WO2021097893A1

WO2021097893A1 - Atomic layer deposition device and method

Info

Publication number: WO2021097893A1
Application number: PCT/CN2019/121707
Authority: WO
Inventors: 卢维尔; 夏洋; 赵丽莉; 李楠; 明帅强
Original assignee: 中国科学院微电子研究所
Priority date: 2019-11-19
Filing date: 2019-11-28
Publication date: 2021-05-27
Also published as: CN112899653A

Abstract

A high-temperature atomic layer deposition device and method. The device comprises a chamber (3), the chamber (3) being a cylindrical tubular cavity structure; a first pipeline (1), the first pipeline (1) being in communication with one end of the chamber (3), and the first pipeline (1) passing through a first precursor into the chamber (3); a second pipeline (2), the second pipeline (2) being in communication with one end of the chamber (3), and the second pipeline (2) passing through a second precursor into the chamber (3); a muffle furnace (4), the muffle furnace (4) being disposed outside the chamber (3); and an evacuation pipeline (6), one end of the evacuation pipeline (6) being communicated with the other end of the chamber (3), such that the technical problem of unsuitability of precursors with low activity for atomic layer deposition caused by the low efficiency in heating and cooling of the chamber of the atomic layer deposition device because the chamber is made of metal and is large is solved, and the technical effects such as guiding the unidirectional flow of precursor gas, shortening the process purging duration, quickly heating or cooling the chamber, implementing temperature-controlled deposition or high-temperature annealing, and improving the crystallinity of a deposited film are achieved.

Description

Atomic layer deposition device and method

Cross-references to related applications

This application claims the priority of patent application No. 201911136184.3 filed with the Chinese Patent Office on November 19, 2019, the entire content of which is hereby incorporated into this application by reference.

Technical field

This application relates to the field of semiconductor technology, in particular to a high-temperature atomic layer deposition apparatus and method.

Background technique

Atomic layer deposition (ALD) is a special chemical vapor deposition technology that can realize monoatomic layer deposition of thin film preparation equipment, with excellent shape retention, large area uniformity and precise film thickness control Features. Since the International Semiconductor Industry Association listed ALD as a candidate technology compatible with microelectronics in 2001, it has won widespread attention from the industry and academia. In 2007, Intel introduced ALD deposition technology into the production line at the 45nm technology node in the semiconductor industry, which reduced the power consumption of the microprocessor and increased the operating speed. In recent years, ALD technology has been widely used in microelectronics, optoelectronics, optics, nanotechnology, micromechanical systems, energy, catalysis and other fields.

At present, atomic layer deposition technology shows great commercial prospects, but it also faces great challenges. First of all, ALD precursors need to have high reactivity. Therefore, suitable ALD precursors are still scarce at present, which directly affects the deposition of some key materials and the quality of the films obtained. Secondly, the current thin films obtained by ALD technology are mainly amorphous thin films and single crystal thin films, and it is difficult to obtain high crystallinity thin film materials, which limits the application of ALD technology in these fields. The use of high-temperature ALD technology can provide higher energy to the precursor, thereby reducing the requirement for high activity of the reaction precursor and expanding the choice of reaction precursors. At the same time, the use of high temperature can improve the crystallinity of the prepared film, so as to meet the requirements of certain devices.

A technical problem in the prior art is that the chamber of the atomic layer deposition equipment is made of metal and the chamber is relatively large, and the heating and cooling speed of the chamber is very slow, which is not suitable for the atomic layer deposition precursor with lower activity.

Summary of the invention

The embodiment of the present invention provides a high-temperature atomic layer deposition apparatus and method to solve the problem that the chamber of the atomic layer deposition equipment in the prior art is made of metal and the cavity is large, and the temperature rise and fall speed of the chamber is very slow, which is not suitable Technical problems of atomic layer deposition precursors with lower activity.

In order to solve the above-mentioned problems, in the first aspect, an embodiment of the present invention provides an atomic layer deposition apparatus, the apparatus comprising: a chamber, the chamber is a cylindrical tubular cavity structure; a first pipeline, the first A pipeline communicates with one end of the chamber, and the first pipeline passes through the first precursor into the chamber; a second pipeline, the second pipeline and the chamber One end is connected, and the second pipeline passes through the second precursor to enter the chamber; a muffle furnace, the muffle furnace is arranged outside the chamber; a vacuum pipeline, the vacuum pipeline One end communicates with the other end of the chamber.

In some embodiments, the device includes: a vacuum pump connected to the other end of the vacuum pipe, and the vacuum pump evacuates the chamber through the vacuum pipe.

In some embodiments, the device includes a vacuum gauge, which is arranged on the first pipeline, the second pipeline, or the vacuuming pipeline.

In some embodiments, the first precursor and the second precursor flow in a unidirectional straight line in the chamber.

In some embodiments, the wall thickness of the chamber is 1-10 mm, the length of the chamber is 0.6-3 m, and the inner diameter of the chamber is 2.5-20 cm.

In some embodiments, the heat-resistant temperature of the chamber is ≤1200°C.

In some embodiments, the chamber is made of quartz tube or corundum tube.

In some embodiments, the heating temperature of the muffle furnace is 25-1200°C.

In a second aspect, an embodiment of the present invention provides a method of atomic layer deposition. The method includes: placing a silicon wafer in a chamber, and the surface of the silicon wafer is aligned with the flow directions of the first precursor and the second precursor. Consistent; turn on the vacuum pump and the muffle furnace, use the muffle furnace to heat the chamber to a first temperature; detect the air pressure in the chamber in real time according to the vacuum gauge, and when the air pressure in the chamber reaches a predetermined threshold, pass The first pipeline and the second pipeline alternately pass the first precursor or the second precursor into the chamber; the first precursor and the second precursor in the chamber are heated by the muffle furnace When the second precursor reaches the second temperature, the thin film material is obtained by atomic layer deposition.

The above one or more technical solutions in the embodiments of the present invention have at least one or more of the following technical effects:

The embodiment of the present invention provides a high-temperature atomic layer deposition apparatus and method. The apparatus includes a chamber, and the chamber has a cylindrical tubular cavity structure; a first pipeline, the first pipeline and the chamber One end of the chamber is communicated, and the first pipeline passes through the first precursor to enter the chamber; the second pipeline, the second pipeline communicates with one end of the chamber, and the second pipe The second precursor body enters the chamber; a muffle furnace, the muffle furnace is arranged on the outside of the chamber; an evacuation pipeline, one end of the evacuation pipeline and the other end of the chamber Connected. By adopting a cylindrical tubular cavity structure chamber, the precursor passes into the pipeline set at one end of the chamber, and the air extraction pipeline is set at the other end of the cylindrical chamber, which is beneficial to realize the unidirectional flow of the precursor airflow and shorten the process The purge time can quickly raise and lower the temperature, realize temperature-controlled deposition or high-temperature annealing, and improve the technical effect of the crystallinity of the deposited film. This solves the problem that the chamber of the atomic layer deposition equipment in the prior art is metal and the cavity is large. The heating and cooling speed of the chamber is very slow, which is not suitable for the technical problems of the precursors of atomic layer deposition with low activity.

The above description is only an overview of the technical solution of the present invention. In order to understand the technical means of the present invention more clearly, it can be implemented in accordance with the content of the specification, and in order to make the above and other objectives, features and advantages of the present invention more obvious and understandable. In the following, specific embodiments of the present invention will be cited.

Description of the drawings

FIG. 1 is a schematic diagram of the structure of a high-temperature atomic layer deposition apparatus in an embodiment of this specification;

Figure 2 is a flow chart of the high-temperature atomic layer deposition method in the embodiment of the specification;

Description of reference signs: first pipeline 1, second pipeline 2, chamber 3, muffle furnace 4, vacuum gauge 5, vacuuming pipeline 6, vacuum pump 7.

Detailed ways

The embodiment of the present invention provides a high-temperature atomic layer deposition apparatus and method to solve the problem that the chamber of the atomic layer deposition equipment in the prior art is made of metal and the cavity is large, and the temperature rise and fall speed of the chamber is very slow, which is not suitable The technical problem of the low-activity atomic layer deposition precursor has achieved the unidirectional flow of the precursor gas flow, shortened the process purge time, can quickly raise and lower the temperature, realize temperature-controlled deposition or high-temperature annealing, and improve the crystallinity of the deposited film Technical effect.

A high-temperature atomic layer deposition apparatus in an embodiment of the present invention includes: a chamber, the chamber having a cylindrical tubular cavity structure; a first pipeline, the first pipeline communicating with one end of the chamber, And the first pipeline leads into the first precursor into the chamber; the second pipeline, the second pipeline communicates with the one end of the chamber, and the second pipeline leads The second precursor enters the chamber; a muffle furnace, the muffle furnace is arranged outside the chamber; and an evacuation pipeline, one end of the evacuation pipeline communicates with the other end of the chamber, It solves the technical problem that the chamber of the atomic layer deposition equipment in the prior art is made of metal and the chamber is large, and the heating and cooling rate of the chamber is very slow, which is not suitable for the atomic layer deposition precursor with lower activity, and the precursor gas flow is achieved The unidirectional flow shortens the process purge time, can quickly raise and lower the temperature, realize temperature-controlled deposition or high-temperature annealing, and improve the technical effect of the crystallinity of the deposited film.

In order to make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments These are a part of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work shall fall within the protection scope of the present invention.

An embodiment of the present invention provides an atomic layer deposition apparatus. Please refer to FIG. 1. The apparatus includes

The chamber 3 is a cylindrical tubular cavity structure.

Further, the wall thickness of the cavity 3 may be 1-10 mm, the length of the cavity 3 may be 0.6-3 m, and the inner diameter of the cavity 3 may be 2.5-20 cm. In some embodiments, the heat-resistant temperature of the chamber 3 is ≤1200°C. Further, the chamber 3 can be made of a quartz tube or a corundum tube.

In a specific embodiment, the chamber 3 is a cylindrical tubular cavity structure, and the chamber 3 is made of a quartz tube or a corundum tube. It has the characteristics of fast temperature rise and high temperature resistance, and can quickly raise and lower temperature. The temperature of the chamber can be controlled at room temperature to 1200°C for deposition process or high temperature annealing. Wherein, the chamber 3 adopts a quartz tube. The wall thickness of the cavity 3 is 1-10 mm, the length of the cavity 3 is 0.6-3 m, and the inner diameter of the cavity 3 is 2.5-20 cm. Preferably, the cylindrical tubular cavity of the chamber 3 has a wall thickness of 3 mm, a tube length of 1.5 m, an inner diameter of 5 cm, and a high temperature resistance of 1200°C.

The device further includes: a first pipeline 1, the first pipeline 1 communicates with one end of the chamber 3, and the first pipeline 1 passes through a first precursor into the chamber 3; The second pipeline 2, the second pipeline 2 communicates with one end of the chamber 3, and the second pipeline 2 passes through the second precursor to enter the chamber 3; and the vacuum pipeline 6, One end of the vacuum pipe 6 is connected to the other end of the chamber 3.

Further, the first precursor and the second precursor flow in a unidirectional straight line in the chamber 3.

Specifically, the first pipeline 1 communicates with one end of the chamber 3, and the first pipeline 1 passes through the first precursor into the chamber 3, and the second pipeline 2 is connected to One end of the chamber 3 is connected, and the second pipeline 2 passes through the second precursor into the chamber 3. The first precursor and the second precursor alternately pass into the first pipeline 1 and the second pipeline 2 respectively, and enter the chamber, and the vacuum pipeline 6 is arranged in the chamber At the other end of 3, this is conducive to realizing the unidirectional linear flow of the precursor gas flow and shortening the purging time in the deposition process.

The device further includes: a muffle furnace 4, the muffle furnace 4 is arranged outside the chamber 3.

The heating temperature of the muffle furnace 4 may be 25-1200°C. In some embodiments, the device further includes: a vacuum pump 7, which is connected to the other end of the vacuum pipe 6, and the vacuum pump 7 drives the chamber 3 through the vacuum pipe 6 Evacuate to vacuum. In some embodiments, the device further includes: a vacuum gauge 5 arranged on the first pipeline 1, the second pipeline 2 or the vacuuming pipeline 6.

Specifically, the muffle furnace 4 is arranged outside the chamber 3, and the muffle furnace 4 can be used to quickly heat the chamber 3, and the heating temperature of the muffle furnace 4 is 25-1200°C According to different film materials, different crystallization temperatures are required, and the heating chamber of the muffle furnace 4 is heated to prepare a single crystal film of excellent quality. The device of the embodiment of the present application further includes a vacuum pump 7 and a vacuum gauge 5. The vacuum pump 7 is connected to the other end of the vacuum pipeline 6, and the vacuum pump 7 evacuates the chamber 3 through the vacuum pipeline 6. The vacuum gauge 5 is arranged on the first pipeline 1, the second pipeline 2 or the vacuum pipeline 6. Preferably, the vacuum gauge 5 can be installed on the vacuum pipeline 6, Real-time detection shows the air pressure in the chamber 3. When the air pressure in the chamber 3 meets the requirements for the atomic layer deposition of thin film materials, the first pipeline 1 and the second pipeline 2 are alternately passed through A precursor and a second precursor deposit thin film materials.

The embodiment of the present invention also provides a high-temperature atomic layer deposition method. Please refer to FIG. 2. The method includes step 110-step 140:

Step 110: Place the silicon wafer in the chamber, and the surface of the silicon wafer is consistent with the flow direction of the first precursor and the second precursor;

Step 120: Turn on the vacuum pump and the muffle furnace, and use the muffle furnace to heat the chamber to a first temperature;

In one embodiment, a 5cm×5cm silicon wafer is placed horizontally in the chamber, so that the surface of the silicon wafer is consistent with the flow direction of the first precursor and the second precursor, which is beneficial to the uniform adsorption of the precursor; The vacuum pump turns on the muffle furnace heating chamber, and the muffle furnace is used to heat the chamber to a first temperature. As in the embodiment of the present invention, aluminum nitride is deposited, and the first precursor is passed into the first pipeline. A precursor is an aluminum source, and the aluminum source is preferably trimethylaluminum; the second precursor is passed into the second pipeline, and the second precursor is a nitrogen source, and the nitrogen source is preferably ammonia. Since the preferred process temperature of the two selected precursors is 400°C, the substrate temperature needs to be maintained at 400°C. At this time, the temperature of the chamber is heated to 400°C and maintained at a constant temperature through a muffle furnace. temperature.

Step 130: Detect the air pressure in the chamber in real time according to the vacuum gauge, and when the air pressure in the chamber reaches a predetermined threshold, alternately pass the first precursor into the chamber through the first pipeline and the second pipeline Or the second precursor;

Step 140: heating the first precursor and the second precursor in the chamber to a second temperature by the muffle furnace, and obtaining a thin film material by atomic layer deposition.

Specifically, the air pressure in the chamber is detected in real time by a vacuum gauge, and when the air pressure in the chamber reaches a predetermined threshold, the first precursor is alternately introduced into the chamber through the first pipeline and the second pipeline. Or the second precursor is deposited to obtain a thin film material. When the crystallization temperature of some thin film materials is relatively high, which may be higher than the temperature window of the atomic layer deposition process, when the film needs to be deposited at a higher temperature, the chamber is heated to the second temperature by using the muffle furnace After reaching the second temperature, the temperature is maintained for a certain period of time, and the single crystal film material with excellent quality will be obtained after the temperature is lowered.

The technical solutions provided in the embodiments of this application have at least the following technical effects or advantages:

The embodiment of the present invention provides a high-temperature atomic layer deposition apparatus and method. The apparatus includes a chamber, and the chamber has a cylindrical tubular cavity structure; a first pipeline, the first pipeline and the chamber One end of the chamber is communicated, and the first pipeline passes through the first precursor to enter the chamber; the second pipeline, the second pipeline communicates with one end of the chamber, and the second pipe The second precursor enters the chamber; the muffle furnace, the muffle furnace is arranged outside the chamber; and the vacuum pipeline, one end of the vacuum pipeline is connected to the other of the chamber Connect at one end. By adopting a chamber with a cylindrical tubular cavity structure, the precursor passes into the pipeline set at one end of the chamber, and the air extraction pipeline is set at the other end of the cylindrical chamber, which is beneficial to realize the unidirectional flow of the precursor airflow and shorten the process The purging time can quickly raise and lower the temperature, realize temperature-controlled deposition or high-temperature annealing, improve the crystallinity of the deposited film, and solve the problem that the chamber of the atomic layer deposition equipment in the prior art is made of metal and has a large cavity. The temperature increase and decrease rate of the chamber is very slow, which is not suitable for the technical problem of the atomic layer deposition precursor with lower activity.

Although the preferred embodiments of the present invention have been described, those skilled in the art can make additional changes and modifications to these embodiments once they learn the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications falling within the scope of the present invention.

Obviously, those skilled in the art can make various changes and modifications to the embodiments of the present invention without departing from the spirit and scope of the embodiments of the present invention. In this way, if these modifications and variations of the embodiments of the present invention fall within the scope of the claims of the present invention and equivalent technologies, the present invention is also intended to include these modifications and variations.

Claims

An atomic layer deposition device, including:

The chamber (3), the chamber is a cylindrical tubular cavity structure;

A first pipeline (1), the first pipeline communicates with one end of the chamber, and the first pipeline passes through a first precursor into the chamber;

A second pipeline (2), the second pipeline communicates with the one end of the chamber, and the second pipeline passes through a second precursor into the chamber;

A muffle furnace (4), the muffle furnace is arranged outside the chamber; and

An evacuation pipeline (6), one end of the evacuation pipeline communicates with the other end of the chamber.
5. The atomic layer deposition apparatus of claim 1, wherein the apparatus further comprises:

A vacuum pump (7), the vacuum pump is connected with the other end of the evacuating pipeline, and the vacuum pump evacuates the chamber through the evacuating pipeline.
5. The atomic layer deposition apparatus of claim 1, wherein the apparatus further comprises:

The vacuum gauge is arranged on the first pipeline, the second pipeline or the vacuuming pipeline.
8. The atomic layer deposition apparatus according to claim 1, wherein the first precursor and the second precursor flow in a unidirectional straight line in the chamber.
3. The atomic layer deposition apparatus according to claim 1, wherein the wall thickness of the chamber is 1-10 mm, the length of the chamber is 0.6-3 m, and the inner diameter of the chamber is 2.5-20 cm.
The atomic layer deposition apparatus according to claim 1, wherein the heat-resistant temperature of the chamber is ≤ 1200°C.
The apparatus for crystallization of thin film materials according to claim 1, wherein the chamber is made of a quartz tube or a corundum tube.
The atomic layer deposition apparatus according to claim 1, wherein the heating temperature of the muffle furnace is 25 to 1200°C.
A method of atomic layer deposition, including:

Placing the silicon wafer in the chamber, and the surface of the silicon wafer is consistent with the flow direction of the first precursor and the second precursor;

Turn on the vacuum pump and the muffle furnace, and use the muffle furnace to heat the chamber to a first temperature;

The air pressure in the chamber is detected in real time by a vacuum gauge. When the air pressure in the chamber reaches a predetermined threshold, the first precursor or the first precursor or the first precursor is alternately passed into the chamber through the first pipeline and the second pipeline. Second precursor; and

The first precursor and the second precursor in the chamber are heated by the muffle furnace to a second temperature, and a thin film material is obtained by atomic layer deposition.