CN112941493B - Device and method for rapid vapor deposition of pulse type uniform film - Google Patents

Device and method for rapid vapor deposition of pulse type uniform film Download PDF

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CN112941493B
CN112941493B CN202110127372.0A CN202110127372A CN112941493B CN 112941493 B CN112941493 B CN 112941493B CN 202110127372 A CN202110127372 A CN 202110127372A CN 112941493 B CN112941493 B CN 112941493B
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valve
pipeline
carrier gas
inert carrier
reaction chamber
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CN112941493A (en
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冯昊
李建国
张王乐
惠龙飞
秦利军
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Xian Modern Chemistry Research Institute
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
    • C23C16/45534—Use of auxiliary reactants other than used for contributing to the composition of the main film, e.g. catalysts, activators or scavengers
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/52—Controlling or regulating the coating process

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

The application discloses a device and a method for pulse type uniform film rapid vapor deposition, comprising a reaction chamber, a sampling part arranged at one end of the reaction chamber and a plurality of precursor vapor injection units arranged at the other end of the reaction chamber; the precursor steam injection unit comprises a precursor steam pipeline and an inert carrier gas pipeline which are converged into a main pipeline and then extend into the reaction chamber, a vacuum evacuation branch communicated with the precursor steam pipeline, an inert carrier gas evacuation branch communicated with the inert carrier gas pipeline, a gas distributor positioned in the reaction chamber and connected with the end part of the main pipeline, a flow controller arranged on the inert carrier gas pipeline, valves arranged on each pipeline and the branch pipeline and a storage tank connected with the precursor steam pipeline. The precursor vapors can be continuously or intermittently injected in pulse mode, and the concentration of the precursor vapors can be diluted and adjusted by inert carrier gas; the reaction precursor can be saved to the greatest extent while the film deposition speed is ensured, the resource waste is reduced, and the environmental pollution is reduced.

Description

Device and method for rapid vapor deposition of pulse type uniform film
Technical Field
The application belongs to the field of device development and film material preparation, relates to a vapor film deposition technology including chemical vapor deposition and atomic layer deposition, and in particular relates to a device and a method for pulse type uniform film rapid vapor deposition.
Background
Chemical vapor deposition is a technique that utilizes one or more precursor species in a gaseous or vapor state to decompose or react at a gas-phase or gas-solid interface to produce a solid deposit. Atomic layer deposition can be considered as one of chemical vapor deposition reactions that achieve controlled growth of thin films on the surface of a substrate material by means of two-step surface chemical reactions with self-limiting properties by alternately injecting gaseous precursors into the reactor. CVD and ALD are both chemical vapor deposition techniques in a broad sense, and are both suitable for surface modification of substrate materials with complex pore, trench structures and high specific surface areas, but there are significant differences between the two techniques: unlike CVD processes, the two-step surface chemistry involved in ALD processes is self-limiting. In the ALD reaction process, a first precursor is firstly adsorbed on the surface of a substrate, after saturated adsorption is completed, unreacted precursor is removed through purging by inert carrier gas, and then a second precursor is injected to react with the first precursor to generate a target product. The self-limiting nature of the ALD reaction allows unreacted precursors to be removed after each surface reaction step has taken place, ensuring that the two precursors can react in exactly stoichiometric ratios, thereby achieving precise control of the film growth process at the single atomic layer scale.
The thin film deposited by the ALD technology has the advantages of low deposition temperature, strong adhesion between the thin film and a substrate, high density and the like, but has the defect of slower growth rate of the thin film (S.M. George, atomic layer deposition: an overview, chem. Rev.110 (2010) 111-131); the deposition of thin films by CVD techniques has the advantages of high deposition temperature, fast film rate, etc., but its film density and adhesion to the substrate material are inferior to those of thin films prepared by ALD (X.Wang, G.Yushin, chemical vapor deposition and atomic layer deposition for advanced lithium ion batteries and supercapacitors, energy environment. Sci.8 (2015) 1889-1904.). Currently, a single CVD apparatus or ALD apparatus is difficult to achieve multiple precursor vapor injection, including ALD and CVD, and the preparation of ALD-VCD composite thin films that have both ALD and CVD technical advantages is not possible. In addition, conventional CVD or ALD apparatus lack control over the precursor concentration and gas distribution during thin film deposition, which can lead to waste of precursor vapor and failure to deposit target thin films with high uniformity on the surface of large-area substrate materials.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the application aims to provide a pulse type uniform film rapid vapor deposition device and method, each precursor vapor can realize continuous pulse injection and intermittent pulse injection, the precursor vapor concentration of each precursor vapor pulse is adjustable, the uniform deposition of a film on the surface of a sample is realized through arranging a gas distributor at the front end of the sample, and the typical ALD film deposition long mode, the typical CVD film deposition mode or the novel ALD+CVD film deposition mode is realized by controlling the injection mode and injection time sequence of each precursor vapor.
In order to achieve the above purpose, the technical scheme of the application is as follows:
a pulse type uniform film rapid vapor deposition device comprises a reaction chamber, a sampling part arranged at one end of the reaction chamber, and a plurality of precursor vapor injection units arranged at the other end of the reaction chamber;
the precursor vapor injection unit includes: the precursor vapor pipeline and the inert carrier gas pipeline are converged into a main pipeline and then extend into the reaction chamber, a vacuum evacuation branch communicated with the precursor vapor pipeline, an inert carrier gas evacuation branch communicated with the inert carrier gas pipeline, a gas distributor positioned in the reaction chamber and connected with the end part of the main pipeline, a flow controller arranged on the inert carrier gas pipeline, valves arranged on the pipelines and the branch pipeline and a storage tank connected with the precursor vapor pipeline.
The application also comprises the following technical characteristics:
specifically, the precursor vapor injection units are an A precursor vapor injection unit and a B precursor vapor injection unit respectively;
the a-precursor vapor injection unit includes: the precursor vapor pipeline A and the inert carrier gas pipeline A are converged into a main pipeline A and then extend into the reaction chamber, a branch vacuum evacuation branch A arranged on the precursor vapor pipeline A, a branch inert carrier gas evacuation branch A arranged on the inert carrier gas pipeline A, a storage tank A connected on the precursor vapor pipeline A, a gas distributor A positioned in the reaction chamber and connected at the end part of the main pipeline A, a flow controller A arranged on the inert carrier gas pipeline A, a valve AI arranged on the precursor vapor pipeline A, a valve AIII arranged on the inert carrier gas pipeline A, a valve AII arranged on the vacuum evacuation branch A and a valve AIV arranged on the inert carrier gas evacuation branch A; the valve AI is positioned between the storage tank A and the valve AII, and the inert carrier gas evacuation branch A is positioned between the valve AIII and the flow controller A;
the B precursor vapor injection unit includes: the precursor vapor pipeline B and the inert carrier gas pipeline B are combined into a main pipeline B and then extend into the reaction chamber, a branch vacuum evacuation branch B arranged on the precursor vapor pipeline B, a branch inert carrier gas evacuation branch B arranged on the inert carrier gas pipeline B, a storage tank B connected on the precursor vapor pipeline B, a gas distributor B positioned in the reaction chamber and connected at the end part of the main pipeline B, a flow controller B arranged on the inert carrier gas pipeline B, a valve BI arranged on the precursor vapor pipeline B, a valve BIII arranged on the inert carrier gas pipeline B, a valve BII arranged on the vacuum evacuation branch B and a valve BIV arranged on the inert carrier gas evacuation branch B; and valve BI is located between reservoir B and valve BII, and inert carrier gas evacuation branch B is located between valve BIII and flow controller B.
Specifically, the vacuum evacuation branch A and the vacuum evacuation branch B are both connected with a vacuum pump I;
the controllable gas flow rate of the flow controller A and the flow controller B is 0-500sccm; the switching time of each valve is 0-10000s.
Specifically, the gas distributor is provided with a plurality of gas outlet holes, and the gas distributor is communicated with the main pipeline through a metal pipeline; the gas distributor is arranged close to the sample to be treated; after entering the gas distributor, the precursor vapor is uniformly distributed on the surface of the sample to be treated through a plurality of gas outlet holes.
Specifically, the reaction chamber, the main pipeline, the precursor steam pipeline and the storage tank are all sleeved with heating sleeves.
Specifically, the sampling portion includes the cross connection, and the sealed intercommunication reaction chamber of first interface of cross connection, the second interface of cross connection even has vacuum pump II and is equipped with manual angle valve on the second interface, and the third interface of cross connection is the sample and gets the mouth of sending, and the fourth interface of cross connection is equipped with vacuum sensor.
A method for pulse type uniform film rapid vapor deposition includes controlling valve switch on each precursor vapor pipeline and vacuum evacuation branch to realize continuous pulse type injection of each precursor vapor into reaction chamber or intermittent pulse type injection of precursor vapor into reaction chamber;
the injection time sequence of different precursor steam pulses is realized by controlling the switching time length of each valve on each precursor steam pipeline and each valve on the inert gas carrying pipeline;
by controlling the injection mode and injection time sequence of each precursor vapor, an ALD thin film deposition mode, a CVD thin film deposition mode and an ALD+CVD thin film deposition mode can be realized; and the concentration of each precursor vapor can be diluted and adjusted before being injected into the reaction chamber.
Specifically, in the ALD thin film deposition mode in the method, reaction precursor vapor pulses are alternately injected into a reaction chamber, inert carrier gas purging processes are inserted between different reaction precursor vapor pulse injection, and a target thin film with accurately controllable thickness is obtained on the surface of a sample to be processed; the method specifically comprises the following steps:
step 1: opening a valve AI, and injecting precursor vapor A into the reaction chamber for a period of time t1;
step 2: closing the valve AI, opening the valve AIII, injecting inert carrier gas to blow unadsorbed A precursor molecules physically adsorbed on the surface of the sample to be processed and byproducts generated by surface chemical reaction out of the reaction chamber, wherein the injection time of the inert carrier gas is t2;
step 3: opening a valve BI, and injecting precursor steam B into the reaction chamber for a period of time t3;
step 4: closing a valve BI, opening the valve BIII, injecting inert carrier gas to blow unadsorbed B precursor molecules physically adsorbed on the surface of the sample to be processed and byproducts generated by surface chemical reaction out of the reaction chamber, wherein the injection time of the inert carrier gas is t4;
and (3) repeatedly executing the steps 1-4, and depositing a target film with a required thickness on the surface of the sample to be treated.
Specifically, in the CVD film deposition mode in the method, each reaction precursor vapor pulse is synchronously injected into a reaction chamber, and each reaction precursor vapor is subjected to chemical reaction in a gas phase region to generate a target product and is deposited on the surface of a sample to be processed to form a target film; the method specifically comprises the following steps:
step 1: simultaneously opening a valve AI and a valve BI, and synchronously injecting precursor vapor A and precursor vapor B into the reaction chamber, wherein the injection duration is t5;
step 2: after the target film grows rapidly on the surface of the sample to be treated and reaches the required target thickness, simultaneously closing the valve AI and the valve BI, opening the valve AIII and the valve BIII, injecting inert carrier gas to blow precursor molecules which do not participate in the reaction out of the reaction chamber, and injecting the precursor molecules for a period of time of t6.
Specifically, the ALD+CVD film deposition mode in the method is different precursor vapor injection modes and has the precursor vapor injection modes in the ALD film deposition mode and the CVD film deposition mode, different precursor vapor pulse injection sequences are partially overlapped, and the rapid vapor deposition of the uniform film is realized, and the method specifically comprises the following steps:
step 1: opening a valve AI, and injecting precursor vapor A into the reaction chamber for a period of time of t7+t8; when the duration of pulse injection of the precursor vapor A into the reaction chamber reaches t7, opening a valve BI, and injecting the precursor vapor B into the reaction chamber, wherein the duration of injection is t8;
step 2: closing the valve AI, keeping the valve BI in an open state, and continuously injecting the precursor steam pulse B into the reaction chamber for the injection time period of t9;
step 3: opening a valve AIII and a valve BIII to inject inert carrier gas to blow precursor molecules which do not participate in the reaction out of the reaction chamber, wherein the injection time is t10;
and (3) repeatedly executing the steps 1-3, and depositing a target film with a required thickness on the surface of the sample to be treated.
Compared with the prior art, the application has the beneficial technical effects that:
1. the precursor vapors of the application can be continuously and intermittently injected in pulse form, and the concentration of the precursor vapors of each precursor vapor pulse can be diluted and adjusted by the bypass inert carrier gas.
2. The modularized gas distributor can realize the uniformity of film deposition on the surfaces of various samples to be treated.
3. The application can realize various thin film deposition thin films by controlling the injection mode and injection time sequence of each precursor vapor, including a typical ALD thin film deposition long mode, a typical CVD thin film deposition mode or a novel ALD+CVD thin film deposition mode. The precursor vapor injection modes for the three film deposition can control the concentration of precursor vapor by controlling the injection and dilution of bypass carrier gas, so that the reaction precursor can be furthest saved while the film deposition speed is ensured, the resource waste is reduced, and the environmental pollution is reduced.
4. The application can realize the preparation of ALD-CVD composite film, fully exert the respective advantages of ALD technology and CVD technology, and realize the rapid deposition of film while ensuring the quality of deposited film.
Drawings
Fig. 1 is a schematic view of the overall structure of the apparatus of the present application, wherein (a) is a front view of the gas distributor, (b) is a rear view of the gas distributor, and (c) is a top view of the gas distributor.
Reference numerals meaning:
100. reaction chamber, 201, precursor vapor line a,202, inert carrier gas line a,203, main line a,204, vacuum evacuation branch a,205, inert carrier gas evacuation branch a,206, reservoir a,207, gas distributor a,208, flow controller a,209, valve AI,210, valve AII,211, valve AIII,212, valve AIV;301. precursor vapor line B,302, inert carrier gas line B,303, main line B,304, vacuum evacuation branch B,305, inert carrier gas evacuation branch B,306, reservoir B,307, gas distributor B,308, flow controller B,309, valve BI,310, valve BII,311, valve BIII,312, valve BIV;400. heating jacket, 500. Sample to be treated; 601. vacuum pump II,602, manual angle valve 603, sample taking port 604, vacuum sensor; 701. and a vacuum pump I.
Detailed Description
The application provides a device and a method for pulse type uniform film rapid vapor deposition, wherein each precursor vapor can realize continuous pulse injection and intermittent pulse injection, the precursor vapor concentration of each precursor vapor pulse is adjustable, the uniform deposition of a film on the surface of a sample is realized through arranging a gas distributor at the front end of the sample, and a typical ALD film deposition long mode, a typical CVD film deposition mode or a novel ALD+CVD film deposition mode is realized by controlling the injection mode and injection time sequence of each precursor vapor. (1) In a typical ALD film deposition precursor vapor injection mode, different precursors are alternately injected into a reaction chamber and need to be inserted with an inert carrier gas purging process, so that self-limiting surface chemical reaction of each precursor vapor on the surface of a substrate is realized and a target product is generated; (2) A typical CVD film deposition precursor vapor injection mode, that is, multiple precursor vapors are simultaneously injected into a reaction chamber, so that the multiple precursor vapors complete a gas phase chemical reaction in a gas phase region, generate a target product, and deposit on the surface of a substrate; (3) The novel ALD+CVD film deposition precursor vapor injection mode can be realized, namely, the overlapping time length of different precursor vapor injection pulses is controlled, namely, the target film is obtained through the chemical reaction of the substrate surface and the chemical reaction of the gas phase region, and the advantages of the ALD mode and the CVD mode can be simultaneously realized in the film deposition speed and the control precision.
The application provides a pulse type uniform film rapid vapor deposition device, which comprises a reaction chamber 100, a sampling part arranged at one end of the reaction chamber, and a plurality of precursor vapor injection units arranged at the other end of the reaction chamber.
The precursor vapor injection unit includes: the precursor vapor pipeline and the inert carrier gas pipeline are converged into a main pipeline and then extend into the reaction chamber, a vacuum evacuation branch communicated with the precursor vapor pipeline, an inert carrier gas evacuation branch communicated with the inert carrier gas pipeline, a gas distributor positioned in the reaction chamber and connected with the end part of the main pipeline, a flow controller arranged on the inert carrier gas pipeline, valves arranged on the pipelines and the branch pipeline and a storage tank connected with the precursor vapor pipeline.
The precursor steam pipeline is directly led to the reaction chamber, and when the case valve of the precursor steam pipeline is in an open state and the valve of the vacuum evacuation branch is in a closed state, the precursor steam is injected into the reaction chamber.
The vacuum evacuation branch is directly connected to the vacuum pump or connected to the vacuum pump through each vacuum valve pipe fitting, and redundant precursor steam on the precursor steam pipeline is evacuated when the valve of the precursor steam pipeline is in a closed state and the valve of the vacuum evacuation branch is in an open state, so that pipeline blockage or cross contamination is avoided.
When the valve of the inert carrier gas pipeline is in an open state and the valve of the inert carrier gas emptying branch pipeline is in a closed state, the inert carrier gas in the inert carrier gas pipeline is injected into the reaction chamber, and the precursor vapor injected simultaneously is diluted and adjusted.
The inert carrier gas emptying branch is directly led to the atmosphere, and when the valve of the inert carrier gas pipeline is in a closed state and the valve of the inert carrier gas emptying branch is in an open state, inert carrier gas transmitted by the mass flowmeter is emptied, so that the pressure in the pipeline is prevented from being build.
In this embodiment, more specifically, the plurality of precursor vapor injection units are an a-precursor vapor injection unit and a B-precursor vapor injection unit, respectively.
The a-precursor vapor injection unit includes: the precursor vapor pipeline A201 and the inert carrier gas pipeline A202 are converged into a main pipeline A203 and then extend into the reaction chamber 100, a branch vacuum evacuation branch A204 arranged on the precursor vapor pipeline A201, a branch inert carrier gas evacuation branch A205 arranged on the inert carrier gas pipeline A202, a storage tank A206 connected on the precursor vapor pipeline A201, a gas distributor A207 positioned in the reaction chamber 100 and connected with the end part of the main pipeline A203, a flow controller A208 arranged on the inert carrier gas pipeline A202, a valve AI209 arranged on the precursor vapor pipeline A201, a valve AIII211 arranged on the inert carrier gas pipeline A202, a valve AII210 arranged on the vacuum evacuation branch A204 and a valve AIV212 arranged on the inert carrier gas evacuation branch A205; and valve AI209 is located between reservoir a206 and valve AII210, and inert carrier gas evacuation branch a205 is located between valve AIII211 and flow controller a 208.
The B precursor vapor injection unit includes: the precursor vapor pipeline B301 and the inert carrier gas pipeline B302 are merged into a main pipeline B303 and then extend into the reaction chamber 100, a branch vacuum evacuation branch B304 arranged on the precursor vapor pipeline B301, a branch inert carrier gas evacuation branch B305 arranged on the inert carrier gas pipeline B302, a storage tank B306 connected on the precursor vapor pipeline B301, a gas distributor B307 positioned in the reaction chamber 100 and connected to the end part of the main pipeline B303, a flow controller B308 arranged on the inert carrier gas pipeline B302, a valve BI309 arranged on the precursor vapor pipeline B301, a valve BIII311 arranged on the inert carrier gas pipeline B302, a valve BII310 arranged on the vacuum evacuation branch B304 and a valve BIV312 arranged on the inert carrier gas evacuation branch B305; and valve BI309 is located between tank B306 and valve BII310, and inert carrier gas evacuation branch B305 is located between valve BIII311 and flow controller B308.
Vacuum evacuation branch A204 and vacuum evacuation branch B304 are both connected to vacuum pump I701; the controllable gas flow rate of the flow controller A208 and the flow controller B308 is 0-500sccm; the switching time of each valve is 0-10000s.
The gas distributor is provided with a plurality of gas outlet holes, and the gas distributor is communicated with the main pipeline through a metal pipeline; the gas distributor is arranged close to the sample 500 to be treated; after entering the gas distributor, the precursor vapor is uniformly distributed on the surface of the sample 500 to be processed through a plurality of gas outlet holes.
The reaction chamber 100, the main pipeline, the precursor vapor pipeline and the storage tank are all sleeved with a heating sleeve 400. Different storage tanks and reaction chambers can be heated to target temperatures, corresponding temperature ranges can be set according to the specific temperature required by volatilization of the reaction precursor and the film deposition of the reaction chamber, the temperature of the storage tanks is between room temperature and 400 ℃, and the temperature of the reaction chamber is between 60 and 1000 ℃.
The sampling portion includes the cross connection, and the sealed intercommunication reaction chamber of first interface of cross connection, the second interface of cross connection even has vacuum pump II601 and is equipped with manual angle valve 602 on the second interface, and the third interface of cross connection is sample and gets and send mouthful 603, and the fourth interface of cross connection is equipped with vacuum sensor 604.
The embodiment also provides a pulse type uniform film rapid vapor deposition method, which realizes continuous pulse type injection of each precursor vapor into a reaction chamber or intermittent pulse type injection of the precursor vapor into the reaction chamber by controlling valve switches on each precursor vapor pipeline and a vacuum evacuation branch; the continuous pulse type injection of the precursor vapor into the reaction chamber is realized by controlling a valve of the precursor vapor injection reaction chamber to be in a normally open state and a valve of a vacuum evacuation branch to be in a normally closed state; the intermittent pulse type injection of the precursor vapor into the reaction chamber is realized by controlling the valve of the precursor vapor injection reaction chamber and the valve of the vacuum evacuation branch to be alternately in an open and closed state.
The injection time sequence of different precursor steam pulses is realized by controlling the switching time length of each valve on each precursor steam pipeline and each valve on the inert gas carrying pipeline; the injection timing refers to the duration and sequence of each precursor vapor pulse and inert carrier gas injection into the reaction chamber.
By controlling the injection mode and injection time sequence of each precursor vapor, an ALD thin film deposition mode, a CVD thin film deposition mode and an ALD+CVD thin film deposition mode can be realized; and the concentration of each precursor vapor can be diluted and adjusted before being injected into the reaction chamber. The concentration dilution and adjustment can be carried out before each precursor vapor pulse is injected into the reaction chamber, namely, valves of each precursor vapor pipeline and the inert carrier gas pipeline are synchronously opened, and the concentration of the precursor vapor injected into the reaction chamber can be diluted and adjusted by injecting quantitative inert carrier gas while the precursor vapor is injected.
The valve can be controlled to be opened and closed through pneumatic control or electric control, and is arranged on the gas transmission pipeline to block or open the transmission of gas in the pipeline. The inert carrier gas is nitrogen, argon or helium.
The ALD thin film deposition mode in the method is that each reaction precursor vapor pulse is alternately injected into a reaction chamber, inert carrier gas purging processes are inserted between different reaction precursor vapor pulse injection, and a target thin film with accurately controllable thickness is obtained on the surface of a sample to be processed; the method specifically comprises the following steps:
step 1: opening a valve AI, and injecting precursor vapor A into the reaction chamber for a period of time t1;
step 2: closing the valve AI, opening the valve AIII, injecting inert carrier gas to blow unadsorbed A precursor molecules physically adsorbed on the surface of the sample to be processed and byproducts generated by surface chemical reaction out of the reaction chamber, wherein the injection time of the inert carrier gas is t2;
step 3: opening a valve BI, and injecting precursor steam B into the reaction chamber for a period of time t3;
step 4: closing a valve BI, opening the valve BIII, injecting inert carrier gas to blow unadsorbed B precursor molecules physically adsorbed on the surface of the sample to be processed and byproducts generated by surface chemical reaction out of the reaction chamber, wherein the injection time of the inert carrier gas is t4;
and (3) repeatedly executing the steps 1-4, and depositing a target film with a required thickness on the surface of the sample to be treated.
The CVD film deposition mode in the method is that each reaction precursor vapor pulse is synchronously injected into a reaction chamber, each reaction precursor vapor is subjected to chemical reaction in a gas phase area to generate a target product, and the target product is deposited on the surface of a sample to be processed to form a target film; the method specifically comprises the following steps:
step 1: simultaneously opening a valve AI and a valve BI, and synchronously injecting precursor vapor A and precursor vapor B into the reaction chamber, wherein the injection duration is t5;
step 2: after the target film grows rapidly on the surface of the sample to be treated and reaches the required target thickness, simultaneously closing the valve AI and the valve BI, opening the valve AIII and the valve BIII, injecting inert carrier gas to blow precursor molecules which do not participate in the reaction out of the reaction chamber, and injecting the precursor molecules for a period of time of t6.
The ALD+CVD film deposition mode in the method is different precursor vapor injection modes and has the precursor vapor injection modes in the ALD film deposition mode and the CVD film deposition mode, different precursor vapor pulse injection sequences are partially overlapped, and the rapid vapor deposition of the uniform film is realized, and the method specifically comprises the following steps:
step 1: opening a valve AI, and injecting precursor vapor A into the reaction chamber for a period of time of t7+t8; when the duration of pulse injection of the precursor vapor A into the reaction chamber reaches t7, opening a valve BI, and injecting the precursor vapor B into the reaction chamber, wherein the duration of injection is t8;
step 2: closing the valve AI, keeping the valve BI in an open state, and continuously injecting the precursor steam pulse B into the reaction chamber for the injection time period of t9;
step 3: opening a valve AIII and a valve BIII to inject inert carrier gas to blow precursor molecules which do not participate in the reaction out of the reaction chamber, wherein the injection time is t10;
and (3) repeatedly executing the steps 1-3, and depositing a target film with a required thickness on the surface of the sample to be treated.
The following specific embodiments of the present application are given according to the above technical solutions, and it should be noted that the present application is not limited to the following specific embodiments, and all equivalent changes made on the basis of the technical solutions of the present application fall within the protection scope of the present application.
Example 1:
the present example shows a device and method for pulsed ALD ZnO uniform thin film vapor deposition, the device used in the example being shown in FIG. 1. The film prepared was ZnO, and the two precursors used were Zn (C 2 H 5 ) 2 And H 2 O is respectively arranged in a storage tank A and a storage tank B, the storage tank A and the storage tank B are at room temperature, and the flow rates of mass flow meters of bypass inert carrier gas purging main pipelines of the two storage tanks are both set to be 50sccm. The substrate material is silicon wafer, and the inert carrier gas is N 2 The atomic layer deposition experimental temperature was 110 ℃. All odd valves are set to be in a closed state before being triggered by a program, and all even valves are set to be in an open state before being triggered.
The method specifically comprises the following steps:
step 1: opening valve AI, closing valve AII, opening valve AIII, closing valve AIV, keeping other valves in default state, diluting Zn (C) with inert carrier gas 2 H 5 ) 2 Steam is injected into the reaction chamber through the gas distributor, and the injection time is 5.0s;
step 2: opening valve AIII, closing valve AIV, opening valve BIII, closing valve BIV, keeping other valves in default state, injecting inert carrier gas into the reaction cavity to clean physical adsorption and byproducts and the like on the surface of the silicon wafer, wherein the injection time of the inert carrier gas is 10.0s;
step 3: opening valve BI, closing valve BII, opening valve BIII, closing the valve BIV, keeping other valves in a default state, and diluting H by inert carrier gas 2 O steam is injected into the reaction chamber through the gas distributor, and the injection time is 5.0s;
step 4: opening valve AIII, closing valve AIV, opening valve BIII, closing valve BIV, keeping other valves in default state, injecting inert carrier gas into the reaction cavity to clean physical adsorption and byproducts and the like on the surface of the silicon wafer, wherein the injection time of the inert carrier gas is 10.0s;
repeating the steps 1-4 for 200 times, and depositing a target film with the required thickness on the surface of the silicon wafer.
Example 2:
the embodiment provides a device and a method for vapor deposition of a pulse CVD ZnO uniform film, and the device is shown in figure 1. The film prepared was ZnO, and the two precursors used were Zn (C 2 H 5 ) 2 And H 2 O is respectively arranged in a storage tank A and a storage tank B, the storage tank A and the storage tank B are at room temperature, and the flow rates of mass flow meters of bypass inert carrier gas purging main pipelines of the two storage tanks are both set to be 50sccm. The substrate material is silicon wafer, and the inert carrier gas is N 2 The chemical vapor deposition experiment temperature was 450 ℃. All odd valves are set to be in a closed state before being triggered by a program, and all even valves are set to be in an open state before being triggered.
The method specifically comprises the following steps:
step 1: opening valve AI, closing valve AII, opening valve BI, closing valve BII, opening valve AIII, closing valve AIV, opening valve BIII, closing valve BIV, diluting Zn (C) with inert carrier gas 2 H 5 ) 2 Steam and H2O steam are simultaneously injected into the reaction chamber through the gas distributor, and the injection time is 1000.0s;
step 2: opening valve AIII, closing valve AIV, opening valve BIII, closing valve BIV, keeping other valves in default state, injecting inert carrier gas into the reaction cavity to clean physical adsorption and byproducts and the like on the surface of the silicon wafer, wherein the injection time of the inert carrier gas is 100.0s;
and (3) depositing a target film with a required thickness on the surface of the silicon wafer, and changing the continuous injection time of the two precursors in the step (1) according to the requirement on the film thickness.
Example 3:
the present example shows a device and method for rapid vapor deposition of pulsed ALD+CVD ZnO uniform films, the device used in the example being shown in FIG. 1. The film prepared was ZnO, and the two precursors used were Zn (C 2 H 5 ) 2 And H 2 O is respectively arranged in a storage tank A and a storage tank B, the storage tank A and the storage tank B are at room temperature, and the flow rates of mass flow meters of bypass inert carrier gas purging main pipelines of the two storage tanks are both set to be 50sccm. The substrate material is silicon wafer, and the inert carrier gas is N 2 The silicon wafer is at an ambient temperature of 250 ℃. All odd valves are set to be in a closed state before being triggered by a program, and all even valves are set to be in an open state before being triggered.
The method specifically comprises the following steps:
step 1: opening valve AI, closing valve AII, opening valve AIII, closing valve AIV, keeping other valves in default state, diluting Zn (C) with inert carrier gas 2 H 5 ) 2 Steam is injected into the reaction chamber through the gas distributor, and the injection time is 10.0s; wherein Zn (C 2 H 5 ) 2 When the duration of the steam pulse injection into the reaction chamber reaches 5.0s, opening a valve BI, closing the valve BII, opening a valve BIII, closing a valve BIV, and diluting Zn (C) diluted by inert carrier gas 2 H 5 ) 2 Steam and H 2 O steam is injected into the reaction chamber through the gas distributor at the same time, and the injection time is 5.0s;
step 2: opening the valve BI, closing the valve BII, opening the valve BIII, closing the valve BIV, and keeping other valves in a default state to dilute the H by inert carrier gas 2 O steam is injected into the reaction chamber through the gas distributor, and the injection time is 10.0s;
step 3: opening valve AIII, closing valve AIV, opening valve BIII, closing valve BIV, keeping other valves in default state, injecting inert carrier gas into the reaction cavity to clean physical adsorption and byproducts and the like on the surface of the silicon wafer, wherein the injection time of the inert carrier gas is 20.0s;
repeating the steps 1-3 times, and depositing a target film with the required thickness on the surface of the silicon wafer.
Example 4:
the present example shows a pulsed ALD TiO 2 Apparatus and method for uniform thin film vapor deposition, the apparatus used in the examples is shown in FIG. 1. The prepared film is TiO 2 The two precursors used were respectively Ti (OC 3 H 7 ) 4 And H 2 O 2 The material is respectively arranged in a storage tank A and a storage tank B, the storage tank A is heated to 60 ℃, the storage tank B is at room temperature, and the flow rates of mass flow meters of bypass inert carrier gas purging main pipelines of the two storage tanks are both set to be 40sccm. The substrate material is silicon wafer, the inert carrier gas is Ar, and the atomic layer deposition experiment temperature is 150 ℃. All odd valves are set to be in a closed state before being triggered by a program, and all even valves are set to be in an open state before being triggered.
The method specifically comprises the following steps:
step 1: opening valve AI, closing valve AII, opening valve AIII, closing valve AIV, keeping other valves in default state, diluting Ti (OC) with inert carrier gas 3 H 7 ) 4 Steam is injected into the reaction chamber through the gas distributor, and the injection time is 10.0s;
step 2: opening valve AIII, closing valve AIV, opening valve BIII, closing valve BIV, keeping other valves in default state, injecting inert carrier gas into the reaction cavity to clean physical adsorption and byproducts and the like on the surface of the silicon wafer, wherein the injection time of the inert carrier gas is 20.0s;
step 3: opening the valve BI, closing the valve BII, opening the valve BIII, closing the valve BIV, and keeping other valves in a default state to dilute the H by inert carrier gas 2 O 2 Steam is injected into the reaction chamber through the gas distributor, and the injection time is 10.0s;
step 4: opening valve AIII, closing valve AIV, opening valve BIII, closing valve BIV, keeping other valves in default state, injecting inert carrier gas into the reaction cavity to clean physical adsorption and byproducts and the like on the surface of the silicon wafer, wherein the injection time of the inert carrier gas is 20.0s;
repeating the steps 1-4 for 300 times, and depositing TiO with the required thickness on the surface of the silicon wafer 2 A target film.
Example 5:
the present example shows a pulsed CVD TiO 2 Apparatus and method for uniform thin film vapor deposition, the apparatus used in the examples is shown in FIG. 1. The prepared film is TiO 2 The two precursors used were respectively Ti (OC 3 H 7 ) 4 And H 2 O 2 The material is respectively arranged in a storage tank A and a storage tank B, the storage tank A is heated to 60 ℃, the storage tank B is at room temperature, and the flow rates of mass flow meters of bypass inert carrier gas purging main pipelines of the two storage tanks are both set to be 40sccm. The substrate material is silicon wafer, the inert carrier gas is Ar, and the atomic layer deposition experiment temperature is 150 ℃. All odd valves are set to be in a closed state before being triggered by a program, and all even valves are set to be in an open state before being triggered.
The method specifically comprises the following steps:
step 1: opening valve AI, closing valve AII, opening valve BI, closing valve BII, opening valve AIII, closing valve AIV, opening valve BIII, closing valve BIV, diluting Ti (OC) with inert carrier gas 3 H 7 ) 4 Steam and H 2 O 2 Steam is injected into the reaction chamber through the gas distributor at the same time, and the injection time is 2000.0s;
step 2: opening valve AIII, closing valve AIV, opening valve BIII, closing valve BIV, keeping other valves in default state, injecting inert carrier gas into the reaction cavity to clean physical adsorption and byproducts and the like on the surface of the silicon wafer, wherein the injection time of the inert carrier gas is 300.0s;
and (3) depositing a target film with a required thickness on the surface of the silicon wafer, and changing the continuous injection time of the two precursors in the step (1) according to the requirement on the film thickness.
Example 6:
the present embodiment givesAn apparatus and method for pulsed ALD+CVD TiO2 uniform thin film rapid vapor deposition is shown in FIG. 1. The prepared film is TiO 2 The two precursors used were respectively Ti (OC 3 H 7 ) 4 And H 2 O 2 The material is respectively arranged in a storage tank A and a storage tank B, the storage tank A is heated to 60 ℃, the storage tank B is at room temperature, and the flow rates of mass flow meters of bypass inert carrier gas purging main pipelines of the two storage tanks are both set to be 40sccm. The substrate material is silicon wafer, the inert carrier gas is Ar, and the atomic layer deposition experiment temperature is 150 ℃. All odd valves are set to be in a closed state before being triggered by a program, and all even valves are set to be in an open state before being triggered.
The method specifically comprises the following steps:
step 1: opening valve AI, closing valve AII, opening valve AIII, closing valve AIV, keeping other valves in default state, diluting Zn (C) with inert carrier gas 2 H 5 ) 2 Steam is injected into the reaction chamber through the gas distributor, and the injection time is 10.0s; wherein Zn (C 2 H 5 ) 2 When the duration of the steam pulse injection into the reaction chamber reaches 5.0s, opening the valve BI, closing the valve BII, opening the valve BIII, closing the valve BIV, and diluting the Ti (OC) diluted by the inert carrier gas 3 H 7 ) 4 Steam and H 2 O 2 Steam is injected into the reaction chamber through the gas distributor at the same time, and the injection time is 5.0s;
step 2: opening the valve BI, closing the valve BII, opening the valve BIII, closing the valve BIV, and keeping other valves in a default state to dilute the H by inert carrier gas 2 O 2 Steam is injected into the reaction chamber through the gas distributor, and the injection time is 10.0s;
step 3: opening valve AIII, closing valve AIV, opening valve BIII, closing valve BIV, keeping other valves in default state, injecting inert carrier gas into the reaction cavity to clean physical adsorption and byproducts and the like on the surface of the silicon wafer, wherein the injection time of the inert carrier gas is 20.0s;
repeating the steps 1-3 for 200 times, and depositing a target film with the required thickness on the surface of the silicon wafer.

Claims (4)

1. The pulse type uniform film rapid vapor deposition method is characterized by being realized by a pulse type uniform film rapid vapor deposition device, wherein the device comprises a reaction chamber (100), a sampling part arranged at one end of the reaction chamber and a plurality of precursor vapor injection units arranged at the other end of the reaction chamber;
the precursor vapor injection unit includes: the precursor vapor pipeline and the inert carrier gas pipeline are converged into a main pipeline and then extend into the reaction chamber, a vacuum evacuation branch communicated with the precursor vapor pipeline, an inert carrier gas evacuation branch communicated with the inert carrier gas pipeline, a gas distributor positioned in the reaction chamber and connected with the end part of the main pipeline, a flow controller arranged on the inert carrier gas pipeline, valves arranged on the pipelines and the branches and a storage tank connected with the precursor vapor pipeline;
the gas distributor is provided with a plurality of gas outlet holes, and the gas distributor is communicated with the main pipeline through a metal pipeline; the gas distributor is arranged close to the sample (500) to be treated; after entering the gas distributor, the precursor steam is uniformly distributed on the surface of a sample (500) to be treated through a plurality of gas outlet holes;
the reaction chamber (100), the main pipeline, the precursor steam pipeline and the storage tank are all sleeved with heating sleeves (400);
the sampling part comprises a four-way joint, a first interface of the four-way joint is communicated with the reaction chamber in a sealing way, a second interface of the four-way joint is connected with a vacuum pump II (601) and is provided with a manual angle valve (602), a third interface of the four-way joint is a sample taking and delivering port (603), and a fourth interface of the four-way joint is provided with a vacuum degree sensor (604);
the precursor vapor injection units are respectively an A precursor vapor injection unit and a B precursor vapor injection unit;
the a-precursor vapor injection unit includes: a precursor vapor pipeline A (201) and an inert carrier gas pipeline A (202) are converged into a main pipeline A (203) and then extend into the reaction chamber (100), a branch vacuum evacuation branch A (204) arranged on the precursor vapor pipeline A (201), a branch inert carrier gas evacuation branch A (205) arranged on the inert carrier gas pipeline A (202), a storage tank A (206) connected on the precursor vapor pipeline A (201), a gas distributor A (207) positioned in the reaction chamber (100) and connected to the end part of the main pipeline A (203), a flow controller A (208) arranged on the inert carrier gas pipeline A (202), a valve AI (209) arranged on the precursor vapor pipeline A (201), a valve AIII (211) arranged on the inert carrier gas pipeline A (202), a valve AII (210) arranged on the vacuum evacuation branch A (204) and a valve AIV (212) arranged on the inert carrier gas evacuation branch A (205); and valve AI (209) is located between reservoir a (206) and valve AII (210), inert carrier gas evacuation branch a (205) is located between valve AIII (211) and flow controller a (208);
the B precursor vapor injection unit includes: the precursor vapor pipeline B (301) and the inert carrier gas pipeline B (302) are converged into a main pipeline B (303) and then extend into the reaction chamber (100), a branch vacuum evacuation branch B (304) arranged on the precursor vapor pipeline B (301), a branch inert carrier gas evacuation branch B (305) arranged on the inert carrier gas pipeline B (302), a storage tank B (306) connected on the precursor vapor pipeline B (301), a gas distributor B (307) positioned in the reaction chamber (100) and connected at the end part of the main pipeline B (303), a flow controller B (308) arranged on the inert carrier gas pipeline B (302), a valve BI (309) arranged on the precursor vapor pipeline B (301), a valve BIII (311) arranged on the inert carrier gas pipeline B (302), a valve BII (310) arranged on the vacuum evacuation branch B (304) and a valve BIV (312) arranged on the inert carrier gas evacuation branch B (305); and valve BI (309) is located between tank B (306) and valve BII (310), inert carrier gas evacuation branch B (305) is located between valve BIII (311) and flow controller B (308);
the method realizes continuous pulse injection of each precursor vapor into the reaction chamber or intermittent pulse injection of the precursor vapor into the reaction chamber by controlling the valve switch on each precursor vapor pipeline and the vacuum evacuation branch;
the injection time sequence of different precursor steam pulses is realized by controlling the switching time length of each valve on each precursor steam pipeline and each valve on the inert gas carrying pipeline;
by controlling the injection mode and injection time sequence of each precursor vapor, an ALD thin film deposition mode, a CVD thin film deposition mode and an ALD+CVD thin film deposition mode can be realized; and the concentration of each precursor vapor can be diluted and adjusted before being injected into the reaction chamber;
the ALD+CVD film deposition mode in the method is different precursor vapor injection modes and has the precursor vapor injection modes in the ALD film deposition mode and the CVD film deposition mode, different precursor vapor pulse injection sequences are partially overlapped, and the rapid vapor deposition of the uniform film is realized, and the method specifically comprises the following steps:
step 1: opening a valve AI, and injecting precursor vapor A into the reaction chamber for a period of time of t7+t8; when the duration of pulse injection of the precursor vapor A into the reaction chamber reaches t7, opening a valve BI, and injecting the precursor vapor B into the reaction chamber, wherein the duration of injection is t8;
step 2: closing the valve AI, keeping the valve BI in an open state, and continuously injecting the precursor steam pulse B into the reaction chamber for the injection time period of t9;
step 3: opening a valve AIII and a valve BIII to inject inert carrier gas to blow precursor molecules which do not participate in the reaction out of the reaction chamber, wherein the injection time is t10;
and (3) repeatedly executing the steps 1-3, and depositing a target film with a required thickness on the surface of the sample to be treated.
2. The method for rapid vapor deposition of pulsed uniform films of claim 1, wherein the ALD film deposition mode of the method is to alternately inject each reaction precursor vapor pulse into a reaction chamber, and the different reaction precursor vapor pulse injections are interspersed with inert carrier gas purging processes to obtain a target film with precisely controllable thickness on the surface of the sample to be processed; the method specifically comprises the following steps:
step 1: opening a valve AI, and injecting precursor vapor A into the reaction chamber for a period of time t1;
step 2: closing the valve AI, opening the valve AIII, injecting inert carrier gas to blow unadsorbed A precursor molecules physically adsorbed on the surface of the sample to be processed and byproducts generated by surface chemical reaction out of the reaction chamber, wherein the injection time of the inert carrier gas is t2;
step 3: opening a valve BI, and injecting precursor steam B into the reaction chamber for a period of time t3;
step 4: closing a valve BI, opening the valve BIII, injecting inert carrier gas to blow unadsorbed B precursor molecules physically adsorbed on the surface of the sample to be processed and byproducts generated by surface chemical reaction out of the reaction chamber, wherein the injection time of the inert carrier gas is t4;
and (3) repeatedly executing the steps 1-4, and depositing a target film with a required thickness on the surface of the sample to be treated.
3. The method of claim 1, wherein the CVD film deposition mode is to inject each reaction precursor vapor pulse into the reaction chamber simultaneously, and each reaction precursor vapor chemically reacts in the gas phase to form a target product and deposits the target product on the surface of the sample to be processed to form a target film; the method specifically comprises the following steps:
step 1: simultaneously opening a valve AI and a valve BI, and synchronously injecting precursor vapor A and precursor vapor B into the reaction chamber, wherein the injection duration is t5;
step 2: after the target film grows rapidly on the surface of the sample to be treated and reaches the required target thickness, simultaneously closing the valve AI and the valve BI, opening the valve AIII and the valve BIII, injecting inert carrier gas to blow precursor molecules which do not participate in the reaction out of the reaction chamber, and injecting the precursor molecules for a period of time of t6.
4. The pulsed, uniform, thin film rapid vapor deposition method of claim 1, wherein the vacuum evacuation branch a (204) and the vacuum evacuation branch B (304) are both connected to a vacuum pump I (701);
the controllable gas flow rate of the flow controller A (208) and the flow controller B (308) is 0-500sccm; the switching time of each valve is 0-10000s.
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