Atomic layer deposition method, and furnace tube device and vacuumizing method therefor

Abstract

The present invention relates to the technical field of semiconductor manufacturing. Disclosed are an atomic layer deposition method, and a furnace tube device and a vacuumizing method therefor. The atomic layer deposition method comprises: S100, placing a substrate into a reaction chamber, and vacuumizing the reaction chamber; S110, introducing a precursor into the reaction chamber until the precursor overspreads the surface of the substrate; S120, discharging the excess precursor; S130, introducing a reaction gas into the reaction chamber and fully reacting same with the precursor; and S140, vacuumizing the reaction chamber to a vacuum degree of 10-4 torr or less. After the reaction gas is introduced, the reaction chamber is vacuumized to a vacuum degree of 10-4 torr or less; therefore, the excess reaction gas and reaction byproducts can be rapidly pumped away, which is beneficial for reducing impurities in a film layer, improving film-forming quality and purity, and reducing the leakage current. The vacuum degree in the reaction chamber is 10-4 torr or less, which is beneficial for reducing by-products adsorbed onto the surface of the film layer, and the desorption of the by-products can further reduce the generation of impurities.

Description

Atomic layer deposition method, furnace tube device and vacuumizing method thereof TECHNICAL FIELD

[0001] The present application relates to the technical field of semiconductor manufacturing, in particular to an atomic layer deposition method, a furnace tube device and a vacuumizing method thereof. BACKGROUND

[0002] The material constituting the high dielectric constant (High-K) material layer, such as ZrO2, has a high dielectric constant, and can obtain a high capacitance value, but has a narrow band gap, and has the disadvantage of high leakage. In order to overcome this disadvantage, the conventional method is to introduce a wide band gap material layer, such as Al2O3, which has a lower dielectric constant but a wider band gap, into the High-K material. The composite capacitor dielectric structure formed by stacking the high dielectric constant material (such as ZrO2) and the wide band gap material (such as Al2O3) (ZAZ) can have the advantages of high dielectric constant and low leakage.

[0003] The stacked layer of high dielectric constant materials ZrO2 and Al2O3 is generally prepared by atomic layer deposition (ALD), but the prepared dielectric oxide layer generally contains a large amount of impurities such as C and H which are difficult to remove, which reduces the dielectric constant ε of the dielectric material layer, and further affects the leakage current and breakdown voltage of the film layer and other characteristics. SUMMARY

[0004] The present application provides an atomic layer deposition method, a furnace tube device and a vacuumizing method thereof, which is beneficial to reduce the impurities of the film layer and reduce the leakage current of the film layer.

[0005] The present application solves the above technical problems by the following technical solutions:

[0006] An atomic layer deposition method, comprising:

[0007] S100, placing a substrate in a reaction chamber, and vacuumizing the reaction chamber to a vacuum state;

[0008] S110, introducing a precursor into the reaction chamber until the surface of the substrate is fully covered;

[0009] S120, discharging excess precursor;

[0010] S130, introducing a reaction gas into the reaction chamber and fully reacting with the precursor;

[0011] S140, vacuumizing the vacuum degree of the reaction chamber to 10 -4 The following.

[0012] A furnace tube device, comprising:

[0013] an inner tube, an inner reaction chamber is formed inside the inner tube;

[0014] an outer tube, the outer tube is sleeved outside the inner tube, a gap region is formed between the outer tube and the inner tube, an exhaust port is arranged on the inner tube, so that the reaction chamber is communicated with the gap region;

[0015] an outer tube exhaust pipeline, provided with a first vacuum pump and a first valve, the first valve is arranged upstream of the first vacuum pump, the outer tube exhaust pipeline is communicated with the gap region;

[0016] an inner tube exhaust pipeline, provided with a second vacuum pump and a second valve, the second valve is arranged upstream of the second vacuum pump, the inner tube exhaust pipeline is communicated with the reaction chamber;

[0017] The limit vacuum degree of the second vacuum pump is greater than that of the first vacuum pump.

[0018] The positive progress effect of the present application is that:

[0019] The reaction chamber is evacuated before the precursor is introduced, which can remove the residual impurities in the reaction chamber and improve the cleanliness of the reaction chamber. After the reaction gas is introduced, the vacuum degree in the reaction chamber is extracted to 10 -4 Pa, which can quickly remove the excess reaction gas and reaction by-products, reduce the impurities in the film layer, improve the film forming quality and purity, and reduce the leakage current. Moreover, the vacuum degree in the reaction chamber is 10 -4 Pa, which is conducive to reducing the by-products adsorbed on the surface of the film layer, and the desorption of the by-products can further reduce the generation of impurities.

[0020] SUMMARY

[0021] The features and performances of the present application are further described by the following examples and drawings.

[0022] Fig. 1 is a flow chart of an atomic layer deposition method according to an embodiment of the present application;

[0023] Fig. 2 is a schematic diagram of a furnace tube device according to an embodiment of the present application;

[0024] Fig. 3 is a schematic diagram of a first structure of a furnace tube device according to an embodiment of the present application;

[0025] Fig. 4 is a schematic diagram of a second structure of a furnace tube device according to an embodiment of the present application;

[0026] Fig. 5 is a schematic diagram of a third structure of a furnace tube device according to an embodiment of the present application;

[0027] Fig. 6 is a schematic diagram of a furnace tube device according to an embodiment of the present application;

[0028] Figure 7 is a schematic diagram of a furnace tube apparatus according to an embodiment of the present application;

[0029] Figure 8 is a schematic diagram of a furnace tube apparatus according to an embodiment of the present application; and

[0030] Figure 9 is a timing diagram of the operation of a furnace tube apparatus according to an embodiment of the present application.

[0031] Preferred embodiments of the present application

[0032] The present application is further illustrated by the following examples without thereby limiting the present application to the examples.

[0033] Example 1

[0034] As shown in Figure 1, an atomic layer deposition method according to an embodiment of the present application comprises:

[0035] S100, placing a substrate in a reaction chamber and evacuating the reaction chamber to a vacuum state.

[0036] S110, introducing a precursor into the reaction chamber until the precursor covers the surface of the substrate.

[0037] S120, evacuating excess precursor.

[0038] S130, introducing a reaction gas into the reaction chamber and allowing the reaction gas to fully react with the precursor;

[0039] S140, evacuating the reaction chamber to a vacuum degree of 10 -4 torr or less.

[0040] In this embodiment, the reaction chamber is evacuated before the precursor is introduced, which evacuates impurities remaining in the reaction chamber and improves the cleanliness of the reaction chamber. After the precursor covers the surface of the substrate, excess precursor in the reaction chamber is evacuated, which further reduces impurities remaining in the reaction chamber. At this time, the reaction gas is introduced to react with the precursor on the surface of the substrate to form a first film layer. After the reaction gas fully reacts with the precursor, the vacuum degree in the reaction chamber is evacuated to 10 -4 torr or less, which evacuates excess reaction gas and reaction byproducts quickly, reduces impurities in the film layer, improves film formation quality and purity, and reduces leakage current. Moreover, the vacuum degree in the reaction chamber is 10 -4 torr or less, which facilitates the desorption of byproducts adsorbed on the surface of the film layer and further reduces the generation of impurities. By increasing the vacuum degree in the reaction chamber, impurities in the film layer are reduced, the purity of the film layer is improved, and the leakage current of the film layer is reduced.

[0041] In the embodiment, the cleaning gas is introduced in the step S120 and the step S140, and the cleaning gas is introduced for a preset time length. The cleaning gas is N2 or inert gas such as Ar, and the cleaning gas does not react with the precursor and the reaction gas. By introducing the cleaning gas, the excess precursor or reaction gas can be quickly exhausted.

[0042] In order to further reduce the impurities in the reaction chamber and improve the quality of the film, in the step S100 or the step S120 or the step S140, the vacuum degree in the reaction chamber can be extracted to 10 -5 The following.

[0043] In the embodiment, the step S110-S140 is repeated, and the predetermined film layer is deposited on the substrate until the film layer on the substrate reaches the predetermined thickness.

[0044] The method can be used to prepare any one of zirconium oxide, hafnium oxide, titanium zirconium oxide, titanium oxide, ruthenium oxide, antimony oxide, and aluminum oxide, or a stacked layer formed by two or more of the above.

[0045] The following will take the preparation of a zirconium oxide (ZrO2) and aluminum oxide (Al2O3) stacked layer as an example to describe the above process in detail.

[0046] The precursor for preparing ZrO2 can be selected from ZrCl4, Zr(N(CH3)C2H5)4, Zr(O-tBu)4, Zr(N(CH3)2)4, Zr(N(C2H5)(CH3))4, or other metal compounds containing Zr.

[0047] The precursor for preparing Al2O3 can be selected from Al(CH3)3, Al(C2H5)3, or other organometallic compounds containing Al.

[0048] The reaction gas can be selected from ozone (O3), oxygen (O2), O2 plasma, nitrogen oxide (N2O), N2O plasma, or H2O vapor, and can also contain other reaction gases with oxidation effect.

[0049] The step S100 is performed to extract the vacuum in the reaction chamber, and preferably, the vacuum degree is 10 -5 The following is to reduce the impurities in the reaction chamber and improve the quality of the subsequent film formation on the substrate.

[0050] The step S110 is performed to introduce the precursor Zr[N(CH3)C2H5]4 gas, and the Zr[N(CH3)C2H5]4 gas is introduced for a preset time length, so that the Zr[N(CH3)C2H5]4 gas covers the entire surface of the substrate and forms an adsorption layer on the surface of the substrate.

[0051] The step S120 is performed to introduce the cleaning gas, which can accelerate the exhaust of the excess Zr[N(CH3)C2H5]4.

[0052] Step S130 is performed to introduce the reaction gas O3 for a preset time period, so that the O3 reacts with the precursor Zr[N(CH3)C2H5]4 to form a ZrO2 thin film layer and by-products on the surface of the substrate.

[0053] Step S140 is performed to preferably evacuate the vacuum degree in the reaction chamber to 10 -5 Therefore, the excess reaction gas O3 and by-products can be evacuated to the maximum extent, which is beneficial to reduce the C, H and other impurities in the ZrO2 thin film layer and improve the film quality of the ZrO2 thin film layer and reduce the leakage current. Similarly, in step S140, a cleaning gas can also be introduced to accelerate the evacuation of the excess reaction gas O3 and by-products. Thus, the deposition of the first layer Z r O2 thin film is completed. r O2 thin film is completed.

[0054] After that, the above steps S110-S140 are repeated to deposit an Al2O3 thin film on the substrate, the precursor is selected as Al(CH3)3 and the reaction gas is selected as O3. After the deposition of the Al2O3 thin film is completed, the above steps S110-S140 can be continuously repeated to alternately deposit the ZrO2 thin film and the Al2O3 thin film to form a ZrO2 and Al2O3 stacked layer. The ZrO2 and Al2O3 stacked layer formed by the method is a High-K material, which has a low content of C, H and other impurities, which is beneficial to reduce the leakage current.

[0055] The above Zr[N(CH3)C2H5]4, Al(CH3)3 and O3 are introduced in the form of gas.

[0056] Example 2

[0057] As shown in Fig. 2, the furnace tube device provided in the embodiment can improve the vacuum pumping capacity of the furnace tube device, and comprises an inner tube 210, an outer tube 220, an inner tube pumping line 300, and an outer tube pumping line 400. The inner tube 210 is internally formed with a reaction chamber S1. The outer tube 220 is sleeved outside the inner tube 210, and a gap region S2 is present between the inner wall of the outer tube 220 and the outer wall of the inner tube 210. An exhaust port 211 is arranged on the inner tube 210 to communicate the reaction chamber S1 with the gap region S2. The outer tube pumping line 400 is provided with a first vacuum pump 411 and a first valve 412, the first valve 412 is arranged upstream of the first vacuum pump 411, and the outer tube pumping line 400 is in communication with the gap region S2. The inner tube pumping line 300 is provided with a second vacuum pump 311 and a second valve 312, the second valve 312 is arranged upstream of the second vacuum pump 311. One end of the inner tube pumping line 300 is in communication with the reaction chamber S1, and the other end of the inner tube pumping line 300 is connected to the outer tube pumping line 400 between the first vacuum pump 411 and the first valve 411. The inner tube pumping line 300 and the outer tube pumping line 400 share a common part, and the arrangement is more convenient.

[0058] In other embodiments, the other end of the inner tube pumping line 300 can also be connected to the outer tube pumping line 400 downstream of the dry pump 411.

[0059] In other embodiments, the inner tube pumping line 300 can also be independently arranged and not connected to the outer tube pumping line 400.

[0060] The limit vacuum degree of the second vacuum pump 311 is greater than the limit vacuum degree of the first vacuum pump 411. In the embodiment, the first vacuum pump 411 is selected as a dry pump, and the second vacuum pump 311 is selected as a molecular pump, and the limit vacuum degree of the molecular pump is higher than that of the dry pump.

[0061] In the embodiment, the inner tube pumping line 300 is in communication with the reaction chamber S1, the outer tube pumping line 400 is in communication with the gap region S2, and the outer tube pumping line 400 is provided with a dry pump 411. The dry pump 411 has high pumping efficiency under low vacuum, and the dry pump 411 can quickly exhaust the gas in the gap region S2 and the reaction chamber S1 region, and can pump the vacuum degree inside the furnace tube device to 10 -2 -10 -3 torr. The inner tube pumping line 300 is provided with a molecular pump 311, and the molecular pump 311 has higher pumping capacity under high vacuum than the dry pump 411, and the molecular pump 311 can further improve the vacuum degree in the reaction chamber S1. Under the cooperation of the dry pump 411 and the molecular pump 311, the furnace tube device has the ability to pump high vacuum, and the vacuum degree in the reaction chamber S1 can be pumped to 10 -5 torr or below.

[0062] In the embodiment, the exhaust ports 211 are arranged in multiple layers along the vertical direction of the inner tube 210, and the exhaust ports 211 of each layer are arranged in multiple in the circumferential direction of the inner tube, which is conducive to improving the uniformity of exhaust.

[0063] As shown in FIG. 2, the furnace tube device further comprises a first gas inlet pipe 510 and a second gas inlet pipe 520 for supplying precursors and process gases into the furnace tube device.

[0064] The furnace tube device is further provided with a third gas inlet pipe (not shown in the figure) for supplying cleaning gas into the furnace tube device.

[0065] In the embodiment, three different structures of furnace tube devices are provided.

[0066] I. As shown in FIG. 3, the furnace tube device further comprises a first gas extraction port 610 and a second gas extraction port 620, the first gas extraction port 610 is arranged on the inner tube 210 through the outer tube 220 and the gap area S2, the inner tube gas extraction pipe 300 is connected with the first gas extraction port 610 and communicates with the reaction chamber S1 through the first gas extraction port 610. The second gas extraction port 620 is arranged on the outer tube 220, the outer tube gas extraction pipe 400 is connected with the second gas extraction port 620 and communicates with the gap area S2 through the second gas extraction port 620.

[0067] II. As shown in FIG. 4, the furnace tube device further comprises a substantially cylindrical manifold 700 connected with the bottom ends of the inner tube 210 and the outer tube 220. The manifold 700 communicates with the reaction chamber S1 and does not communicate with the gap area S2, and the first gas extraction port 610 is arranged on the manifold 700 and communicates with the reaction chamber S1. The inner tube gas extraction pipe 300 is connected with the first gas extraction port 610 and communicates with the reaction chamber S1 through the first gas extraction port 610. The second gas extraction port 620 is arranged on the outer tube 220 above the first gas extraction port 610, and the outer tube gas extraction pipe 400 is connected with the second gas extraction port 620 and communicates with the gap area S2 through the second gas extraction port 620.

[0068] The first gas extraction port 610 is arranged on the manifold 700, which is conducive to reducing the processing difficulty of the inner tube 210 and the outer tube 220 compared with the first gas extraction port 610 arranged on the inner tube 210 through the outer tube 220 and the gap area S2. Moreover, the manifold is usually made of metal material, and arranging the first gas extraction port 610 on the manifold can also reduce the processing difficulty of the first gas extraction port 610.

[0069] III. As shown in FIG. 5, the manifold 700 includes a first region S3 and a second region S4, which are not in communication with each other, the first region S3 being in communication with the reaction chamber S1, and the second region S4 being in communication with the gap region S2. The first gas extraction port 610 is provided on the manifold 700, and the first gas extraction port 610 is in communication with the first region S3. The inner tube gas extraction pipeline 300 is connected to the first gas extraction port 610, and is in communication with the reaction chamber S1 through the first gas extraction port 610. The second gas extraction port 620 is provided on the manifold 700, and the second gas extraction port 620 is in communication with the second region S4. The outer tube gas extraction pipeline 400 is connected to the second gas extraction port 620, and is in communication with the gap region S2 through the second gas extraction port 620.

[0070] Specifically, the manifold 700 includes a first pipe 710 and a second pipe 720, one end of the second pipe 720 being connected to the inner tube 210 and the outer tube 220, and the other end of the second pipe 720 being connected to the first pipe 710. The first pipe 710 is a single-layer structure in a substantially cylindrical shape, and the second pipe 720 is a double-layer structure with a sandwiched hollow. The first region S3 is a region surrounded by the inner layer of the second pipe 720 and the first pipe 710, and the second region S4 is a sandwiched hollow region of the second pipe 720. The inner layer of the second pipe 720 has a smaller lateral dimension than the first pipe 710, and there is a step between the two. The first gas extraction port 610 is provided on the first pipe 710, and the second gas extraction port 620 is provided on the second pipe 720. The bottom end of the gap region S2 of the inner tube 210 and the outer tube 220 is provided with a communication port 800, and the second region S4 is in communication with the gap region S2 through the communication port 800. By opening the communication port 800 and modifying the structure of the manifold 700, the position of the second gas extraction port 620 can be set on the manifold.

[0071] The first gas extraction port 610 and the second gas extraction port 620 do not need to be provided on the inner tube 210 and the outer tube 220, the processing defects of the inner tube 210 and the outer tube 220 are reduced, and the sealing performance of the furnace tube equipment as a whole is better.

[0072] Embodiment 3

[0073] This embodiment is basically the same as the scheme of Embodiment 2, and the difference is that:

[0074] As shown in FIG. 6, the furnace tube equipment further includes a first branch pipeline 330, one end of the first branch pipeline 330 being connected to the outer tube gas extraction pipeline 400 upstream of the first valve 412, and the other end of the first branch pipeline 330 being connected to the inner tube gas extraction pipeline 300 upstream of the molecular pump 311.

[0075] The furnace tube equipment extracts high vacuum (for example, 10 -5When the vacuum degree of the reaction chamber S1 is to be increased to 5x10 -3 -2 Pa, the first valve 412 is closed, the molecular pump 311 and the second valve 312 are opened to further increase the vacuum degree of the reaction chamber S1. However, in this process, the gas in the outer-pipe evacuation pipeline 400 upstream of the first valve 412 can be evacuated into the reaction chamber S1, and the gas has poor cleanliness and can easily contaminate the film layer on the substrate. By adding the first branch pipeline 330, when the molecular pump 311 is working, the gas in the outer-pipe evacuation pipeline 400 upstream of the first valve 412 is evacuated by the molecular pump 311 through the first branch pipeline 330, avoiding the gas in the outer-pipe evacuation pipeline 400 upstream of the first valve 412 from flowing back and being re-evacuated into the reaction chamber S1.

[0076] In the embodiment, the third valve 331 is arranged on the first branch pipeline 330, and the first branch pipeline 330 is connected to the inner-pipe evacuation pipeline 300 upstream of the second valve 312.

[0077] In some embodiments, the third valve 331 can also be replaced by a flow restrictor. The flow restrictor can control the flow of the gas in the first branch pipeline 330, which has a similar effect to the third valve 331.

[0078] In some embodiments, the third valve 331 can also be replaced by a flow restrictor. The flow restrictor can control the flow of the gas in the first branch pipeline 330, which has a similar effect to the third valve 331.

[0079] The embodiment also provides a vacuum evacuation method of the furnace tube device. In the method, the dry pump 411 is always in an open state, and the vacuum evacuation method comprises the following steps:

[0080] S200, opening the dry pump 411 and the first valve 412 to evacuate the vacuum degree in the reaction chamber S1 to a first preset value.

[0081] S210, closing the first valve 412, opening the molecular pump 311 and the second valve 312, and opening the third valve 331 or the flow restrictor to continue evacuating the vacuum degree to a second preset value.

[0082] In the embodiment, the first preset value is, for example, 10-2-10 -3 -2 Pa. After the first preset value is reached, the first valve 412 is closed, the molecular pump 311 is opened, and the second valve 312 and the third valve 331 are opened, so that the vacuum degree of the reaction chamber S1 can be further increased to the second preset value, for example, 10 -4 -10 -5In this process, because the first valve 412 is closed and the third valve 331 is opened, the gas in the outer pipe exhaust pipeline 400 upstream of the first valve 412 is pumped away by the molecular pump 311 through the first branch pipeline 330, avoiding backflow into the reaction chamber S1 again, and further improving the cleanliness in the reaction chamber S1.

[0083] In this embodiment, the vacuum pumping method further comprises:

[0084] S220, close the molecular pump 311 and the second valve 312, and introduce clean gas into the reaction chamber S1, and after the vacuum degree in the reaction chamber S1 is lower than or equal to the vacuum degree in the outer pipe exhaust pipeline 400, open the first valve 412.

[0085] When the first valve 412 is opened, because the reaction chamber S1 is filled with clean gas and the vacuum degree is not higher than the vacuum degree in the outer pipe exhaust pipeline 400, the gas in the outer pipe exhaust pipeline 400 downstream of the first valve 412 will not be sucked back into the reaction chamber S1.

[0086] When it is necessary to introduce precursor and process gas into the reaction chamber S1, the third valve 331 or the flow restrictor is closed, and the second valve 312 is closed.

[0087] The first vacuum gauge (not shown in the figure) is arranged between the dry pump 411 and the first valve 412 of the outer pipe exhaust pipeline 400, and is used to detect the vacuum degree of the outer pipe exhaust pipeline 400. The second vacuum gauge (not shown in the figure) is arranged upstream of the first valve 412 of the outer pipe exhaust pipeline 400, and is used to detect the vacuum degree in the reaction chamber S1.

[0088] Embodiment 4

[0089] This embodiment is basically the same as the scheme of embodiment 2, and the difference is that:

[0090] As shown in FIG. 7, the furnace tube device further comprises a second branch pipeline 320, which is provided with a fourth valve 321, one end of the second branch pipeline 320 is connected to the outer pipe exhaust pipeline 400 between the dry pump 411 and the first valve 412, and the other end of the second branch pipeline 320 is connected to the inner pipe exhaust pipeline 300 upstream of the molecular pump 311.

[0091] The dry pump 411 can not only draw gas from the gap area S2 through the outer tube gas extraction pipeline 400, but also directly communicate with the reaction chamber S1 through the second branch pipeline 320. Taking the ALD process as an example, during the process of inputting the precursor or the reaction gas, the fourth valve 321 is closed, and the first valve 412 is opened to only communicate the outer tube gas extraction pipeline 400. During the process of vacuumizing or discharging excess precursors, the first valve 412 can be closed, and the fourth valve 321 is opened to directly extract gas from the reaction chamber S1 through the second branch pipeline 320, which is beneficial to improve the exhaust efficiency.

[0092] The embodiment also provides a vacuumizing method of the furnace tube device, in which the dry pump 411 is always in an open state, and the vacuumizing method comprises the following steps.

[0093] S300, opening the dry pump 411 and the fourth valve 321, closing the first valve 412, and vacuumizing the vacuum degree in the reaction chamber S1 to a first preset value.

[0094] S310, closing the fourth valve 321, opening the molecular pump 311 and the second valve 312, and continuing to vacuumize the vacuum degree to a second preset value.

[0095] The first preset value and the second preset value are the same as the scheme in the embodiment 3.

[0096] In the method, the dry pump 411 directly extracts gas from the reaction chamber S1 through the second branch pipeline 320, which has higher exhaust efficiency compared with extracting gas from the reaction chamber S1 through the outer tube gas extraction pipeline 400.

[0097] The vacuumizing method further comprises the following steps.

[0098] S320, closing the molecular pump 311 and the second valve 312, inputting the cleaning gas into the reaction chamber S1, and opening the first valve 412 after the vacuum degree in the reaction chamber S1 is lower than or equal to the vacuum degree in the outer tube gas extraction pipeline 400.

[0099] Embodiment 5

[0100] As shown in FIG. 8, the furnace tube device in the embodiment simultaneously comprises the first branch pipeline 330 in the embodiment 3 and the second branch pipeline 320 in the embodiment 4. The first branch pipeline 330 can avoid the gas in the outer tube gas extraction pipeline 400 upstream of the first valve 412 from flowing back into the reaction chamber S1, and the second branch pipeline 320 enables the dry pump 411 to directly extract gas from the reaction chamber S1, which is beneficial to improve the exhaust efficiency.

[0101] The embodiment also provides a vacuumizing method of the furnace tube device, which is basically the same as the vacuumizing method in Embodiment 4, and the difference is that the vacuumizing method in the embodiment further comprises opening the third valve 331 or the flow restrictor in step S310. By opening the third valve 331 or the flow restrictor, the gas in the outer pipe exhaust pipeline 400 upstream of the first valve 412 can be prevented from flowing back into the reaction chamber S1.

[0102] Next, the working process of the furnace tube device is described with reference to Embodiment 1 and FIG. 9.

[0103] The substrate is placed in the reaction chamber S1, and the dry pump 411 and the first valve 412 are opened to vacuumize the reaction chamber S1 to 10 -2 -10 -3 tor. The dry pump 411 is kept on during the whole process.

[0104] The precursor A is introduced into the reaction chamber S1 through the first gas inlet pipeline 510, and the output power of the dry pump 411 or the opening degree of the first valve 412 at the outer pipe exhaust pipeline 400 is appropriately reduced during the introduction of the precursor A, so that the precursor A flows in the reaction chamber S1 and fills the reaction chamber S1, and the precursor A can cover the surface of the whole substrate.

[0105] After the precursor A covers the surface of the whole substrate, the output power of the dry pump 411 and the opening degree of the first valve 412 at the outer pipe exhaust pipeline 400 are increased to quickly discharge the excess precursor A. During this process, the cleaning gas C is introduced to discharge the precursor A.

[0106] The reaction gas B is introduced into the reaction chamber S1 through the second gas inlet pipeline 520, and the output power of the dry pump 411 or the opening degree of the first valve 412 at the outer pipe exhaust pipeline 400 is appropriately reduced, so that the reaction gas B fills the reaction chamber S1 and reacts with the precursor A to form a film layer on the surface of the substrate.

[0107] After the reaction gas B and the precursor A are reacted, the vacuumizing method in the embodiment is used to vacuumize.

[0108] S300, the first valve 412 is closed, the fourth valve 321 is opened, and the vacuum degree in the reaction chamber S1 is vacuumized to a first preset value.

[0109] S310, the fourth valve 321 is closed, the molecular pump 311, the second valve 312, and the third valve 331 or the flow restrictor are opened, and the vacuum degree is continuously vacuumized to a second preset value.

[0110] S320, the molecular pump 311 and the second valve 312 are closed, the cleaning gas C is introduced into the reaction chamber S1, after the vacuum degree in the reaction chamber S1 is lower than or equal to the vacuum degree in the outer pipe exhaust pipeline 400, the first valve 412 is opened, and the third valve 331 or the flow restrictor is closed.

[0111] In some embodiments, the third valve 331 or the flow restrictor can also be closed when the precursor A is introduced.

[0112] Although the specific embodiments of the present application are described above, those skilled in the art should understand that this is only an example, the protection scope of the present application is defined by the appended claims. Those skilled in the art can make various changes or modifications to these embodiments without departing from the principles and essence of the present application, and these changes and modifications all fall within the protection scope of the present application.

Claims

1. An atomic layer deposition method, characterized in that: include: S100, placing a substrate in a reaction chamber, and evacuating the reaction chamber to a vacuum state; S110, introducing a precursor into the reaction chamber until the precursor covers the entire surface of the substrate; S120, discharge excess precursor; S130, introducing a reaction gas into the reaction chamber to fully react with the precursor; S140, pumping the vacuum degree of the reaction chamber to below 10-4 Torr.

2. The atomic layer deposition method according to claim 1, wherein: The method further includes repeating steps S110 - S140 to deposit a predetermined film layer on the substrate until the film layer on the substrate reaches a predetermined thickness.

3. The atomic layer deposition method according to claim 2, wherein: The predetermined film layer includes a stacked layer formed by any one or more of zirconium oxide, hafnium oxide, titanium zirconium oxide, titanium oxide, ruthenium oxide, antimony oxide, and aluminum oxide.

4. The atomic layer deposition method according to claim 1, wherein: The step S120 and / or the step S140 further includes introducing a cleaning gas.

5. The atomic layer deposition method according to claim 1, wherein: In the step S100, the step S120 or the step S140, the vacuum degree in the reaction chamber is pumped to 10 -5 Support below.

6. A furnace tube device, characterized in that: include: an inner tube, the interior of which forms a reaction chamber; an outer tube, sleeved on the outer portion of the inner tube, with a gap region between the outer tube and the inner tube, and an exhaust port provided on the inner tube to connect the reaction chamber with the gap region; an outer tube exhaust pipeline, which is provided with a first vacuum pump and a first valve, wherein the first valve is provided upstream of the first vacuum pump, and the outer tube exhaust pipeline is in communication with the gap area; an inner tube exhaust pipeline, which is provided with a second vacuum pump and a second valve, wherein the second valve is provided upstream of the second vacuum pump, and the inner tube exhaust pipeline is in communication with the reaction chamber; The ultimate vacuum degree of the second vacuum pump is greater than the ultimate vacuum degree of the first vacuum pump.

7. The furnace tube equipment according to claim 6, characterized in that The first vacuum pump is a dry pump, and the second vacuum pump is a molecular pump.

8. The furnace tube equipment according to claim 6, characterized in that It also includes a first branch pipeline, one end of which is connected to the outer tube exhaust pipeline upstream of the first valve, and the other end of the first branch pipeline is connected to the inner tube exhaust pipeline upstream of the second vacuum pump.

9. The furnace tube equipment according to claim 8, characterized in that The first branch pipeline is provided with a third valve or a flow restrictor.

10. The furnace tube equipment according to claim 6 or 8, characterized in that: It also includes a second branch pipeline, which is provided with a fourth valve. One end of the second branch pipeline is connected to the outer tube exhaust pipeline between the first vacuum pump and the first valve, and the other end of the second branch pipeline is connected to the inner tube exhaust pipeline upstream of the second vacuum pump.

11. The furnace tube equipment according to claim 6, characterized in that The inner tube air extraction pipeline passes through the outer tube and the gap area and is arranged on the inner tube, and the outer tube air extraction pipeline is arranged on the outer tube.

12. The furnace tube equipment according to claim 6, characterized in that It also includes a manifold connected to the bottom ends of the inner tube and the outer tube, the manifold is connected to the reaction chamber, the manifold is not connected to the gap area, the inner tube exhaust pipeline is arranged on the manifold, and the outer tube exhaust pipeline is arranged on the outer tube.

13. The furnace tube device according to claim 6, characterized in that: It also includes a manifold connected to the bottom end of the inner tube and the bottom end of the outer tube, the manifold includes a first area and a second area, the first area is connected to the reaction chamber, the second area is connected to the gap area, the inner tube exhaust pipeline is arranged on the manifold, the inner tube exhaust pipeline is connected to the first area, the outer tube exhaust pipeline is arranged on the manifold, and the outer tube exhaust pipeline is connected to the second area.

14. The furnace tube equipment according to claim 13, characterized in that The manifold comprises: a first pipe fitting; a second pipe, one end of the second pipe being connected to the inner pipe and the outer pipe, and the other end of the second pipe being connected to the first pipe, the second pipe being a double-layer structure with a hollow sandwich, the first region being the region enclosed by the inner layer of the second pipe and the first pipe, and the second region being the hollow region of the sandwich of the second pipe; The inner tube air extraction pipeline is arranged on the first pipe fitting, and the outer tube air extraction pipeline is arranged on the second pipe fitting.

15. A vacuuming method for furnace tube equipment, characterized in that: It includes the furnace tube device according to claim 9, and the vacuuming method includes: S200, turning on the first vacuum pump and the first valve to reduce the vacuum level in the reaction chamber to a first preset value; S210, closing the first valve, opening the second vacuum pump and the second valve, and opening the third valve or the flow limiter, and continuing to pump the vacuum degree to a second preset value; The vacuum degree of the second preset value is higher than the vacuum degree of the first preset value.

16. The vacuuming method for furnace tube equipment according to claim 15, characterized in that: The vacuuming method further comprises: S220, closing the second vacuum pump and the second valve, introducing a cleaning gas into the reaction chamber, and opening the first valve after the vacuum degree in the reaction chamber is lower than or equal to the vacuum degree of the outer exhaust pipe.

17. A vacuuming method for furnace tube equipment, characterized in that: It includes the furnace tube device according to claim 10, and the vacuuming method includes: S300, closing the first valve, opening the first vacuum pump and the fourth valve, and pumping the vacuum level in the reaction chamber to a first preset value; S310, closing the fourth valve, opening the second vacuum pump and the second valve, and continuing to pump the vacuum degree to a second preset value; The vacuum degree of the second preset value is higher than the vacuum degree of the first preset value.

18. The vacuuming method for furnace tube equipment according to claim 17, wherein: The vacuuming method further comprises: S320, closing the second vacuum pump and the second valve, introducing a cleaning gas into the reaction chamber, and opening the first valve after the vacuum degree in the reaction chamber is lower than or equal to the vacuum degree of the outer exhaust pipe.

19. The vacuum evacuation method for furnace tube equipment according to claim 17, wherein: It is characterized by: The step S310 further includes opening the third valve or flow restrictor.

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