CN109306465B - To Cu3Method for realizing quantitative doping of N film - Google Patents

To Cu3Method for realizing quantitative doping of N film Download PDF

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CN109306465B
CN109306465B CN201811365374.8A CN201811365374A CN109306465B CN 109306465 B CN109306465 B CN 109306465B CN 201811365374 A CN201811365374 A CN 201811365374A CN 109306465 B CN109306465 B CN 109306465B
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power
flow
started
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CN109306465A (en
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杜允
俞优姝
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School of Information Engineering of Hangzhou Dianzi University
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C23C14/0042—Controlling partial pressure or flow rate of reactive or inert gases with feedback of measurements
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process

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Abstract

The invention discloses aFor Cu3A method for realizing quantitative doping of an N film. The vacuum cavity is internally provided with a sample table, a heating wire, a substrate and a target, wherein the sample table is arranged at the bottom in the vacuum cavity, the upper surface of the sample table is provided with the heating wire, and the heating wire is provided with the substrate; the target is arranged at the top in the vacuum cavity; a magnet is arranged above the target, and a cooling water system is arranged above the magnet and used for cooling the magnet; one end of the matching box is connected with a cooling water system, and the other end of the matching box is connected with a radio frequency source; the gas cylinder is connected with the vacuum cavity through a gas pipe, and the gas pipe is provided with a flow controller, a rough vacuum gauge and a vent valve; the mechanical pump is connected with one end of the molecular pump, and the other end of the molecular pump is connected with the vacuum cavity through a flange; the outer wall of the vacuum cavity is provided with a cold cathode gauge. The invention can observe the air pressure of the air pipe in real time during breath holding, can control the starting air pressure, has small damage to the molecular pump, saves cost and can realize the starting of gases such as nitrogen and the like which are difficult to start.

Description

To Cu3Method for realizing quantitative doping of N film
The application is a divisional application, and the original application specific information is as follows:
application date: year 2017, month 1, day 25;
application No.: 201710060592X;
the invention name is as follows: an apparatus for generating a pure nitrogen plasma and a method of using the same;
Technical Field
The invention belongs to the field of semiconductor film preparation, and particularly relates to a Cu-doped copper alloy3A method for realizing quantitative doping of an N film.
Background
Magnetron sputtering methods are common methods for preparing nitride and oxide films. Usually with a metal target, argon and a reactive gas such as nitrogen or oxygen are added. When the metal target particles collide with the substrate, they combine with the reactive gas to form a nitride or an oxide due to energy conversion.
However, for Cu3N and other noble metal nitrides, Cu and other noble metals have very weak chemical bonds with N, and if argon is introduced as a reaction gas during the preparation of the magnetron sputtering method, the nitrogen is easy to damageThe formed noble metal such as Cu-N bond is bonded with N, so that the nitride film with non-ideal chemical ratio is easily formed. Therefore, it is desired to prepare stoichiometric Cu3And N and the like, and pure nitrogen is required as a working gas. However, pure nitrogen is difficult to ignite and to generate a pure nitrogen plasma.
Theoretically, the increase of the air pressure is beneficial to the ignition of the N2, but in the actual operation process, the air pressure is too large and easily exceeds the working range of the molecular pump, thereby damaging the molecular pump. In addition, different gases are difficult to ignite, inert gases such as Ar gas are easy to ignite, N2 is difficult to ignite, and how to ignite nitrogen gas on the premise of not damaging a molecular pump is a very skillful and challenging matter.
Disclosure of Invention
The invention aims to solve the problem of luminance starting and provides a method for preparing Cu3A method for realizing quantitative doping of an N film.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention comprises a vacuum cavity, a sample stage, a heating wire, a substrate, a target, a cooling water system, a matching box, a radio frequency source, a cold cathode gauge, a molecular pump, a mechanical pump, a gas cylinder, a flow controller, a vent valve and a rough vacuum gauge. The vacuum chamber is internally provided with a sample table, a heating wire, a substrate and a target, the sample table is arranged at the bottom in the vacuum chamber, the upper surface of the sample table is provided with the heating wire, and the heating wire is provided with the substrate; the target is arranged at the top in the vacuum cavity; a magnet is arranged above the target, and a cooling water system is arranged above the magnet and used for cooling the magnet; one end of the matching box is connected with a cooling water system, and the other end of the matching box is connected with a radio frequency source; the gas bottle is connected with the vacuum cavity through a gas pipe, the gas pipe is provided with a flow controller, a rough vacuum gauge and a vent valve, the flow controller is used for controlling the gas flow, the rough vacuum gauge is used for measuring the gas pressure of the gas pipe during gas holding, and the vent valve is used for regulating the inflow of gas to the vacuum cavity and the working gas pressure; the mechanical pump is connected with one end of the molecular pump, and the other end of the molecular pump is connected with the vacuum cavity through a flange; the outer wall of the vacuum cavity is provided with a cold cathode gauge.
To Cu3A using method of a device for carrying out quantitative doping on an N film specifically comprises the following steps:
step 1, the substrate is placed on a sample holder.
And 2, adjusting the target distance, putting a baffle plate and closing the cavity door.
Step 3, vacuumizing, wherein when the background air pressure in the vacuum cavity reaches 10－6And when the mbar magnitude is greater, turning on a power switch of the flowmeter, and turning on a radio frequency power switch.
And 4, opening a nitrogen vent valve, and adjusting the flow of the nitrogen to the working flow.
And 5, adjusting the power to the working power and loading the power.
And 6, observing the vacuum cavity and observing whether the nitrogen is bright or not.
And 7, if the glow is started in the step 6, carrying out pre-sputtering and then carrying out thin film deposition.
And 8, if the glow is not started in the step 6, increasing the power and observing whether the glow is started or not.
And 9, if the glow is started in the step 8, reducing the power to the working power, and performing the step 7.
And 10, if the glow is not started in the step 8, unloading the power, increasing the nitrogen flow, reloading the power and observing whether the glow is started or not.
And 11, if the glow is started in the step 10, reducing the nitrogen flow to the working flow, reducing the power to the working power, and performing the step 7.
And 12, if the step 10 does not start, unloading the power. And reducing the nitrogen flow to the working flow, closing the nitrogen vent valve, holding the gas for 2-3min, adjusting the power to the working power, loading the power, opening the nitrogen vent valve, and observing whether the light is started.
And step 13, if the step 12 is started, performing the step 7.
And 14, if the glow is not started in the step 12, unloading the power, closing the nitrogen vent valve, holding the gas for 2-3min, increasing the power, loading the power, opening the nitrogen vent valve, and observing whether the glow is started or not.
And 15, if the step 14 is started, performing the step 7.
To Cu3Another method for using the device for quantitatively doping the N film specifically comprises the following steps:
step 1, the substrate is placed on a sample holder.
And 2, adjusting the target distance, putting a baffle plate and closing the cavity door.
Step 3, vacuumizing, wherein when the background air pressure in the vacuum cavity reaches 10－6And when the mbar magnitude is greater, turning on a power switch of the flowmeter, and turning on a radio frequency power switch.
And 4, opening a nitrogen vent valve, and adjusting the flow of the nitrogen to the working flow.
And 5, adjusting the power to the working power and loading the power.
And 6, observing the vacuum cavity and observing whether the nitrogen is bright or not.
And 7, if the glow is started in the step 6, carrying out pre-sputtering and then carrying out thin film deposition.
And 8, if the glow is not started in the step 6, increasing the power and observing whether the glow is started or not.
And 9, if the glow is started in the step 8, reducing the power to the working power, and performing the step 7.
And 10, if the glow is not started in the step 8, unloading the power, increasing the nitrogen flow, reloading the power and observing whether the glow is started or not.
And 11, if the glow is started in the step 10, reducing the nitrogen flow to the working flow, reducing the power to the working power, and performing the step 7.
And 12, if the step 10 does not start, unloading the power. And reducing the nitrogen flow to the working flow, closing the nitrogen vent valve, holding the gas for 2-3min, adjusting the power to the working power, loading the power, opening the nitrogen vent valve, and observing whether the light is started.
And step 13, if the step 12 is started, performing the step 7.
And 14, if the glow is not started in the step 12, unloading the power, closing the nitrogen vent valve, holding the gas for 2-3min, increasing the power, loading the power, opening the nitrogen vent valve, and observing whether the glow is started or not.
And 15, if the step 14 is started, performing the step 7.
And step 16, if the glow is not generated in the step 14, opening the baffle, changing the environment in the vacuum cavity, observing whether the glow is generated, reducing the power to the working power after the glow is generated, adding the baffle, rotating the sample table to the next position, and performing pre-sputtering and film deposition.
To Cu3Another method for using the device for quantitatively doping the N thin film specifically comprises the following steps:
step 1, the substrate is placed on a sample holder.
And 2, adjusting the target distance, putting a baffle plate and closing the cavity door.
Step 3, vacuumizing, wherein when the background air pressure in the vacuum cavity reaches 10－6And when the mbar magnitude is greater, turning on a power switch of the flowmeter, and turning on a radio frequency power switch.
And 4, opening a vent valve, and adjusting the flow of the nitrogen to the working flow.
And 5, adjusting the power to the working power and loading the power.
And 6, observing the vacuum cavity and observing whether the nitrogen is bright or not.
And 7, if the glow is started in the step 6, adjusting the air release valve, adjusting the working air pressure, carrying out pre-sputtering, and then carrying out thin film deposition.
And 8, if the glow is not started in the step 6, increasing the power and observing whether the glow is started or not.
And 9, if the glow is started in the step 8, reducing the power to the working power, and performing the step 7.
And 10, if the glow is not started in the step 8, unloading the power, increasing the nitrogen flow, reloading the power and observing whether the glow is started or not.
And 11, if the glow is started in the step 10, reducing the nitrogen flow to the working flow, reducing the power to the working power, and performing the step 7.
And 12, if the step 10 does not start, unloading the power. And reducing the nitrogen flow to the working flow, closing the vent valve, holding the air for 2-3min, adjusting the power to the working power, loading the power, opening the vent valve, and observing whether the light is started.
And step 13, if the step 12 is started, performing the step 7.
And step 14, if the glow is not started in the step 12, unloading the power, closing the vent valve, holding the gas for 2-3min, increasing the power, loading the power, opening the nitrogen vent valve, and observing whether the glow is started or not.
And 15, if the step 14 is started, performing the step 7.
And step 16, if the glow is not started in the step 14, unloading the power, reducing the flow of the nitrogen to be half of the working flow, increasing the flow of the argon to be half of the working flow, closing the vent valve, holding the gas for 2-3min, adjusting the power to be the working power, loading the power, opening the vent valve, and observing whether the glow is started or not.
And 17, if glow is started in the step 16, after glow is started, on the premise of keeping the total flow unchanged, gradually increasing the nitrogen flow and simultaneously reducing the argon flow until the nitrogen flow is increased to the working flow and the argon flow is reduced to 0, and then performing the step 7.
And 18, if the light does not start in the step 16, unloading the power, closing the vent valve, holding the gas for 2-3min, increasing the power, loading the power, opening the vent valve, observing whether the light starts, after the light starts, gradually increasing the nitrogen flow and simultaneously reducing the argon flow on the premise of keeping the total flow unchanged until the nitrogen flow is increased to the working flow and the argon flow is reduced to 0, and performing the step 7.
The working process of the invention is as follows:
firstly, placing a copper target and a substrate in a vacuum cavity, placing a baffle, closing a cavity door, and vacuumizing. When the vacuum reaches 10－6And when the mbar magnitude is reached, turning on a power switch of the flowmeter for preheating, and turning on a radio frequency power switch for preheating. And opening a vent valve, and adjusting the flow of the nitrogen to the working flow. Closing the vent valve, holding the air for a period of time, observing the reading of the rough vacuum gauge on the air pipe, setting working power and loading power when a certain numerical value is reached, opening the vent valve, and starting the light. After glow starting, adjusting the air release valve to working air pressure, carrying out pre-sputtering, and then carrying out thin film deposition.
The invention has the following beneficial effects:
compared with the prior art, the method is simple, the vacuum degree in the trachea can be observed in real time when the trachea is suffocated, and the glow starting air pressure in the vacuum cavity at the moment when the corresponding vent valve is opened can be obtained through conversion, so that the suffocated time is conveniently controlled, the glow starting air pressure is conveniently controlled, repeated experiments are convenient, the lowest glow starting air pressure is conveniently explored and adopted, and the damage of the atmospheric glow starting air pressure to the molecular pump can be avoided.
Drawings
FIG. 1 is a block diagram of the present invention.
Detailed Description
The invention will be further explained with reference to the drawings.
As shown in FIG. 1, a pair of Cu3The device for quantitatively doping the N film comprises a vacuum cavity 1, a sample table 2, a heating wire 3, a substrate, a target 4, a cooling water system 5, a matching box 6, a radio frequency source 7, a cold cathode gauge 8, a molecular pump 9, a mechanical pump 10, a gas cylinder, a flow controller 11, a rough vacuum gauge 13 and a vent valve 12.
A sample table 2, a heating wire 3, a substrate and a target 4 are arranged in the vacuum cavity 1, the sample table 2 is arranged at the bottom in the vacuum cavity 1, the heating wire 3 is arranged on the lower surface of the sample table 2, and the substrate is arranged on the sample table 2; the target 4 is arranged at the top in the vacuum chamber 1; a magnet is arranged above the target 4, a cooling water system 5 is arranged above the magnet, and the cooling water system 5 is used for cooling the magnet; one end of the matching box 6 is connected with the cooling water system 5, and the other end is connected with the radio frequency source 7; the gas bottle is connected with the vacuum cavity 1 through a gas pipe, a flow controller 11, a vent valve 12 and a rough vacuum gauge 13 are sequentially arranged on the gas pipe between the gas bottle and the vacuum cavity 1, the flow controller 11 is used for controlling the gas flow, the rough vacuum gauge 13 is used for measuring the gas pressure in the pipe during gas holding, and the vent valve 12 is used for adjusting the inflow of gas to the vacuum cavity and the working gas pressure; the mechanical pump 10 is connected with one end of the molecular pump 9, and the other end of the molecular pump 9 is connected with the vacuum cavity 1 through a flange; the outer wall of the vacuum chamber 1 is provided with a cold cathode gauge 8.
To Cu3A using method of a device for carrying out quantitative doping on an N film specifically comprises the following steps:
step 1, the substrate is placed on a sample holder.
And 2, adjusting the target distance, putting a baffle plate and closing the cavity door.
Step 3, vacuumizing, wherein when the background air pressure in the vacuum cavity reaches 10－6When mbar magnitude is reached, a power switch of the flowmeter is turned onAnd turning on a radio frequency power switch.
And 4, opening a nitrogen vent valve, and adjusting the flow of the nitrogen to the working flow.
And 5, adjusting the power to the working power and loading the power.
And 6, observing the vacuum cavity and observing whether the nitrogen is bright or not.
And 7, if the glow is started in the step 6, carrying out pre-sputtering and then carrying out thin film deposition.
And 8, if the glow is not started in the step 6, increasing the power and observing whether the glow is started or not.
And 9, if the glow is started in the step 8, reducing the power to the working power, and performing the step 7.
And 10, if the glow is not started in the step 8, unloading the power, increasing the nitrogen flow, reloading the power and observing whether the glow is started or not.
And 11, if the glow is started in the step 10, reducing the nitrogen flow to the working flow, reducing the power to the working power, and performing the step 7.
And 12, if the step 10 does not start, unloading the power. And reducing the nitrogen flow to the working flow, closing the nitrogen vent valve, holding the gas for 2-3min, adjusting the power to the working power, loading the power, opening the nitrogen vent valve, and observing whether the light is started.
And step 13, if the step 12 is started, performing the step 7.
And 14, if the glow is not started in the step 12, unloading the power, closing the nitrogen vent valve, holding the gas for 2-3min, increasing the power, loading the power, opening the nitrogen vent valve, and observing whether the glow is started or not.
And 15, if the step 14 is started, performing the step 7.
To Cu3Another method for using the device for quantitatively doping the N film specifically comprises the following steps:
step 1, the substrate is placed on a sample holder.
And 2, adjusting the target distance, putting a baffle plate and closing the cavity door.
Step 3, vacuumizing, wherein when the background air pressure in the vacuum cavity reaches 10－6And when the mbar magnitude is greater, turning on a power switch of the flowmeter, and turning on a radio frequency power switch.
And 4, opening a nitrogen vent valve, and adjusting the flow of the nitrogen to the working flow.
And 5, adjusting the power to the working power and loading the power.
And 6, observing the vacuum cavity and observing whether the nitrogen is bright or not.
And 7, if the glow is started in the step 6, carrying out pre-sputtering and then carrying out thin film deposition.
And 8, if the glow is not started in the step 6, increasing the power and observing whether the glow is started or not.
And 9, if the glow is started in the step 8, reducing the power to the working power, and performing the step 7.
And 10, if the glow is not started in the step 8, unloading the power, increasing the nitrogen flow, reloading the power and observing whether the glow is started or not.
And 11, if the glow is started in the step 10, reducing the nitrogen flow to the working flow, reducing the power to the working power, and performing the step 7.
And 12, if the step 10 does not start, unloading the power. And reducing the nitrogen flow to the working flow, closing the nitrogen vent valve, holding the gas for 2-3min, adjusting the power to the working power, loading the power, opening the nitrogen vent valve, and observing whether the light is started.
And step 13, if the step 12 is started, performing the step 7.
And 14, if the glow is not started in the step 12, unloading the power, closing the nitrogen vent valve, holding the gas for 2-3min, increasing the power, loading the power, opening the nitrogen vent valve, and observing whether the glow is started or not.
And 15, if the step 14 is started, performing the step 7.
And step 16, if the glow is not generated in the step 14, opening the baffle, changing the environment in the vacuum cavity, observing whether the glow is generated, reducing the power to the working power after the glow is generated, adding the baffle, rotating the sample table to the next position, and performing pre-sputtering and film deposition.
To Cu3Another method for using the device for quantitatively doping the N thin film specifically comprises the following steps:
step 1, the substrate is placed on a sample holder.
And 2, adjusting the target distance, putting a baffle plate and closing the cavity door.
Step 3, vacuumizing, wherein when the background air pressure in the vacuum cavity reaches 10－6And when the mbar magnitude is greater, turning on a power switch of the flowmeter, and turning on a radio frequency power switch.
And 4, opening a vent valve, and adjusting the flow of the nitrogen to the working flow.
And 5, adjusting the power to the working power and loading the power.
And 6, observing the vacuum cavity and observing whether the nitrogen is bright or not.
And 7, if the glow is started in the step 6, adjusting the air release valve, adjusting the working air pressure, carrying out pre-sputtering, and then carrying out thin film deposition.
And 8, if the glow is not started in the step 6, increasing the power and observing whether the glow is started or not.
And 9, if the glow is started in the step 8, reducing the power to the working power, and performing the step 7.
And 10, if the glow is not started in the step 8, unloading the power, increasing the nitrogen flow, reloading the power and observing whether the glow is started or not.
And 11, if the glow is started in the step 10, reducing the nitrogen flow to the working flow, reducing the power to the working power, and performing the step 7.
And 12, if the step 10 does not start, unloading the power. And reducing the nitrogen flow to the working flow, closing the vent valve, holding the air for 2-3min, adjusting the power to the working power, loading the power, opening the vent valve, and observing whether the light is started.
And step 13, if the step 12 is started, performing the step 7.
And step 14, if the glow is not started in the step 12, unloading the power, closing the vent valve, holding the gas for 2-3min, increasing the power, loading the power, opening the nitrogen vent valve, and observing whether the glow is started or not.
And 15, if the step 14 is started, performing the step 7.
And step 16, if the glow is not started in the step 14, unloading the power, reducing the flow of the nitrogen to be half of the working flow, increasing the flow of the argon to be half of the working flow, closing the vent valve, holding the gas for 2-3min, adjusting the power to be the working power, loading the power, opening the vent valve, and observing whether the glow is started or not.
And 17, if glow is started in the step 16, after glow is started, on the premise of keeping the total flow unchanged, gradually increasing the nitrogen flow and simultaneously reducing the argon flow until the nitrogen flow is increased to the working flow and the argon flow is reduced to 0, and then performing the step 7.
And 18, if the light does not start in the step 16, unloading the power, closing the vent valve, holding the gas for 2-3min, increasing the power, loading the power, opening the vent valve, observing whether the light starts, after the light starts, gradually increasing the nitrogen flow and simultaneously reducing the argon flow on the premise of keeping the total flow unchanged until the nitrogen flow is increased to the working flow and the argon flow is reduced to 0, and performing the step 7.
Example 1:
RF magnetron co-sputtering of copper targets to deposit Cu on Si (100) substrates3And (6) N thin films. The substrate was ultrasonically cleaned with detergent, acetone, absolute alcohol and deionized water for 15 minutes in this order before use, and then placed on a sample stage parallel to and spaced 55mm from the target surface. The target material is arranged right above the substrate. When the background air pressure of the vacuum cavity is lower than 6 x 10－6Introducing 7sccm pure nitrogen (99.99%) into the chamber at mbar, controlling gas flow by flow controller, closing the vent valve, holding the gas for a period of time, and observing the gas tube when the reading of the rough vacuum gauge reaches a certain value (corresponding to the instantaneous gas pressure in the vacuum chamber of 10%－2mbar-10－1In mbar), the operating power is set at 50W, the power is loaded, the vent valve is opened and the glow is initiated. After glow starting, the air release valve is adjusted to the working air pressure (10)－3mbar-10－2mbar), pre-sputtering is performed, followed by thin film deposition.
Example 2
And preparing the cuprous nitride film on the Si (100) substrate by using a radio frequency magnetron sputtering method. The substrate for depositing the sample was first ultrasonically cleaned with detergent, acetone, absolute alcohol and deionized water in this order for 15 minutes, and then placed on a sample holder parallel to and spaced 50mm from the target surface. When the background air pressure in the vacuum cavity is lower than 6 x 10－6And when mbar exists, turning on a power switch of the flowmeter for preheating, and turning on a radio frequency power switch for preheating. The nitrogen gas is openedAnd a gas valve which injects pure nitrogen (99.99%) with the working flow of 7sccm into the vacuum cavity. And closing the nitrogen gas vent valve, keeping the gas for 2-3min, adjusting the power to 50W, loading the power, starting the light, carrying out pre-sputtering, and then carrying out thin film deposition.
Example 3
And preparing the cuprous nitride film on the Si (100) substrate by using a radio frequency magnetron sputtering method. The substrate for depositing the sample was first ultrasonically cleaned with detergent, acetone, absolute alcohol and deionized water in this order for 15 minutes, and then placed on a sample holder parallel to and spaced 50mm from the target surface. When the background air pressure in the vacuum cavity is lower than 6 x 10－6And when mbar exists, turning on a power switch of the flowmeter for preheating, and turning on a radio frequency power switch for preheating. The nitrogen vent valve was opened, and pure nitrogen (99.99%) was introduced into the vacuum chamber at a working flow of 7 sccm. Closing the nitrogen gas vent valve, keeping the gas for 2-3min, adjusting the power to the starting power of 100W, loading the power, starting the light, reducing the power to the working power of 50W, carrying out pre-sputtering, and then carrying out thin film deposition.
Example 4:
and preparing the cuprous nitride film on the Si (100) substrate by using a radio frequency magnetron sputtering method. The substrate for depositing the sample was first ultrasonically cleaned with detergent, acetone, absolute alcohol and deionized water in this order for 15 minutes, and then placed on a sample holder parallel to and spaced 50mm from the target surface. When the background air pressure in the vacuum cavity is lower than 6 x 10－6And when mbar exists, turning on a power switch of the flowmeter for preheating, and turning on a radio frequency power switch for preheating. The nitrogen vent valve was opened, and pure nitrogen (99.99%) was introduced into the vacuum chamber at a working flow of 7 sccm. Closing the nitrogen gas vent valve, keeping the gas for 2-3min, adjusting the power to 100W, loading the power, turning on the baffle, changing the environment in the vacuum chamber, turning on the light, reducing the power to 50W after the light is turned on, adding the baffle, rotating the sample table to the next position, and performing pre-sputtering and film deposition.
Example 5:
and preparing the cuprous nitride film on the Si (100) substrate by using a radio frequency magnetron sputtering method. Firstly, a substrate for depositing a sample is sequentially treated with liquid detergent, acetone and absolute alcoholAnd deionized water for 15 minutes, and then the substrate was placed on a sample holder parallel to and 50mm from the target surface. When the background air pressure in the vacuum cavity is lower than 6 x 10－6And when mbar exists, turning on a power switch of the flowmeter for preheating, and turning on a radio frequency power switch for preheating. The nitrogen vent valve was opened, and pure nitrogen (99.99%) was introduced into the vacuum chamber at a working flow of 7 sccm. And (4) closing the nitrogen vent valve, keeping the air for 2-3min, adjusting the power to 100W, loading the power and keeping the power from glowing. Unloading 100W of power, reducing the flow of nitrogen to half 3.5sccm of the working flow, opening an argon gas vent valve, increasing the flow of argon to half 3.5sccm of the working flow, closing the nitrogen and argon gas vent valves, holding the gas for 2-3min, loading 100W of power, opening the nitrogen and argon gas vent valves, starting luminance, gradually increasing the flow of nitrogen and simultaneously reducing the flow of argon gas on the premise of keeping the total flow of 7sccm unchanged, until the flow of nitrogen increases to 7sccm of the working flow, reducing the flow of argon gas to 0, and performing pre-sputtering and film deposition.

Claims (2)

1. To Cu3The method for realizing the quantitative doping of the N film is characterized by comprising the following steps of:
step 1, placing a substrate on a sample table;
step 2, adjusting the target distance, placing a baffle plate, and closing a cavity door;
step 3, vacuumizing, wherein when the background air pressure in the vacuum cavity reaches 10－6When the mbar magnitude is greater, turning on a power switch of the flowmeter, and turning on a radio frequency power switch;
step 4, opening a vent valve, and adjusting the flow of the nitrogen to the working flow;
step 5, adjusting the power to the working power and loading the power;
step 6, observing the vacuum cavity, and observing whether the nitrogen is bright or not;
step 7, if the glow is started in the step 6, adjusting an air release valve, adjusting to working air pressure, carrying out pre-sputtering, and then carrying out thin film deposition;
step 8, if the glow is not started in the step 6, increasing the power and observing whether the glow is started or not;
step 9, if the glow is started in the step 8, reducing the power to the working power, and performing the step 7;
step 10, if the glow is not started in the step 8, unloading the power, increasing the nitrogen flow, reloading the power and observing whether the glow is started or not;
step 11, if the glow is started in the step 10, reducing the nitrogen flow to the working flow, reducing the power to the working power, and performing the step 7;
step 12, if the glow is not started in the step 10, the power is unloaded; reducing the nitrogen flow to the working flow, closing a vent valve, holding the air for 2-3min, adjusting the power to the working power, loading the power, opening the vent valve, and observing whether the light is started;
step 13, if the glow is started in the step 12, performing the step 7;
step 14, if the glow is not started in the step 12, unloading the power, closing the vent valve, holding the gas for 2-3min, increasing the power, loading the power, opening the nitrogen vent valve, and observing whether the glow is started or not;
step 15, if the glow is started in the step 14, performing the step 7;
step 16, if the glow is not started in the step 14, unloading the power, reducing the flow of the nitrogen to be half of the working flow, increasing the flow of the argon to be half of the working flow, closing a vent valve, holding the gas for 2-3min, adjusting the power to be the working power, loading the power, opening the vent valve, and observing whether the glow is started or not;
step 17, if the glow is started in the step 16, after the glow is started, on the premise of keeping the total flow unchanged, gradually increasing the nitrogen flow and simultaneously reducing the argon flow until the nitrogen flow is increased to the working flow and the argon flow is reduced to 0, and performing the step 7;
and 18, if the light does not start in the step 16, unloading the power, closing the vent valve, holding the gas for 2-3min, increasing the power, loading the power, opening the vent valve, observing whether the light starts, after the light starts, gradually increasing the nitrogen flow and simultaneously reducing the argon flow on the premise of keeping the total flow unchanged until the nitrogen flow is increased to the working flow and the argon flow is reduced to 0, and performing the step 7.
2. A pair of Cu as claimed in claim 13The method for realizing the quantitative doping of the N film is characterized in that the device used by the method comprises a vacuum cavity,The device comprises a sample table, a heating wire, a substrate, a target, a cooling water system, a matching box, a radio frequency source, a cold cathode gauge, a molecular pump, a mechanical pump, a gas cylinder, a flow controller, a rough vacuum gauge and a vent valve;
the vacuum chamber is internally provided with a sample table, a heating wire, a substrate and a target, the sample table is arranged at the bottom in the vacuum chamber, the upper surface of the sample table is provided with the heating wire, and the heating wire is provided with the substrate; the target is arranged at the top in the vacuum cavity; a magnet is arranged above the target, and a cooling water system is arranged above the magnet and used for cooling the magnet; one end of the matching box is connected with a cooling water system, and the other end of the matching box is connected with a radio frequency source; the gas bottle is connected with the vacuum cavity through a gas pipe, the gas pipe is provided with a flow controller, a rough vacuum gauge and a vent valve, the flow controller is used for controlling the gas flow, the rough vacuum gauge is used for measuring the gas pressure of the gas pipe during gas holding, and the vent valve is used for regulating the inflow of gas to the vacuum cavity and the working gas pressure; the mechanical pump is connected with one end of the molecular pump, and the other end of the molecular pump is connected with the vacuum cavity through a flange; the outer wall of the vacuum cavity is provided with a cold cathode gauge.
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