the thermostatic container 10. The substance placed inside the thermostatic container 10 can be a solid or a gas. In one embodiment, the sidewall 101 can be a jacket structure. That is, the interior of the sidewall 101 is filled with water, and the temperature of the water can be changed. In other words, the temperature of the substance inside the thermostatic container 10 is controlled by controlling the temperature of the water.

[0047] In one embodiment, along the height direction of the thermostatic container 10, a first partition 20 and a second partition 30 are sequentially provided in the thermostatic container 10. The first partition 20 and the second partition 30 divide the inner cavity of the thermostatic container 10 into a first cavity 11, a second cavity 12, and a third cavity 13, which are sequentially distributed. That is, the first partition 20 separates the first cavity 11 and the second cavity 12, and the second partition 30 separates the second cavity 12 and the third cavity 13. Figure 1 As shown, the first cavity 11 is disposed near the cover 103, and the third cavity 13 is disposed near the bottom 102.

[0048] like Figure 1As shown, the cover 103, the side wall 101 and the first partition 20 together form the first cavity 11, the first partition 20, the side wall 101 and the second partition 30 together form the second cavity 12, and the second partition 30, the side wall 101 and the bottom 102 together form the third cavity 13.

[0049] Please see Figure 1 and Figure 3 In one embodiment, the first partition 20 includes a first movable part 201 and a first fixed part 202 connected to the first movable part 201. The first movable part 201 controls the communication between the first cavity 11 and the second cavity 12. In one embodiment, the first movable part 201 may be a movable plate, and the first fixed part 202 may be a fixed plate. When communication between the first cavity 11 and the second cavity 12 is required, only the movable plate needs to be opened. In one embodiment, the movable plate can open automatically and does not require manual opening.

[0050] Please see Figure 1 and Figure 4 In one embodiment, the second partition 30 includes a second movable part 301 and a second fixed part 302 connected to the second movable part 301. The second movable part 301 controls the communication between the second cavity 12 and the third cavity 13. In one embodiment, the second movable part 301 can also be a movable plate, and the second fixed part 302 can also be a fixed plate. When communication between the second cavity 12 and the third cavity 13 is required, only the movable plate needs to be opened. In one embodiment, the movable plate can also open automatically without manual opening.

[0051] In one embodiment, the first driving device and the first movable part 201 are connected. The first driving device drives the first movable part 201 to open or close it, thereby controlling whether the first cavity 11 and the second cavity 12 are connected.

[0052] In one embodiment, the second driving device and the second movable part 301 are connected. The second driving device drives the second movable part 301 to open or close it, thereby controlling whether the second cavity 12 and the third cavity 13 are connected.

[0053] Please see Figure 1 and Figure 2In one embodiment, the first timing device 40 is located on the outer surface of the sidewall 101 corresponding to the first cavity 11. The first timing device 40 is used for timing. That is, a time is set for the first timing device 40, and when that time is reached, the first driving device drives the first movable part 201 to open, thereby connecting the first cavity 11 and the second cavity 12.

[0054] The second timing device 50 is located on the outer surface of the side wall 101 corresponding to the second cavity 12. The second timing device 50 is used for timing. Specifically, a time is set for the second timing device 50, and when that time is reached, the second driving device drives the second movable part 301 to open, thereby connecting the second cavity 12 and the third cavity 13.

[0055] Please see Figure 5 At least one embodiment of the present invention provides a method for testing the corrosion rate of a metal thin film using the testing device 100, comprising the following steps:

[0056] Step S11, please refer to Figure 1 A test piece 200 with a metal thin film is provided, and the thickness of the metal thin film is measured to obtain a first thickness value.

[0057] Specifically, the test piece 200 with a metal thin film is provided, and a first measurement point is selected on the surface of the metal thin film. Then, a four-probe resistance meter is used to test the resistance of the metal thin film at the first measurement point to obtain a first resistance value. Finally, the thickness of the metal thin film at the first measurement point is calculated based on the first resistance value, i.e., the first thickness value is obtained. The number of the first measurement points can be one or more.

[0058] In one embodiment, the material of the metal thin film is selected from at least one of aluminum, copper, tantalum, titanium, tungsten, cobalt, ruthenium, and copper.

[0059] In one embodiment, the test device 200 may be a wafer. That is, the test device 200 having a metal thin film is a wafer having a metal thin film.

[0060] Step S12: Place the test piece 200 in the second cavity 12.

[0061] Specifically, the cover 103 is opened, and the test piece 200 is placed on the second partition 30. This allows the test piece 200 to be located in the second cavity 12.

[0062] Since the first movable part 201 can be opened, the test piece 200 can be placed on the second partition 30.

[0063] Step S13: Add polishing liquid to the first cavity 11 and perform constant temperature treatment on the polishing liquid added to the first cavity 11 for a first predetermined time, so that the temperature of the polishing liquid in the first cavity 11 is a predetermined temperature.

[0064] Specifically, a chemical mechanical polishing slurry is added to the first cavity 11, the cover 13 is placed on top, and the chemical mechanical polishing slurry added to the first cavity 11 is subjected to constant temperature treatment for 10 min to 60 min, so that the temperature of the chemical mechanical polishing slurry in the first cavity 11 is 25℃ to 75℃.

[0065] Due to the obstruction of the first partition 20, the chemical mechanical polishing liquid in the first cavity 11 will not flow into the second cavity 12.

[0066] Step S14: Open the first movable part 201 to allow the polishing liquid in the first cavity 11 to flow into the second cavity 12 and immerse the test piece 200, so that the polishing liquid in the second cavity 12 corrodes the metal film in the test piece 200, and set the corrosion time to a second preset time.

[0067] Specifically, the first driving device opens the first movable part 201 so that all the chemical mechanical polishing liquid in the first cavity 11 flows into the second cavity 12 and immerses the test piece 200, so that the chemical mechanical polishing liquid in the second cavity 12 corrodes the metal film in the test piece 200, and the corrosion time is set to 10 min to 60 min.

[0068] The temperature at which the metal film in the test piece 200 corrodes in the second cavity 12 is 25°C to 75°C.

[0069] Similarly, due to the obstruction of the second partition 30, the chemical mechanical polishing liquid in the second cavity 12 will not flow into the third cavity 13.

[0070] Step S15: Open the second movable part 301 to allow the polishing liquid in the second cavity 12 to flow into the third cavity 13.

[0071] Specifically, the second driving device opens the second movable part 301 so that all the chemical mechanical polishing liquid in the second cavity 12 flows into the third cavity 13.

[0072] Step S16: Measure the thickness of the metal film in the test piece 200 after corrosion to obtain a second thickness value, and calculate the corrosion rate of the metal film based on the first thickness value, the second thickness value and the second preset time.

[0073] Specifically, the cover 103 is opened, the corroded test piece 200 is taken out, and a second measurement point is selected on the surface of the corroded metal film, with the position of the second measurement point corresponding to the position of the first measurement point. Then, a four-probe resistance meter is used to test the resistance of the corroded metal film at the second measurement point to obtain a second resistance value. Finally, the thickness of the metal film at the second measurement point is calculated based on the second resistance value, i.e., the second thickness value is obtained. The corrosion rate of the metal film is then calculated according to the following formula:

[0074] Corrosion rate of metal thin film = (first thickness value - second thickness value) / second preset time.

[0075] In one embodiment, after removing the etched test piece 200 and before selecting the second measurement point, the etched test piece 200 can be rinsed with pure water to remove the residual chemical mechanical polishing fluid on the surface of the etched test piece 200.

[0076] The number of the second measurement points is the same as the number of the first measurement points, and the positions of the multiple second measurement points correspond one-to-one with the positions of the multiple first measurement points.

[0077] It is understandable that when both the first and second measurement points are one, a single result is obtained: the corrosion rate of the metal film at that measurement point. Conversely, when both the first and second measurement points are multiple, multiple results are obtained: the corrosion rates of the metal film at different measurement points. It is also understood that the corrosion rates of the metal film at different measurement points are approximately equal.

[0078] Step S17: Test the metal ion content in the polishing fluid in the third cavity 13, and calculate the corrosion rate of the metal film based on the metal ion content.

[0079] Specifically, the metal ion content in the chemical mechanical polishing slurry in the third chamber 13 was measured using inductively coupled plasma mass spectrometry (ICP-MS), and the corrosion rate of the metal film was calculated according to the following formula:

[0080] Corrosion rate of metal film = (Metal ion content in chemical mechanical polishing slurry in third chamber × Total mass of chemical mechanical polishing slurry in third chamber) / (Density of metal film × Area of ​​metal film in test piece × Second preset time).

[0081] The metal ion content in a chemical mechanical polishing slurry refers to the mass fraction of metal ions in the slurry.

[0082] The testing device 100 provided by this invention includes a constant temperature container 10, which can maintain the temperature of the polishing solution and avoid the influence of polishing solution temperature, ambient temperature, and changes in ambient temperature on the corrosion rate of the metal film, thereby improving the accuracy of the measurement. Furthermore, the testing device 100 provided by this invention can test the corrosion rate of the metal film using two methods. One method is to test the corrosion rate of the metal film by measuring the thickness difference; the other method is to test the corrosion rate of the metal film by measuring the content of metal ions in the polishing solution. Compared to testing with a single method, the present invention uses two methods, resulting in more accurate measurement results and a wider range of applications.

[0083] This invention measures the thickness of a metal film at a specific point, rather than measuring the overall thickness of the metal film. This solves the problem of inaccurate measurement results caused by uneven thickness of the metal film.

[0084] This invention employs two methods to test the corrosion rate of metal thin films, which can avoid the inability to calculate the corrosion rate due to the error of the four-probe resistance tester when the metal corrosion rate is too low.

[0085] The present invention will be further illustrated by specific embodiments below.

[0086] Example 1

[0087] (1) Provide a wafer with a metal thin film, and select a first measurement point on the surface of the metal thin film. Then, use a four-probe resistance meter to test the resistance of the metal thin film at the first measurement point to obtain a first resistance value. Finally, calculate the thickness of the metal thin film at the first measurement point based on the first resistance value, that is, obtain the first thickness value. The material of the metal thin film is copper.

[0088] (2) Open the cover and place the wafer on the second partition so that the wafer is located in the second cavity.

[0089] (3) The first polishing slurry is added to the first cavity, and the first polishing slurry added to the first cavity is subjected to constant temperature treatment for 20 minutes to make the temperature of the first polishing slurry in the first cavity reach a predetermined temperature. The predetermined temperature is 25℃. In the first polishing slurry, the mass fraction of silicon dioxide is 1%, the particle size of silicon dioxide is 80nm, the mass fraction of dipotassium ethylenediaminetetraacetate is 1%, the mass fraction of benzotriazole is 0.02%, the mass fraction of hydrogen peroxide is 1%, and the pH of the first polishing slurry is 7.00.

[0090] (4) The first movable part is opened by the first driving device so that all the first polishing liquid in the first cavity flows into the second cavity and immerses the wafer, so that the first polishing liquid in the second cavity etches the metal film in the wafer, and the etching time is set to 10 min. The etching temperature is the predetermined temperature mentioned above, that is, the etching temperature is 25°C.

[0091] (5) Open the second movable part by the second drive device so that all the first polishing liquid in the second cavity flows into the third cavity.

[0092] (6) Open the cover, remove the etched wafer, wash it with water, and select a second measurement point on the surface of the etched metal film, ensuring that the position of the second measurement point corresponds to the position of the first measurement point. Then, use a four-probe resistance meter to test the resistance of the etched metal film at the second measurement point to obtain the second resistance value. Finally, calculate the thickness of the metal film at the second measurement point based on the second resistance value, i.e., obtain the second thickness value, and calculate the corrosion rate of the metal film according to the following formula:

[0093] Corrosion rate of metal thin film = (first thickness value - second thickness value) / corrosion time.

[0094] (7) The mass fraction of metal ions in the first polishing solution in the third chamber was measured using inductively coupled plasma mass spectrometry (ICP-MS), and the corrosion rate of the metal film was calculated according to the following formula:

[0095] The corrosion rate of the metal thin film = (mass fraction of metal ions in the first polishing solution in the third chamber × total mass of the first polishing solution in the third chamber) / (density of the metal thin film × area of ​​the metal thin film in the wafer × corrosion time).

[0096] Example 2

[0097] The test method in Example 2 is basically the same as that in Example 1, except that:

[0098] In step (4), the etching time is 30 minutes.

[0099] Example 3

[0100] The test method in Example 3 is basically the same as that in Example 1, except that:

[0101] In step (3), the predetermined temperature is 55°C;

[0102] In step (4), the corrosion temperature is also 55°C.

[0103] Example 4

[0104] The test method in Example 4 is basically the same as that in Example 1, except that:

[0105] In step (1), the material of the metal film is cobalt.

[0106] Example 5

[0107] The test method in Example 5 is basically the same as that in Example 1, except that:

[0108] In step (1), the material of the metal film is tantalum;

[0109] In step (3), the predetermined temperature is 55°C;

[0110] In step (4), the corrosion temperature is also 55°C.

[0111] Example 6

[0112] The test method in Example 6 is basically the same as that in Example 1, except that:

[0113] In step (1), the material of the metal film is titanium.

[0114] Example 7

[0115] The test method in Example 7 is basically the same as that in Example 1, except that:

[0116] In step (3), the first polishing solution is changed to the second polishing solution. In the second polishing solution, the mass fraction of silica is 1%, the particle size of silica is 80 nm, the mass fraction of dipotassium ethylenediaminetetraacetate is 1%, the mass fraction of 1,2,4-triazole is 0.02%, the mass fraction of hydrogen peroxide is 1%, and the pH of the second polishing solution is 7.00.

[0117] In step (4), the etching time is 15 min.

[0118] Example 8

[0119] The test method in Example 8 is basically the same as that in Example 1, except that:

[0120] In step (1), the material of the metal film is tantalum.

[0121] In step (3), the first polishing solution is changed to the second polishing solution. In the second polishing solution, the mass fraction of silica is 1%, the particle size of silica is 80 nm, the mass fraction of dipotassium ethylenediaminetetraacetate is 1%, the mass fraction of 1,2,4-triazole is 0.02%, the mass fraction of hydrogen peroxide is 1%, and the pH of the second polishing solution is 7.00.

[0122] In step (4), the etching time is 15 min.

[0123] Example 9

[0124] The test method in Example 9 is basically the same as that in Example 1, except that:

[0125] In step (3), the first polishing solution is changed to the second polishing solution. In the second polishing solution, the mass fraction of silica is 1%, the particle size of silica is 80 nm, the mass fraction of dipotassium ethylenediaminetetraacetate is 1%, the mass fraction of 1,2,4-triazole is 0.02%, the mass fraction of hydrogen peroxide is 1%, and the pH of the second polishing solution is 7.00.

[0126] In step (3), the predetermined temperature is 35°C;

[0127] In step (4), the corrosion temperature is also 35°C and the corrosion time is 15 min.

[0128] Example 10

[0129] The test method in Example 10 is basically the same as that in Example 1, except that:

[0130] In step (3), the first polishing solution is changed to the second polishing solution. In the second polishing solution, the mass fraction of silica is 1%, the particle size of silica is 80 nm, the mass fraction of dipotassium ethylenediaminetetraacetate is 1%, the mass fraction of 1,2,4-triazole is 0.02%, the mass fraction of hydrogen peroxide is 1%, and the pH of the second polishing solution is 7.00.

[0131] In step (3), the predetermined temperature is 45°C;

[0132] In step (4), the corrosion temperature is also 45°C and the corrosion time is 15 min.

[0133] Example 11

[0134] The test method in Example 11 is basically the same as that in Example 1, except that:

[0135] In step (1), the material of the metal thin film is tungsten;

[0136] In step (3), the first polishing solution is changed to the third polishing solution. In the third polishing solution, the mass fraction of ferric nitrate is 0.1%, the mass fraction of malonic acid is 0.2%, the mass fraction of lysine is 0.005%, and the mass fraction of hydrogen peroxide is 1%. The pH of the third polishing solution is 2.0.

[0137] Example 12

[0138] The test method in Example 12 is basically the same as that in Example 1, except that:

[0139] In step (1), the material of the metal thin film is tungsten;

[0140] In step (3), the first polishing solution is changed to the third polishing solution. In the third polishing solution, the mass fraction of ferric nitrate is 0.1%, the mass fraction of malonic acid is 0.2%, the mass fraction of lysine is 0.005%, and the mass fraction of hydrogen peroxide is 1%. The pH of the third polishing solution is 2.0, and the predetermined temperature is 55°C.

[0141] In step (4), the corrosion temperature is also 55°C.

[0142] Example 13

[0143] The test method in Example 13 is basically the same as that in Example 1, except that:

[0144] In step (3), the first polishing solution is changed to the fourth polishing solution. In the fourth polishing solution, the mass fraction of silica is 8%, the particle size of silica is 60 nm, the mass fraction of citric acid is 0.5%, the mass fraction of polyvinylpyrrolidone is 0.2%, the mass fraction of benzotriazole is 0.01%, the mass fraction of hydrogen peroxide is 1%, and the pH of the fourth polishing solution is 10.50.

[0145] In step (4), the etching time is 30 minutes.

[0146] Example 14

[0147] The test method in Example 14 is basically the same as that in Example 1, except that:

[0148] In step (3), the first polishing solution is changed to the fourth polishing solution. In the fourth polishing solution, the mass fraction of silica is 8%, the particle size of silica is 60 nm, the mass fraction of citric acid is 0.5%, the mass fraction of polyvinylpyrrolidone is 0.2%, the mass fraction of benzotriazole is 0.01%, the mass fraction of hydrogen peroxide is 1%, the pH of the fourth polishing solution is 10.50, and the predetermined temperature is 55°C.

[0149] In step (4), the corrosion temperature is also 55°C and the corrosion time is 30 min.

[0150] The corrosion conditions and test results of Examples 1 to 14 are shown in Table 1 below.

[0151] Table 1 Corrosion conditions and test results of Examples 1-14

[0152]

[0153] It should be noted that the difference between the first and second thickness values ​​in Example 13 is negative, while the difference between the first and second thickness values ​​in Example 14 is zero. This is because the metal film corrosion rate is low in Examples 13 and 14, resulting in a small difference between the first and second thickness values. Furthermore, due to the measurement error inherent in the four-probe resistance meter, the difference between the first and second thickness values ​​is not positive. This also demonstrates that the two testing methods employed in this invention have a wider range of applications. That is, when testing by thickness difference is not possible, the mass fraction of metal ions can be used for testing.

[0154] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0155] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. A device for testing the corrosion rate of a metal film, characterized by The test device comprises: a constant-temperature container, a first partition plate and a second partition plate being arranged in sequence along the height direction of the constant-temperature container, the first partition plate and the second partition plate separating the inner cavity of the constant-temperature container into a first cavity, a second cavity and a third cavity arranged in sequence; wherein the first partition plate comprises a first movable part and a first fixed part connected with the first movable part, the first movable part being used for controlling the communication between the first cavity and the second cavity, the second partition plate comprises a second movable part and a second fixed part connected with the second movable part, the second movable part being used for controlling the communication between the second cavity and the third cavity; the constant-temperature container comprises a side wall, a bottom located at one end of the side wall and a cover located at the other end of the side wall, the bottom and the cover being connected with the side wall, and the bottom and the cover being oppositely arranged, the side wall being a heating layer; the test device further comprises a first timing device and a second timing device, the first timing device being located on the outer surface of the side wall corresponding to the first cavity, and the second timing device being located on the outer surface of the side wall corresponding to the second cavity.

2. The apparatus for testing the etching rate of a metal thin film according to claim 1, wherein the test device further comprises a first driving device and a second driving device, the first driving device being connected with the first movable part, and the second driving device being connected with the second movable part.

3. A method of testing the corrosion rate of a metal film using the test device of any one of claims 1 to 2, characterized by, The method comprises the following steps: providing a test piece with a metal film, and measuring the thickness of the metal film to obtain a first thickness value; placing the test piece in the second cavity; adding polishing liquid into the first cavity, and performing constant-temperature treatment on the polishing liquid added into the first cavity for a first predetermined time, so that the temperature of the polishing liquid in the first cavity is a predetermined temperature; opening the first movable part, so that the polishing liquid in the first cavity flows into the second cavity and immerses the test piece, so that the polishing liquid in the second cavity corrodes the metal film in the test piece, and the corrosion time is set as a second predetermined time; opening the second movable part, so that the polishing liquid in the second cavity flows into the third cavity; measuring the thickness of the metal film in the test piece after corrosion to obtain a second thickness value, and calculating the corrosion rate of the metal film according to the first thickness value, the second thickness value and the second predetermined time; and testing the metal ion content in the polishing liquid in the third cavity, and calculating the corrosion rate of the metal film according to the metal ion content.

4. The method for testing the corrosion rate of a metal thin film using the testing apparatus as described in claim 3, characterized in that, The step of measuring the thickness of the metal film comprises the following steps: selecting a first measurement point on the surface of the metal film; using a four-probe resistance tester to test the resistance of the metal film at the first measurement point to obtain a first resistance value; and calculating the thickness of the metal film at the first measurement point according to the first resistance value; The step of measuring the thickness of the metal film in the test piece after corrosion comprises the following steps: selecting a second measurement point on the surface of the metal film after corrosion, and making the position of the second measurement point correspond to the position of the first measurement point. adopting a four-probe resistance tester to test the resistance of the metal thin film at the second measuring point after corrosion, and obtaining a second resistance value; and calculating the thickness of the metal thin film at the second measuring point according to the second resistance value.

5. The method for testing the corrosion rate of a metal thin film using the testing apparatus as described in claim 3, characterized in that, The first predetermined time is 10 min to 60 min.

6. The method of testing the corrosion rate of a metal film according to claim 3, wherein The predetermined temperature is 25 DEG C to 75 DEG C.

7. The method of testing the corrosion rate of a metal film according to claim 3, wherein The second preset time is 10 min to 60 min.

8. The method for testing the corrosion rate of a metal thin film using the testing apparatus as described in claim 3, characterized in that, The test of the metal ion content in the polishing liquid in the third cavity specifically includes the following steps: Adopting an inductively coupled plasma mass spectrometer to test the metal ion content in the polishing liquid in the third cavity.

9. The method for testing the corrosion rate of a metal thin film using the testing apparatus as described in claim 3, characterized in that, The polishing liquid is a chemical mechanical polishing liquid.

10. The method for testing the corrosion rate of a metal thin film using the testing apparatus as described in claim 3, characterized in that, The material of the metal thin film is selected from at least one of aluminum, copper, tantalum, titanium, tungsten, cobalt, ruthenium and copper.

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