Atomic layer deposition film preparation method and atomic layer deposition equipment

Abstract

The invention relates to the technical field of semiconductor manufacturing, in particular to an atomic layer deposition film preparation method and atomic layer deposition equipment. According to the technical scheme, the reaction chamber comprises the chamber body and the thermal field cover arranged at the opening of the chamber body, and the heating piece and the cooling piece are arranged on the thermal field cover. In the preparation process of the atomic layer deposition film, a first precursor and a second precursor are sequentially and alternately introduced into a reaction chamber according to a preset number of times to react, so that an initial film layer can be formed on the surface of a substrate. Then the whole reaction chamber is heated by controlling the heating piece or the whole reaction chamber is cooled by controlling the cooling piece, so that the time for annealing the obtained initial film layer is shorter, and the chamber body does not need to be opened to heat or cool; and fewer side reactants or defects are obtained on the target film layer. Therefore, the preparation quality of the atomic layer film can be improved.

Description

Technical Field

[0001] The present application relates to the field of semiconductor manufacturing technology, and in particular to an atomic layer deposition film preparation method and an atomic layer deposition device. Background Art

[0002] With the advancement of semiconductor manufacturing technology, thin films are playing an increasingly important role in industrial production and people's daily lives, and the process methods for making atomic layer deposition films are also gaining more and more attention. However, the quality of current atomic layer deposition films needs to be improved. Summary of the invention

[0003] Based on this, the present application provides a thermal field cover, an atomic layer deposition device and an atomic layer deposition film preparation method to improve the preparation quality of the atomic layer deposition film.

[0004] In a first aspect, an embodiment of the present application provides a method for preparing an atomic layer deposition film, comprising:

[0005] A reaction chamber is provided, and a substrate is placed in a chamber body of the reaction chamber; the reaction chamber comprises a thermal field cover arranged at an opening of the chamber body, and a heating element and a cooling element are arranged on the thermal field cover;

[0006] Alternatingly introducing a first precursor and a second precursor into the chamber body at a preset number of times to obtain an initial film layer on the surface of the substrate;

[0007] The heating element is controlled to heat the initial film layer, and the cooling element is controlled to cool the initial film layer, so as to anneal the initial film layer to obtain a target film layer.

[0008] In one embodiment, the step of controlling the heating element to heat the initial film layer and controlling the cooling element to cool the initial film layer to anneal the initial film layer to obtain the target film layer includes:

[0009] The heating process and the cooling process are performed alternately in sequence;

[0010] The heating process includes controlling the heating element to heat the chamber body, and when the temperature in the chamber body rises to the first target temperature, the current temperature in the chamber body is maintained at the first target temperature for a first preset time period;

[0011] The cooling process includes controlling the cooling element to cool the chamber body, and when the temperature in the chamber body is cooled from the first target temperature to the second target temperature, the current temperature in the chamber body is maintained at the second target temperature for a second preset time.

[0012] In one embodiment, the difference between the first target temperature and the second target temperature is 50 degrees Celsius to 100 degrees Celsius.

[0013] In one embodiment, the first precursor and the second precursor are alternately introduced into the chamber body at a predetermined number of times to obtain an initial film layer on the surface of the substrate, which includes:

[0014] Introducing an inert gas into a first storage element containing a first precursor, so that the first precursor can flow from a bottom of the first storage element to a top of the first storage element;

[0015] The top of the first storage element is controllably connected to the chamber body; and the vapor pressure of the first precursor is lower than the vapor pressure of the second precursor.

[0016] In a second aspect, an embodiment of the present application provides an atomic layer deposition device, comprising:

[0017] A reaction chamber, comprising a chamber body and a thermal field cover disposed at an opening of the chamber body;

[0018] A heating element is arranged on the heat field cover;

[0019] The cooling element is arranged on the heat field cover.

[0020] In one embodiment, one of the heating element and the cooling element is disposed on a side of the thermal field cover facing the interior of the chamber body, and the other is disposed on a side of the thermal field cover facing away from the chamber body; and / or

[0021] The atomic layer deposition equipment also includes a detection element, which is arranged on the thermal field cover and is used to detect the temperature inside the chamber body; the heating element can heat in response to the detection signal of the detection element, and the cooling element can cool in response to the detection signal of the detection element.

[0022] In one embodiment, the atomic layer deposition apparatus further comprises:

[0023] A first storage element, for storing a first precursor; an outlet of the first storage element and the interior of the chamber body are controllably connected;

[0024] A second storage element is used to store an inert gas; a first outlet of the second storage element is connected to an inlet of the first storage element;

[0025] The third storage element is used to store the second precursor; the outlet of the third storage element is controllably connected to the chamber body.

[0026] In one embodiment, the atomic layer deposition apparatus further includes a first switching device, the first switching device having a first switching port, a second switching port and a third switching port;

[0027] The first switching port is communicated with the second outlet of the second storage element, the second switching port is communicated with the chamber body, and the third switching port is communicated with the outlet of the first storage element;

[0028] Among them, the first switching device has a first state and a second state; when the first switching device is in the first state, the first switching port is connected to the second switching port; when the first switching device is in the second state, the first switching port is connected to the second switching port, and the third switching port is connected to the second switching port.

[0029] In one embodiment, the atomic layer deposition apparatus further includes a fourth storage element for storing compressed gas; the first switching device further includes a fourth switching port, and a movable blocking element is further provided inside the first switching device;

[0030] The inlet side of the fourth switching port is connected to the outlet side of the fourth storage element, and the outlet sides of the fourth switching port are all connected to the first switching port, the second switching port, and the third switching port;

[0031] In which, the first switching device is in a first state, and the blocking member covers the outlet side of the third switching port and the outlet side of the fourth switching port; the first switching device is in a second state, and the blocking member opens the fourth switching port and the third switching port in response to the compressed gas entering from the fourth switching port, the third switching port is connected to the fourth switching port, and the second switching port is connected to the fourth switching port.

[0032] In one embodiment, the atomic layer deposition apparatus further includes a second switching device, the second switching device having a first conversion interface and a second conversion interface;

[0033] The first conversion interface is communicated with the outlet side of the third storage element, and the second conversion interface is communicated with the reaction chamber;

[0034] When the first conversion interface is in the first state, the first conversion interface is connected to the second conversion interface; when the first conversion interface is in the second state, the first conversion interface is not connected to the second conversion interface.

[0035] In the above-mentioned atomic layer deposition film preparation method and atomic layer deposition device, when the initial film layer is annealed, there is no need to open the chamber body and then heat or cool the chamber body. A heating element and a cooling element are provided on the thermal field cover. When the heating element is controlled to be turned on, the thermal field cover is heated and heated. Since the thermal field cover is arranged at the opening of the chamber body, the thermal field cover and the chamber body constitute a closed space, and the heat of the thermal field cover can be thermally transferred to the chamber body. Similarly, when the cooling element is controlled to be turned on, the thermal field cover is cooled down, and the heat can be thermally transferred to the chamber body so that the chamber body is quickly cooled. Furthermore, the time for annealing the initial film layer can be shortened. Similarly, when multiple annealing treatments are performed, there is no need to open the chamber body, which can shorten the interval time between two adjacent annealing treatments. Since the time for multiple annealing treatments is short, the annealing treatment is carried out before defects are generated on the initial film layer, so that fewer side reactants or defects are obtained on the target film layer. In this way, the preparation quality of the atomic layer deposition film can be improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 This is a flow chart of an embodiment of the atomic layer deposition film preparation method provided in the present application.

[0037] Figure 2 for Figure 1 A flowchart of other steps of the atomic layer deposition film preparation method.

[0038] Figure 3 for Figure 1 Flow chart of yet another step of the atomic layer deposition film preparation method.

[0039] Figure 4 A schematic diagram of the principle of an embodiment of the atomic layer deposition equipment provided in the present application.

[0040] Figure 5 A schematic diagram of the three-dimensional structure of an embodiment of the thermal field cover provided in the present application.

[0041] Figure 6 for Figure 5 Schematic diagram of the three-dimensional structure of the thermal field cover from another angle.

[0042] Figure 7 for Figure 4 Schematic diagram of the principle of the first switching device in.

[0043] Figure 8 Schematic diagram of the temperature rise of the thermal field cover over time.

[0044] Fig. 9 Schematic diagram of the change of thermal field cover temperature reduction over time.

[0045] Fig.10Schematic diagram of the effect in the non-growth area of ​​the initial film layer.

[0046] Fig.11 Schematic diagram of the effect of the target film layer.

[0047] Description of reference numerals:

[0048] Reaction chamber 1; chamber body 11; first precursor; second precursor; inert gas; compressed gas; display element X1; vacuum gauge Z; mechanical pump B1;

[0049] A first storage element Z1; a second storage element Z2; a third storage element Z3, a fourth storage element D4;

[0050] a first switching device Q1 ; a first switching port D1 ; a second switching port D2 ; a third switching port D3 ; a fourth switching port D4 ; a first flow meter L1 ; a second flow meter L2 ; a third flow meter L3 ; a fourth flow meter L4 ; and a blocking member ZD.

[0051] A second switching device Q2; a first conversion interface J1, a second conversion interface J2;

[0052] Thermal field cover 2; heating element 21; cooling element 22; detection element 23, welding head 24, base 25, handle 26, fixed pressing piece 27. DETAILED DESCRIPTION

[0053] In order to make the above-mentioned purposes, features and advantages of the present application more obvious and easy to understand, the specific implementation methods of the present application are described in detail below in conjunction with the accompanying drawings. In the following description, many specific details are set forth to facilitate a full understanding of the present application. However, the present application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without violating the connotation of the present application, so the present application is not limited by the specific embodiments disclosed below.

[0054] In the description of the present application, it should be understood that if the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. appear, the orientation or position relationship indicated by these terms is the orientation or position relationship based on the drawings, which is only for the convenience of describing the present application and simplifying the description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present application.

[0055] In addition, if the terms "first" or "second" appear, these terms are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include at least one of the features. In the description of this application, if the term "plurality" appears, the meaning of "plurality" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

[0056] In this application, unless otherwise clearly specified and limited, if the terms "installed", "connected", "connected", "fixed" and the like appear, these terms should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integrated connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood according to the specific circumstances.

[0057] In the present application, unless otherwise clearly specified and limited, if there is a description that a first feature is "above" or "below" a second feature, etc., or similar descriptions appear, it may mean that the first and second features are in direct contact, or that the first and second features are in indirect contact through an intermediate medium. Moreover, the first feature being "above", "above" and "above" the second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is higher in level than the second feature. The first feature being "below", "below" and "below" the second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature is lower in level than the second feature.

[0058] It should be noted that if an element is referred to as being "fixed to" or "disposed on" another element, it may be directly on the other element or there may be a central element. If an element is considered to be "connected to" another element, it may be directly connected to the other element or there may be a central element at the same time. If any, the terms "vertical", "horizontal", "upper", "lower", "left", "right" and similar expressions used in this application are for illustrative purposes only and do not represent the only implementation method.

[0059] The present application provides a method for preparing an atomic layer deposition film, which can be referred to Figure 1 , Figure 1 The flowchart of one embodiment of the atomic layer deposition film preparation method provided in the present application. The atomic layer deposition film preparation method comprises the following steps:

[0060] Step S100, providing a reaction chamber, placing a substrate in a chamber body of the reaction chamber; the reaction chamber comprises a thermal field cover arranged at an opening of the chamber body, and a heating element and a cooling element are arranged on the thermal field cover;

[0061] Step S200, alternately introducing a first precursor and a second precursor into the chamber body for a preset number of times to obtain an initial film layer on the surface of the substrate;

[0062] Step S300: Control the heating element to heat the initial film layer, and control the cooling element to cool the initial film layer, so as to anneal the initial film layer to obtain a target film layer.

[0063] In step S100, an environmental reaction chamber for preparing an atomic layer deposition film is provided, and a base substrate to be prepared is placed in a chamber body of the reaction chamber, so that the substrate can subsequently undergo a subsequent reaction in the chamber body and generate an atomic layer deposition film. The substrate can be a silicon wafer with a surface having a silicon oxide thickness of about 275nm or a silicon wafer with a tungsten thickness of about 30nm magnetron sputtered.

[0064] The thermal field cover is arranged at the opening of the chamber body. The thermal field cover and the chamber body form a relatively closed space. A heating element and a cooling element are arranged on the thermal field cover. The heating element can be arranged on the side facing the inside of the chamber body, and the cooling element can be arranged on the side of the thermal field cover away from the chamber body. The heating element can also be arranged on the side of the thermal field cover away from the chamber body, and the cooling element can be arranged on the side facing the inside of the chamber body, or arranged in other ways. In the subsequent atomic layer deposition film preparation process, the chamber body can be heated or cooled more quickly and conveniently, and the heating element will not interfere with each other when heating or the cooling element will not interfere with each other when cooling. Among them, "reaction chamber" refers to the space for reaction, and here, it is the space for the atomic layer deposition film preparation reaction. "Precursor" refers to the initial material or compound used to synthesize or generate the target substance in chemistry, materials science and manufacturing processes.

[0065] In step S200, "alternating introduction" means that the first precursor is introduced into the chamber body as the first step, and then the second precursor is introduced into the chamber body, and finally the relative amount of the first precursor and the second precursor in the chamber body is adjusted by the introduced first precursor, so that the first precursor and the second precursor on the surface of the substrate can react to obtain an initial film layer. "Preset number of times" refers to the number of times allowed or planned in advance in the process of introducing the first precursor and the second precursor. Here, the process of first introducing the first precursor, then introducing the second precursor, and finally introducing the first precursor is considered as one process. Alternating introduction allows the relative temperature of the first precursor and the second precursor to be more reliably maintained in the chamber body.

[0066] In step S300, the primary annealing process refers to the process of first heating the initial film layer and then cooling the initial film layer. When the initial film layer is annealed, there is no need to open the chamber body and then heat or cool the chamber body. Since the time for multiple annealing processes is shortened, the annealing process is performed before defects are generated on the initial film layer, so that fewer side reactants or defects are obtained on the target film layer.

[0067] In this way, by providing a reaction chamber, a substrate can be placed inside the reaction chamber to deposit an atomic layer deposition film. In addition to the chamber body, the reaction chamber also includes a thermal field cover arranged at the opening of the chamber body, wherein the thermal field cover is provided with a heating element and a cooling element. In the overall atomic layer deposition film preparation process, it is necessary to alternately introduce the first precursor and the second precursor into the reaction chamber at a preset number of times, and the first precursor and the second precursor can react so that an initial film layer can be formed on the surface of the substrate. Then, the entire reaction chamber is heated by controlling the heating element or the entire reaction chamber is cooled by controlling the cooling element.

[0068] When the initial film layer is annealed, there is no need to open the chamber body and then heat or cool the chamber body. The thermal field cover is provided with a heating element and a cooling element. When the heating element is controlled to be turned on, the thermal field cover is heated and heated. Since the thermal field cover is arranged at the opening of the chamber body, the thermal field cover and the chamber body constitute a closed space, and the heat of the thermal field cover can be thermally transferred to the chamber body. Similarly, when the cooling element is controlled to be turned on, the thermal field cover is cooled down, and heat can be transferred to the chamber body to quickly cool the chamber body. Furthermore, the time for annealing the initial film layer can be shortened. Similarly, when multiple annealing treatments are performed, there is no need to open the chamber body, which can shorten the interval time between two adjacent annealing treatments. Since the time for multiple annealing treatments is short, the annealing treatment is carried out before defects are generated on the initial film layer, so that fewer side reactants or defects are obtained on the target film layer. In this way, the preparation quality of the atomic layer deposition film can be improved.

[0069] In some embodiments, continue to refer to Figure 1 , and combined with reference Figure 2 , Figure 2 for Figure 1 Flow chart of other steps of the method for preparing an atomic layer deposition film in FIG. 1 . Step S300 includes the following steps:

[0070] Step S301, performing the heating process and the cooling process alternately in sequence;

[0071] The heating process includes controlling the heating element to heat the chamber body, and when the temperature in the chamber body rises to the first target temperature, the current temperature in the chamber body is maintained at the first target temperature for a first preset time period;

[0072] The cooling process includes controlling the cooling element to cool the chamber body, and when the temperature in the chamber body is cooled from the first target temperature to the second target temperature, the current temperature in the chamber body is maintained at the second target temperature for a second preset time.

[0073] In step S301, "alternating" means starting with the heating process, followed by cooling, heating, cooling and other steps alternating, and finally ending with the cooling step.

[0074] By controlling the heating element to start heating, the thermal field cover is heated and the temperature is increased. Since the thermal field cover is set at the opening of the chamber body, the thermal field cover and the chamber body form a closed space. The heat of the thermal field cover can be thermally transferred to the chamber body, which increases the temperature inside the chamber body and drives the defective particles on the initial film layer in the chamber body to migrate. After the initial film layer is quickly heated up to reduce the defective particles, the temperature inside the chamber body needs to be reduced to the deposition temperature. The deposition temperature refers to the temperature inside the chamber body before the heating treatment step is performed. In this way, the heating step can be performed again. The initial film layer is annealed multiple times to further reduce the defective particles on the initial film layer. Among them, the first target temperature is greater than the second target temperature.

[0075] In some embodiments, continue to refer to Figure 1 , step 301, the difference between the first target temperature and the second target temperature is 50 degrees Celsius to 100 degrees Celsius.

[0076] It can be understood that when the second target temperature is 200 degrees Celsius, the first target temperature is between 250 degrees Celsius and 300 degrees Celsius.

[0077] At this temperature, defective particles on the initial film layer can be driven to migrate more quickly.

[0078] In some embodiments, see Figure 1 In conjunction with Figure 3 , Figure 3 for Figure 1 Flow chart of another step of the method for preparing an atomic layer deposition film. Before step S200, the following steps are also included:

[0079] Step SA, introducing an inert gas into the first storage element containing the first precursor, so that the first precursor flows from the bottom of the first storage element to the top of the first storage element; the top of the first storage element is controllably connected to the chamber body;

[0080] The vapor pressure of the first precursor is lower than the vapor pressure of the second precursor.

[0081] In step SA, since the vapor pressure of the first precursor involved in the reaction is relatively small, it is not easy for the first precursor to be transferred from the first storage element to the chamber body when it is in the first storage element. The vapor pressure refers to the pressure exerted by the vapor on the container wall when the solid and its vapor are in a dynamic equilibrium state at a certain temperature. Therefore, before the step of introducing the first precursor into the chamber body, an inert gas is introduced into the first storage element containing the first precursor, and the first precursor is brought from the bottom to the top of the first storage element by the inert gas. The top of the first storage element and the chamber body can be connected in a controllable manner. When the first precursor needs to be introduced into the chamber body, the inert gas can carry the first precursor from the top of the first storage element to the chamber body when the first storage element and the chamber body are controlled to be connected.

[0082] Based on the same inventive concept, the present application provides an atomic layer deposition device, which can be referred to Figure 4 , Figure 5 and Figure 6 , Figure 4 A schematic diagram of an embodiment of an atomic layer deposition device provided in the present application. Figure 5 A schematic diagram of the three-dimensional structure of an embodiment of the thermal field cover provided in the present application. Figure 6 for Figure 5 Schematic diagram of the three-dimensional structure of the thermal field cover in another angle. The atomic layer deposition device includes a reaction chamber 1, a heating element 21 and a cooling element 22. The reaction chamber 1 has a chamber body 11, and the reaction chamber 1 includes a thermal field cover 2 arranged on the chamber body 11. The heating element 21 and the cooling element 22 are both arranged on the thermal field cover 2.

[0083] It can be understood that the heating element 21 and the cooling element 22 are arranged on the thermal field cover 2, and the thermal field cover 2 covers the chamber body 11, so when the heating element 21 of the thermal field cover 2 is heated, the thermal field cover 2 can quickly heat up, so that the chamber body 11 can also quickly heat up, and when the cooling element 22 starts to cool, the thermal field cover 2 quickly cools down, so that the chamber body 11 quickly cools down, which is convenient for quickly heating or cooling the chamber body 11 in the atomic layer preparation method.

[0084] When the initial film layer is annealed, there is no need to open the chamber body 11 and then heat or cool the chamber body 11. The thermal field cover 2 is provided with a heating element 21 and a cooling element 22. When the heating element 21 is controlled to be turned on, the thermal field cover 2 is heated and heated. Since the thermal field cover 2 is arranged at the opening of the chamber body 11, the thermal field cover 2 and the chamber body 11 constitute a closed space, and the heat of the thermal field cover 2 can be thermally transferred to the chamber body 11. Similarly, when the cooling element 22 is controlled to be turned on, the thermal field cover 2 is cooled down, and the heat can be thermally transferred to the chamber body 11 to quickly cool the chamber body. Furthermore, the time for annealing the initial film layer can be shortened. Similarly, when multiple annealing treatments are performed, there is no need to open the chamber body 11, which can shorten the interval time between two adjacent annealing treatments. Since the time for multiple annealing treatments is short, the annealing treatment is performed before defects are generated on the initial film layer, so that fewer side reactants or defects are obtained on the target film layer. In this way, the preparation quality of the atomic layer deposition film can be improved.

[0085] In some embodiments, reference Figure 4 , Figure 5 as well as Figure 6 , one of the heating element 21 and the cooling element 22 is arranged on the side of the thermal field cover 2 facing the inside of the chamber body 11, and the other is arranged on the side of the thermal field cover 2 away from the chamber body 11; and or, the atomic layer deposition equipment also includes a detection element 23 for detecting the temperature in the chamber body 11, and the heating element 21 and the cooling element 22 can be heated or cooled in response to the detection signal of the detection element 23.

[0086] The heating element 21 may be disposed on a side facing the interior of the chamber body 11, and the cooling element 22 may be disposed on a side of the thermal field cover 2 facing away from the chamber body 11. Alternatively, the heating element 21 may be disposed on a side of the thermal field cover 2 facing away from the chamber body 11, and the cooling element 22 may be disposed on a side facing the interior of the chamber body 11.

[0087] The heating element 21 and the cooling element 22 are arranged one on the side facing the inside of the chamber body 11 and the other on the side of the thermal field cover 2 away from the chamber body 11, so that the heating element 21 and the cooling element 22 are arranged separately. When the heating element 21 or the cooling element 22 is working, it will not interfere with or affect the other component, making the operation of the heating element 21 and the cooling element 22 safer.

[0088] In other embodiments, the heating element 21 and the cooling element 22 may be both disposed on the side facing the interior of the chamber body 11, or may be both disposed on the side of the thermal field cover 2 facing away from the chamber body 11, and the heating element 21 and the cooling element 22 may be spaced apart.

[0089] The detection element 23 is configured to detect the temperature inside the chamber cavity and transmit the detected temperature signal to the heating element 21 or the cooling element 22. When the temperature of the chamber body 11 received by the heating element 21 or the cooling element 22 reaches the temperature required to start heating or cooling, it can be controlled to start heating or cooling operations, thereby realizing the automation of heating and cooling and further improving the processing rate of heating and cooling operations.

[0090] In addition, the atomic layer deposition apparatus may further include a flow meter, which is arranged on different paths to control the flow of each fluid, such as Figure 4 The flowmeter includes a first flowmeter L1, a second flowmeter L2, a third flowmeter L3 and a fourth flowmeter L4. Specifically, the flowmeter includes MFC1, MFC2, MFC3 and MFC4, wherein MFC (Mass Flow Controller) refers to a mass flow controller, which is a device used to accurately measure and control the flow of gas or liquid. It is based on the principle of mass flow measurement and can directly measure the mass flow of the fluid instead of the volume flow, which is more accurate and reliable.

[0091] In some embodiments, continue to refer to Figure 4 The atomic layer deposition apparatus further includes a first storage element Z1 storing a first precursor, a second storage element Z2 storing an inert gas, and a third storage element Z3 storing a second precursor. The outlet of the first storage element Z1 is controllably connected to the interior of the chamber body 11, the first outlet of the second storage element Z2 is connected to the inlet of the first storage element Z1, and the outlet of the third storage element Z3 is controllably connected to the chamber body 11.

[0092] In this way, since the outlet of the first storage element Z1 is controllably connected to the interior of the chamber body 11, when the first precursor needs to be introduced into the chamber body 11, the outlet of the first storage element Z1 can be controlled to be connected to the interior of the chamber body 11. Since the first outlet of the second storage element Z2 is connected to the inlet of the first storage element Z1, the inert gas can be controlled to be introduced into the chamber body 11. Since the outlet of the third storage element Z3 is controllably connected to the chamber body 11, when the second precursor needs to be introduced into the chamber body 11, the outlet of the first storage element Z1 can be controlled to be connected to the chamber body 11. Here, "controllably connected" means that it can be controlled to be connected or controlled not to be connected.

[0093] In this way, the controllable communication allows the time and dosage of the first precursor entering the chamber body 11 to be controlled, so that the first precursor and the second precursor can fully react in appropriate relative amounts.

[0094] In some embodiments, reference may be made to Figure 4The atomic layer deposition apparatus further includes a first switching device Q1, which is provided with a first switching port D1, a second switching port D2 and a third switching port D3. Here, "port" refers to a port for controlling the on-off and flow direction of a fluid.

[0095] The first switching port D1 is connected to the second outlet of the second storage element Z2, the second switching port D2 is connected to the chamber body 11, and the third switching port D3 is connected to the outlet of the first storage element Z1. The first switching device Q1 can have a first state and a second state. When the first switching device Q1 is in the first state, the first switching port D1 is connected to the second switching port D2, and when the first switching device Q1 is in the second state, the first switching port D1 is connected to the second switching port D2, and the third switching port D3 is connected to the second switching port D2.

[0096] The setting of the first switching device Q1 can be used to switch the third switching port D3 and the second switching port D2 to be connected or disconnected, and thus can switch from the state where the first precursor is stored in the first storage element Z1 to the state where the first precursor is passed into the chamber body 11, or from the state where the first precursor is passed into the chamber body 11 to the state where the first precursor stops passing into the chamber body 11.

[0097] In some embodiments, further reference is made to Figure 4 , and combined with reference Figure 7 , Figure 7 for Figure 4 The schematic diagram of the first switching device in FIG. The atomic layer deposition equipment also includes a fourth storage element Z4 for storing compressed gas, the first switching device Q1 is also provided with a fourth switching port D4, and a movable blocking element ZD is also provided inside the first switching device Q1. The inlet side R1 of the fourth switching port D4 is connected to the outlet side C1 of the fourth storage element Z4, and the outlet side C1 of the fourth switching port D4 is connected to the first switching port D1, the second switching port D2, and the third switching port D3. The blocking element ZD covers the outlet side C2 of the third switching port D3 and the outlet side C1 of the fourth switching port D4.

[0098] Among them, when the first switching device Q1 is in the first state, the blocking member ZD covers the outlet side C2 of the third switching port D3 and the outlet side C1 of the fourth switching port D4, and when the first switching device Q1 is in the second state, the blocking member ZD opens the fourth switching port D4 and the third switching port D3 in response to the compressed gas introduced from the fourth switching port D4, and the third switching port D3 is connected with the fourth switching port D4, and the second switching port D2 is connected with the fourth switching port D4.

[0099] Due to the arrangement of the fourth switching port D4 and the blocking member ZD, in the first state, the blocking member ZD covers the outlet side C2 of the third switching port D3 and the outlet side C1 of the fourth switching port D4, and the third switching port D3 and the fourth switching port D4 are not connected. In the second state, the compressed gas is introduced into the fourth switching port D4, and the blocking member ZD covering the outlet side C1 of the fourth switching port D4 and the outlet side C2 of the third switching port D3 is opened, so that the blocking member ZD is separated from the fourth switching port D4 and the third switching port D3, thereby making the fourth switching port D4 and the third switching port D3 connected, the second switching port D2 and the third switching port D3 connected, and the fourth switching port D4 and the second switching port D2 connected. In this way, the first precursor is controlled to enter the chamber body 11.

[0100] Only by providing the first switching device Q1, it is possible to switch whether the first storage element Z1 is connected to the chamber body 11 to control the amount of the first precursor. Such a design is safe and reliable, and is convenient for the operator to operate.

[0101] In some embodiments, reference Figure 4 The atomic layer deposition apparatus further includes a second switching device Q2, which is provided with a first conversion interface J1 and a second conversion interface J2. The first conversion interface J1 is connected to the outlet side of the third storage element Z3, and the second conversion interface J2 is connected to the reaction chamber 1. When the first conversion interface J1 is in the first state, the first conversion interface J1 is connected to the second conversion interface J2. When the first conversion interface J1 is in the second state, the first conversion interface J1 and the second conversion interface J2 are not connected.

[0102] The second switching device Q2 can be used to switch the connection or disconnection between the first conversion interface J1 and the second conversion interface J2, and thus can switch from the state where the second precursor is stored in the third storage element Z3 to the state where the second precursor is introduced into the chamber body 11, or from the state where the second precursor is introduced into the chamber body 11 to the state where the second precursor stops entering the chamber body 11.

[0103] Only by providing the second switching device Q2, it is possible to control whether the second precursor in the third storage element Z3 is passed into the chamber body 11, so as to control the amount of the second precursor passed into the chamber body.

[0104] In addition, please continue to refer to Figure 4 The atomic layer deposition equipment also includes a mechanical pump B1 driven and connected to the chamber body 11. The mechanical pump B1 can evacuate the chamber body 11 so that the air pressure in the chamber body 11 reaches an expected value, wherein the expected value means that the lid in the reaction chamber can be opened.

[0105] In some embodiments, the atomic layer deposition apparatus further includes a display component X1 , which is connected to the chamber body 11 and is used to display the pressure value in the chamber body 11 . The display component X1 includes a vacuum gauge Z.

[0106] In some embodiments, you may continue to refer to Figure 5 The thermal field cover 2 also includes a base 25, a cooling member 22 disposed on the outer surface of the base, a thermocouple feedthrough 23, and a welding head 24 connecting the thermocouple feedthrough 23 to the base 25. The cooling member 22 may be a cooling pipe 22, and the thermocouple feedthrough 23 may transmit the thermal signal in the chamber body 11 to the outside of the chamber body 11, so as to obtain the temperature information in the chamber body 11. The thermal field cover 2 also includes a handle 26 for conveniently taking the thermal field cover 2.

[0107] In some embodiments, you may continue to refer to Figure 6 The thermal field cover 2 also includes a fixing gasket 27 , and the heating element 21 includes a heating lamp tube, and a copper wire can pass through the through hole on the fixing gasket and be wound around the heating lamp tube multiple times, so that the heating lamp tube is fixed on the base 25 .

[0108] The following is a specific example to illustrate the preparation method of the atomic layer deposition film, taking the inert gas as nitrogen, the first precursor as Ru(EtCp)2, and the second precursor as O2 as an example, combined with reference Figures 1 to 7 To illustrate, the production method comprises the following steps:

[0109] Step 1: The first storage element Z1 of the atomic layer deposition equipment, the chamber body 11, and the pipeline connecting the chamber body 11 and the first storage element Z1 are heated to 90 degrees Celsius, 200 degrees Celsius to 350 degrees Celsius, and 120 degrees Celsius, respectively;

[0110] Step 2: Control the inert gas to flow into the chamber body 11, and simultaneously control the values ​​of the flowmeter L2 and the flowmeter 3 until the pressure value in the chamber body 11 is consistent with the atmospheric pressure value, that is, the reading of the vacuum gauge Z in the chamber body 11 is consistent with the atmospheric pressure value, and stop the inert gas flow, so that the lid of the reaction chamber 11 is opened;

[0111] Step 3: Place the substrate in the chamber body 11, set the readings of flowmeter L2 and flowmeter L3 to 50 sccm, and introduce nitrogen into the chamber body 11 for 1 hour;

[0112] Step 4: Replace the cover of the reaction chamber 1 with the thermal field cover 2;

[0113] Step 5: Turn on the mechanical pump B1 that is connected to the chamber body 11 to evacuate the chamber body 11 until the reading on the display meter X1 is below 5 Pa;

[0114] Step 6: Open the needle valve of the first storage element Z1 and set the flow meter L1 to 100 sccm, so that nitrogen gas flows into the first storage element Z1, and the first precursor in the first storage element Z1 is brought from the bottom of the first storage element A to the top of the first storage element Z1;

[0115] Step 7, open the fourth storage element Z4, and the compressed gas flows outward from the fourth storage element Z4, so that the first switching device Q1 and the second switching device Q2 are changed from the closed state to the open state for 1 second, so that the first precursor flows into the reaction chamber 11 until the reading on the display meter X1 is 80Pa to 90Pa;

[0116] Step 8: Control nitrogen to flow into the chamber body 11 for 10 seconds to purge the unreacted precursor A and the generated by-products in the chamber body 11;

[0117] Step nine, open the third storage element Z3, and introduce the second precursor into the chamber body 11, and the reading of the flow meter L4 is 100 sccm, until the reading of the vacuum gauge Z is 120Pa to 130Pa.

[0118] Step 10, opening the fourth storage element Z4, and the compressed gas flows from the fourth storage element Z4 to the outside, so that the first switching device Q1 and the second switching device Q2 are changed from the closed state to the open state for 5s;

[0119] Step 11: Set the readings of flowmeter L2 and flowmeter L3, control the nitrogen to flow into the chamber body 11, and keep it for 20 seconds to purge the unreacted precursor and generated by-products in the chamber body 11;

[0120] Step 12: After repeating the above steps 6 to 11 for 20 cycles, set the readings of flowmeter L2 and flowmeter L3 to control the nitrogen gas to flow into the chamber body so that the chamber body is in an inert atmosphere;

[0121] Step 13: Plug the outer end plug of the heating element 21 into the power strip. The detection element 23 can detect that the temperature of the chamber body 11 rises rapidly to 250 degrees Celsius to 300 degrees Celsius and maintains in this temperature range for 10 minutes.

[0122] Step 14: After 10 minutes, unplug the plug and pour cold water into the cooling pipe 22, so that the detection element 23 can detect that the temperature in the chamber body 11 has dropped to 200 degrees Celsius;

[0123] Step 15: Repeat steps 6 to 14 until the thickness of the target film layer reaches the expected thickness.

[0124] It is understandable that the reaction chamber 1 may be composed of a chamber body 11 and a thermal field cover 2, or may be composed of a chamber body 11 and a lid provided by the chamber. The above steps 2 to 3 are designed for opening the lid provided by the chamber.

[0125] In some embodiments, reference may be made to Figure 8 and Fig. 9 , Figure 8 Schematic diagram of the temperature rise of the thermal field cover over time. Fig. 9 The schematic diagram of the temperature drop of the thermal field cover over time. The specific heating operation time and the temperature value at each time can be clearly seen in Figure 8 As shown in , the specific cooling operation time and the cooling temperature value at each time can also be Fig. 9 as shown in .

[0126] In some embodiments, reference may be made to Fig.10 and Fig.11 , where "RMS" is the average deviation of the roughness profile from the mean line, Fig.10 It shows the effect diagram of the non-growth area of ​​the initial film layer. The "non-growth area" refers to the part of the substrate that is not coated during the manufacturing process of the atomic layer deposition film. Fig.11 The effect diagram of the target film layer after annealing treatment is shown in FIG. It can be clearly seen that through the annealing treatment of the present application, the target film layer obtained has a smaller roughness, is smoother and has fewer defective particles.

[0127] It should be noted that some of the steps or stages illustrated above are not necessarily executed at the same time, but can be executed at different times, and the execution order of these steps or stages is not necessarily sequential, but can be executed in turn or alternately with other steps or at least part of the steps or stages in other steps. It can be selected according to specific usage requirements and is not specifically limited here.

[0128] The technical features of the above embodiments may be combined arbitrarily. To make the description concise, 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.

[0129] The above embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the patent application. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the patent application shall be subject to the attached claims.

Claims

1. A method for preparing an atomic layer deposition film, characterized in that: include: A reaction chamber is provided, and a substrate is placed in a chamber body of the reaction chamber; the reaction chamber comprises a thermal field cover arranged at an opening of the chamber body, and a heating element and a cooling element are arranged on the thermal field cover; Alternatingly introducing a first precursor and a second precursor into the chamber body at a preset number of times to obtain an initial film layer on the surface of the substrate; The heating element is controlled to heat the initial film layer, and the cooling element is controlled to cool the initial film layer, so as to anneal the initial film layer to obtain a target film layer.

2. The method for preparing an atomic layer deposition film according to claim 1, characterized in that: The step of controlling the heating element to heat the initial film layer, and controlling the cooling element to cool the initial film layer, so as to anneal the initial film layer to obtain a target film layer comprises: The heating process and the cooling process are performed alternately in sequence; The heating process includes controlling the heating element to heat the chamber body, and when the temperature in the chamber body rises to a first target temperature, making the current temperature in the chamber body remain at the first target temperature for a first preset time period; The cooling process includes controlling the cooling element to cool the chamber body, and when the temperature in the chamber body is reduced from the first target temperature to the second target temperature, the current temperature in the chamber body is maintained at the second target temperature for a second preset time period.

3. The method for preparing an atomic layer deposition film according to claim 2, characterized in that: The difference between the first target temperature and the second target temperature is 50 degrees Celsius to 100 degrees Celsius.

4. The method for preparing an atomic layer deposition film according to any one of claims 1 to 3, characterized in that: The first precursor and the second precursor are alternately introduced into the chamber body at a preset number of times to obtain an initial film layer on the surface of the substrate, which includes: Introducing an inert gas into a first storage element containing the first precursor, so that the first precursor can flow from a bottom of the first storage element to a top of the first storage element; The top of the first storage element is controllably connected to the chamber body; and the vapor pressure of the first precursor is lower than the vapor pressure of the second precursor.

5. An atomic layer deposition device, characterized in that: include: A reaction chamber, comprising a chamber body and a thermal field cover disposed at an opening of the chamber body; A heating element, arranged on the thermal field cover; A cooling element is arranged on the thermal field cover.

6. The atomic layer deposition device according to claim 5, characterized in that: One of the heating element and the cooling element is disposed on a side of the thermal field cover facing the interior of the chamber body, and the other is disposed on a side of the thermal field cover facing away from the chamber body; and / or The atomic layer deposition equipment also includes a detection element, which is arranged on the thermal field cover and is used to detect the temperature inside the chamber body; the heating element can heat in response to a detection signal of the detection element, and the cooling element can cool in response to a detection signal of the detection element.

7. The atomic layer deposition device according to claim 5 or 6, characterized in that: The atomic layer deposition apparatus further comprises: A first storage element, for storing a first precursor; an outlet of the first storage element and the interior of the chamber body are controllably connected; A second storage element, for storing an inert gas; a first outlet of the second storage element is communicated with an inlet of the first storage element; The third storage element is used to store the second precursor; the outlet of the third storage element is controllably connected to the chamber body.

8. The atomic layer deposition device according to claim 7, characterized in that: The atomic layer deposition apparatus further includes a first switching device, wherein the first switching device is provided with a first switching port, a second switching port and a third switching port; The first switching port is communicated with the second outlet of the second storage element, the second switching port is communicated with the chamber body, and the third switching port is communicated with the outlet of the first storage element; Among them, the first switching device has a first state and a second state; when the first switching device is in the first state, the first switching port is connected to the second switching port; when the first switching device is in the second state, the first switching port is connected to the second switching port, and the third switching port is connected to the second switching port.

9. The atomic layer deposition device according to claim 8, characterized in that: The atomic layer deposition device further includes a fourth storage element for storing compressed gas; the first switching device is further provided with a fourth switching port, and a movable blocking element is further provided inside the first switching device; The inlet side of the fourth switching port is communicated with the outlet side of the fourth storage element, and the outlet sides of the fourth switching port are all communicated with the first switching port, the second switching port, and the third switching port; In which, the first switching device is in a first state, and the blocking member covers the outlet side of the third switching port and the outlet side of the fourth switching port; the blocking member opens the fourth switching port and the third switching port in response to the compressed gas entering from the fourth switching port, the third switching port is connected to the fourth switching port, and the second switching port is connected to the fourth switching port.

10. The atomic layer deposition device according to claim 7, characterized in that: The atomic layer deposition equipment further includes a second switching device, wherein the second switching device is provided with a first conversion interface and a second conversion interface; The first conversion interface is in communication with the outlet side of the third storage element, and the second conversion interface is in communication with the reaction chamber; Wherein, when the first conversion interface is in a first state, the first conversion interface is connected to the second conversion interface; when the first conversion interface is in a second state, the first conversion interface is not connected to the second conversion interface.

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