CN115589562B - Preparation method of composite loudspeaker diaphragm and related equipment thereof - Google Patents

Preparation method of composite loudspeaker diaphragm and related equipment thereof Download PDF

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Publication number
CN115589562B
CN115589562B CN202211282790.8A CN202211282790A CN115589562B CN 115589562 B CN115589562 B CN 115589562B CN 202211282790 A CN202211282790 A CN 202211282790A CN 115589562 B CN115589562 B CN 115589562B
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aluminum alloy
magnesium
argon
loudspeaker diaphragm
composite
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CN115589562A (en
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孙庆磊
马晓明
陈国平
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Shenzhen 3Nod Digital Technology Co Ltd
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Shenzhen 3Nod Digital Technology Co Ltd
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    • H—ELECTRICITY
    • H04—ELECTRIC COMMUNICATION TECHNIQUE
    • H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
    • H04R9/00—Transducers of moving-coil, moving-strip, or moving-wire type
    • H04R9/06—Loudspeakers
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • 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
    • H—ELECTRICITY
    • H04—ELECTRIC COMMUNICATION TECHNIQUE
    • H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
    • H04R9/00—Transducers of moving-coil, moving-strip, or moving-wire type
    • H04R9/02—Details
    • H—ELECTRICITY
    • H04—ELECTRIC COMMUNICATION TECHNIQUE
    • H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
    • H04R2400/00—Loudspeakers
    • H04R2400/11—Aspects regarding the frame of loudspeaker transducers

Abstract

The embodiment of the application belongs to the electroacoustic field and relates to a preparation method of a composite loudspeaker diaphragm, which comprises the steps of providing a magnesium-aluminum alloy matrix; under the condition of preset cavity pressure, argon and tetramethylsilane are used as first working gases, and a substrate layer is formed on the magnesium-aluminum alloy substrate in a deposition mode; and under the condition of preset cavity pressure, taking argon, tetramethylsilane and acetylene as second working gases, and depositing a diamond-like film layer on the substrate layer to obtain the composite diaphragm. The application also relates to a related device of the composite loudspeaker diaphragm. The technical scheme that this application provided can effectively promote the tone quality of compound speaker vibrating diaphragm.

Description

Preparation method of composite loudspeaker diaphragm and related equipment thereof
Technical Field
The application relates to the electroacoustic technical field, in particular to a preparation method of a composite loudspeaker diaphragm and related equipment thereof.
Background
The sound reproduction system of the modern sound equipment is limited by the high-frequency vibrating diaphragm material, so that the high-frequency loudspeaker of the sound reproduction system is not satisfactory, and the sound reproduction system becomes an important obstacle for improving the overall performance of the high-fidelity sound equipment. Therefore, the development of a novel high-pitch loudspeaker diaphragm material and the development of a high-quality high-frequency loudspeaker become one of research directions of the domestic and foreign material world and the electroacoustic world.
The requirements on the tone quality of sound are higher and higher based on the loudspeaker box products, so new requirements are put on the expansion of the frequency spectrum width of the loudspeaker. The diamond-like film layer is an ideal diaphragm material, but the bonding strength of the traditional loudspeaker diaphragm and the diamond-like film layer is poor, so that the bending vibration amplitude of the loudspeaker diaphragm during working cannot be effectively restrained, the frequency response curve is relatively changed to be more concave-convex, and the tone quality of the composite loudspeaker diaphragm is poor.
Disclosure of Invention
The embodiment of the application provides a preparation method of a composite loudspeaker diaphragm and related equipment thereof, which are used for solving the problem of poor sound quality of the composite loudspeaker diaphragm in the prior art.
In order to solve the above technical problems, the embodiment of the present application provides a method for preparing a composite loudspeaker diaphragm, which adopts the following technical scheme:
providing a magnesium-aluminum alloy matrix;
under the condition of preset cavity pressure, argon and tetramethylsilane are used as first working gases, and a base layer is formed on the magnesium-aluminum alloy substrate in a deposition mode;
and under the condition of the preset cavity pressure, taking argon, tetramethylsilane and acetylene as second working gases, and depositing a diamond-like film layer on the substrate layer to obtain the composite diaphragm.
Further, the volume flow rate of the argon in the first working gas is 100-300 sccm;
and/or the volumetric flow rate of the tetramethylsilane in the first working gas is 10 to 40sccm;
and/or depositing a base layer on the magnesium-aluminum alloy substrate under a first pulse magnetron sputtering condition, wherein the first pulse magnetron sputtering condition comprises at least one of excitation voltage of 1200-2200V, excitation current of 50-150A, pulse width of 10-30 mu s, pulse frequency of 1000-1500 Hz, bias voltage of-300-100V and working air pressure of 0.7-2 Pa;
and/or depositing and forming a basal layer on the magnesium-aluminum alloy matrix for 5 to 30 minutes.
Further, the volume flow rate of the argon in the second working gas is 100-300 sccm;
and/or the volumetric flow rate of the tetramethylsilane in the second working gas is 10 to 40sccm;
and/or the volumetric flow rate of the acetylene in the second working gas is 100 to 300sccm;
and/or depositing a diamond-like film layer on the substrate layer under a second pulse magnetron sputtering condition, wherein the second pulse magnetron sputtering condition comprises at least one of an excitation voltage of 1000 to 2000V, an excitation current of 10 to 70A, a pulse width of 10 to 30 μs, a pulse frequency of 1000 to 1500Hz, a bias voltage of-200 to 0V and an operating pressure of 1 to 4 Pa;
and/or depositing a diamond-like film layer on the substrate layer for 5 to 30 minutes;
and/or the diamond-like film layer has a thickness of 0.9 to 1.4 μm.
Further, the step of providing a magnesium aluminum alloy substrate comprises the following steps:
providing a magnesium-aluminum alloy raw material;
and carrying out ultrasonic cleaning on the magnesium aluminum alloy raw material to obtain a magnesium aluminum alloy matrix.
Further, the step of ultrasonically cleaning the magnesium-aluminum alloy raw material comprises the following steps:
and after performing first ultrasonic cleaning treatment on the magnesium-aluminum alloy raw material for 10 to 50 minutes through an acetone solution or a sodium hydroxide solution, performing second ultrasonic cleaning treatment on the magnesium-aluminum alloy raw material subjected to the first ultrasonic cleaning treatment for 10 to 50 minutes through deionized water or absolute ethyl alcohol.
Further, before the step of using argon and tetramethylsilane as the first working gas, the method further comprises:
and forming a rough surface on the magnesium-aluminum alloy substrate by taking inert gas as third working gas under the preset cavity pressure condition.
Further, the inert gas is at least one of helium, neon, argon, krypton, xenon, radon and Og;
and/or the volume flow of the inert gas in the third working gas is 100 to 300sccm;
and/or forming a rough surface on the magnesium-aluminum alloy substrate under a third pulse magnetron sputtering condition, wherein the third pulse magnetron sputtering condition comprises at least one of excitation voltage of 1200-2200V, excitation current of 50-150A, pulse width of 10-30 mu s, pulse frequency of 1000-1500 Hz, bias voltage of-500-200V and working air pressure of 0.6-1.6 Pa;
and/or forming the rough surface on the magnesium-aluminum alloy substrate for 10 to 50 minutes.
In order to solve the technical problem, the embodiment of the application also provides a composite loudspeaker diaphragm, which adopts the following technical scheme:
is prepared by the preparation method of the composite loudspeaker diaphragm.
In order to solve the above technical problems, the embodiment of the present application further provides a speaker, which adopts the following technical scheme:
the composite loudspeaker diaphragm prepared by the preparation method of the composite loudspeaker diaphragm or the composite loudspeaker diaphragm.
In order to solve the above technical problems, the embodiment of the present application further provides an electronic device, which adopts the following technical scheme:
including the speaker as described above.
Compared with the prior art, the embodiment of the application has the following main beneficial effects: according to the method, argon and tetramethylsilane are used as first working gases, the surface oxide film of the magnesium aluminum alloy substrate is removed through the argon, the substrate layer is deposited on the magnesium aluminum alloy substrate through the tetramethylsilane, so that the internal stress of the magnesium aluminum alloy substrate and the diamond-like carbon film layer in the follow-up process is effectively reduced, then argon, tetramethylsilane and acetylene are used as second working gases, the surface oxide film of the magnesium aluminum alloy substrate is further removed through the argon, the bonding force between the substrate layer formed by the deposition of the tetramethylsilane on the magnesium aluminum alloy substrate and the magnesium aluminum alloy substrate is further improved, and meanwhile, the diamond-like carbon film layer is formed on the substrate layer through the cooperation of the acetylene, so that the composite diaphragm is obtained, the film base bonding force between the magnesium aluminum alloy substrate and the diamond-like carbon film layer can be effectively improved, the prepared composite diaphragm is further improved to have higher elastic modulus and Vickers hardness, the bending vibration amplitude of the loudspeaker diaphragm is restrained in working, the frequency response curve is relatively flat, the replay frequency band is widened, and the tone quality of the loudspeaker diaphragm is effectively improved.
Drawings
For a clearer description of the solution of the present application, a brief introduction will be given to the drawings needed in the description of the embodiments, which are some embodiments of the present application, and from which other drawings can be obtained for a person skilled in the art without the inventive effort.
Fig. 1 is a flow chart of a method of making a composite loudspeaker diaphragm of the present application.
FIG. 2 is a Raman spectrum of example 2-1 of the preparation method of the composite loudspeaker diaphragm;
FIG. 3 is a Raman spectrum of comparative example 1-1;
FIG. 4 is a graph comparing frequency response curves of example 2-2, comparative example 1-2, and comparative example 2-1 in the preparation method of the composite loudspeaker diaphragm of the present application.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; the terminology used in the description of the applications herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application; the terms "comprising" and "having" and any variations thereof in the description and claims of the present application and in the description of the figures above are intended to cover non-exclusive inclusions. The terms first, second and the like in the description and in the claims or in the above-described figures, are used for distinguishing between different objects and not necessarily for describing a sequential or chronological order.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment may be included in at least one embodiment of the present application. The appearances of such phrases in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Those of skill in the art will explicitly and implicitly appreciate that the embodiments described herein may be combined with other embodiments.
Referring to fig. 1, the present application provides a method for preparing a composite loudspeaker diaphragm, including:
step S101, providing a magnesium-aluminum alloy matrix.
In this embodiment, the magnesium-aluminum alloy substrate has the characteristics of low density, good specific elasticity, good rigidity and excellent ductility, and in the formed diaphragm, the magnesium-aluminum alloy substrate has excellent rigidity under the condition of ensuring the light and thin state, and the magnesium-aluminum alloy substrate is prepared to form the diaphragm relative to the aluminum alloy substrate or the diaphragm prepared from the traditional paper diaphragm material.
And S102, under the condition of preset cavity pressure, taking argon and tetramethylsilane as first working gases, and depositing and forming a substrate layer on the magnesium-aluminum alloy substrate.
In this embodiment, the argon is used to remove the oxide film on the magnesium-aluminum alloy substrate, and the tetramethylsilane is used to provide silicon atoms, so that a silicon transition layer is formed on the surface of the magnesium-aluminum alloy substrate, and is used as a substrate layer, so that the internal stress of the magnesium-aluminum alloy substrate when being combined with the diamond-like film layer can be effectively reduced, and the bonding strength of the film substrate can be further improved.
And step 103, under the preset cavity pressure condition, taking argon, tetramethylsilane and acetylene as second working gases, and depositing a diamond-like film layer on the substrate layer to obtain the composite diaphragm.
In this example, diamond-like film (DLC) is an amorphous carbon film containing a Diamond structure, having properties similar to Diamond: low specific gravity, high elastic modulus, high sound velocity and good thermal conductivity; therefore, the diamond-like film layer is formed on the basal layer by deposition, so that the vibrating diaphragm formed by compounding the magnesium aluminum alloy and the diamond-like film layer has higher upper limit of frequency response, improves transient response and harmonic distortion characteristics, has wide range, mellow and moist tone quality, is crisp and bright in high tone, and effectively improves hearing.
According to the method, argon and tetramethylsilane are used as first working gases, the surface oxide film of the magnesium aluminum alloy substrate is removed through the argon, the substrate layer is deposited on the magnesium aluminum alloy substrate through the tetramethylsilane, so that the internal stress of the magnesium aluminum alloy substrate and the diamond-like carbon film layer in the follow-up process is effectively reduced, then argon, tetramethylsilane and acetylene are used as second working gases, the surface oxide film of the magnesium aluminum alloy substrate is further removed through the argon, the bonding force between the substrate layer formed by the deposition of the tetramethylsilane on the magnesium aluminum alloy substrate and the magnesium aluminum alloy substrate is further improved, and meanwhile, the diamond-like carbon film layer is formed on the substrate layer through the cooperation of the acetylene, so that the composite diaphragm is obtained, the film base bonding force between the magnesium aluminum alloy substrate and the diamond-like carbon film layer can be effectively improved, the prepared composite diaphragm is further improved to have higher elastic modulus and Vickers hardness, the bending vibration amplitude of the loudspeaker diaphragm is restrained in working, the frequency response curve is relatively flat, the replay frequency band is widened, and the tone quality of the loudspeaker diaphragm is effectively improved.
In some embodiments, the present application deposits a base layer on a magnesium aluminum alloy substrate by magnetron sputtering, wherein the pre-chamber pressure conditions are 1×10 -4 Up to 1X 10 -2 The deposition of the basal layer is carried out under vacuum condition, so that enough gas ions in the first working gas/the second working gas bombard the target material through electric energy in the magnetron sputtering process, and the gas quantity which loses too much energy because of collision of too much gas in the bombardment process is avoided.
In some embodiments, the volume flow of argon in the first working gas is 100 to 300sccm.
The volume flow rate of the argon gas in the first working gas may be selected from one or more of 100sccm, 110sccm, 120sccm, 130sccm, 140sccm, 150sccm, 160sccm, 170sccm, 180sccm, 190sccm, 200sccm, 210sccm, 220sccm, 230sccm, 240sccm, 250sccm, 260sccm, 270sccm, 280sccm, 290sccm, and 300sccm.
In this embodiment, the volume flow of argon in the first working gas is 100-300 sccm, so that the surface of the magnesium-aluminum alloy substrate is prevented from being damaged by excessive argon in the first working gas while the oxide film is removed from the magnesium-aluminum alloy substrate, and the effect of removing the oxide film on the magnesium-aluminum alloy substrate is stronger as the volume flow of argon in the first working gas is larger in the range.
In some embodiments, the volumetric flow rate of the tetramethylsilane in the first working gas is from 10 to 40sccm.
The volumetric flow rate of the tetramethylsilane in the first working gas may be selected from one or more of 10sccm, 15sccm, 20sccm, 25sccm, 30sccm, 35sccm, and 40sccm.
In this embodiment, the volume flow of the tetramethylsilane in the first working gas is 10 to 40sccm, so as to ensure the deposition effect of the silicon transition layer on the magnesium-aluminum alloy substrate in the magnetron sputtering process, thereby ensuring the bonding strength of the magnesium-aluminum alloy substrate and the diamond-like film layer, and also ensuring the structural compactness of the formed composite diaphragm.
In some embodiments, a base layer is deposited on the magnesium aluminum alloy substrate under first pulsed magnetron sputtering conditions, wherein the first pulsed magnetron sputtering conditions include at least one of an excitation voltage of 1200 to 2200V, an excitation current of 50 to 150A, a pulse width of 10 to 30 μs, a pulse frequency of 1000 to 1500Hz, a bias voltage of-300 to-100V, and an operating gas pressure of 0.7 to 2 Pa.
The excitation voltage in the first pulse magnetron sputtering condition is selected from one or two of 1200V, 1300V, 1400V, 1500V, 1600V, 1700V, 1800V, 1900V, 2000V, 2100V, 2200V.
The excitation current in the first pulsed magnetron sputtering condition is selected from a range of values between one or both of 50A, 60A, 70A, 80A, 90A, 100A, 110A, 120A, 130A, 140A, 150A.
The pulse width in the first pulse magnetron sputtering condition is selected from one or two of 10 μs, 15 μs, 20 μs, 25 μs and 30 μs.
The pulse frequency in the first pulse magnetron sputtering condition is selected from one or two of 1000Hz, 1100Hz, 1200Hz, 1300Hz, 1400Hz and 1500 Hz.
The operating air pressure in the first pulsed magnetron sputtering condition is selected from a range of values between one or two of 0.7Pa, 0.8Pa, 0.9Pa, 1Pa, 1.1Pa, 1.2Pa, 1.3Pa, 1.4Pa, 1.5Pa, 1.6Pa, 1.7Pa, 1.8Pa, 1.9Pa, 2 Pa.
The pulse plasma in the pulse magnetron sputtering is used for enhancing the chemical vapor deposition rate, has large and uniform deposition area and low cost, and is easy for industrialized mass production.
In some embodiments, the time to deposit the base layer on the magnesium aluminum alloy substrate is from 5 to 30 minutes.
The time for depositing and forming the basal layer on the magnesium-aluminum alloy matrix is selected from one or two of 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min, 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min and 30min.
In this range, the longer the deposition time, the stronger the bonding strength between the base layer deposited on the magnesium-aluminum alloy substrate and the magnesium-aluminum alloy substrate.
In some embodiments, the volume flow of argon in the second working gas is 100 to 300sccm.
The volume flow rate of the argon gas in the second working gas is selected from one or two of 100sccm, 110sccm, 120sccm, 130sccm, 140sccm, 150sccm, 160sccm, 170sccm, 180sccm, 190sccm, 200sccm, 210sccm, 220sccm, 230sccm, 240sccm, 250sccm, 260sccm, 270sccm, 280sccm, 290sccm, and 300sccm.
In this embodiment, the volume flow of argon in the second working gas is 100-300 sccm, so that the damage to the surface of the magnesium-aluminum alloy substrate caused by excessive argon in the second working gas is avoided while the oxide film is removed from the magnesium-aluminum alloy substrate, and the greater the volume flow of argon in the second working gas in the range, the stronger the effect of removing the oxide film from the magnesium-aluminum alloy substrate. And after the oxide film on the magnesium-aluminum alloy substrate is removed through the argon in the first working gas, argon is still contained in the introduced second working gas so as to further remove the oxide film on the magnesium-aluminum alloy substrate, thereby ensuring the deposition effect of the diamond-like carbon film layer.
In some embodiments, the volume flow of the tetramethylsilane in the second working gas is 10 to 40sccm, so as to ensure the deposition effect of the silicon transition layer on the magnesium-aluminum alloy substrate in the magnetron sputtering process, thereby ensuring the bonding strength of the magnesium-aluminum alloy substrate and the diamond-like film layer, and also ensuring the structural compactness of the formed composite diaphragm, and in this range, the larger the volume flow of the tetramethylsilane in the second working gas, the thicker the silicon transition layer is, and the bonding strength of the magnesium-aluminum alloy substrate and the diamond-like film layer is stronger.
The volumetric flow rate of the tetramethylsilane in the second working gas is selected from one or two of 10sccm, 15sccm, 20sccm, 25sccm, 30sccm, 35sccm, and 40sccm.
In some embodiments, the volumetric flow rate of acetylene in the second working gas is 100 to 300sccm.
The volume flow rate of acetylene in the second working gas is selected from one or two of 100sccm, 110sccm, 120sccm, 130sccm, 140sccm, 150sccm, 160sccm, 170sccm, 180sccm, 190sccm, 200sccm, 210sccm, 220sccm, 230sccm, 240sccm, 250sccm, 260sccm, 270sccm, 280sccm, 290sccm, and 300sccm.
In some embodiments, a diamond-like film layer is deposited on the base layer under second pulsed magnetron sputtering conditions, wherein the second pulsed magnetron sputtering conditions comprise at least one of an excitation voltage of 1000 to 2000V, an excitation current of 10 to 70A, a pulse width of 10 to 30 μs, a pulse frequency of 1000 to 1500Hz, a bias voltage of-200 to 0V, and an operating gas pressure of 1 to 4 Pa.
The excitation voltage in the second pulse magnetron sputtering condition is selected from one or two of 1000V, 1100V, 1200V, 1300V, 1400V, 1500V, 1600V, 1700V, 1800V, 1900V, 2000V.
The excitation current in the second pulse magnetron sputtering condition is selected from one or two of 10A, 20A, 30A, 40A, 50A, 60A and 70A.
The pulse width in the second pulse magnetron sputtering condition is selected from one or two of 10 μs, 15 μs, 20 μs, 25 μs and 30 μs.
The pulse frequency in the second pulse magnetron sputtering condition is selected from one or two of 1000Hz, 1100Hz, 1200Hz, 1300Hz, 1400Hz and 1500 Hz.
The operating air pressure in the second pulse magnetron sputtering condition is selected from one or two of the range values of 1Pa, 1.1Pa, 1.2Pa, 1.3Pa, 1.4Pa, 1.5Pa, 1.6Pa, 1.7Pa, 1.8Pa, 1.9Pa, 2Pa, 2.1Pa, 2.2Pa, 2.3Pa, 2.4Pa, 2.5Pa, 2.6Pa, 2.7Pa, 2.8Pa, 2.9Pa, 3Pa, 3.1Pa, 3.2Pa, 3.3Pa, 3.4Pa, 3.5Pa, 3.6Pa, 3.7Pa, 3.8Pa, 3.9Pa, 4 Pa.
The pulse plasma in the pulse magnetron sputtering is used for enhancing the chemical vapor deposition rate, has large and uniform deposition area and low cost, and is easy for industrialized mass production.
In some embodiments, the time to deposit the diamond-like film layer on the substrate layer is from 5 to 30 minutes.
The time for depositing the diamond-like film layer on the substrate layer is selected from one or two range values of 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min, 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min and 30min.
In this range, the longer the deposition time, the stronger the bond strength of the deposition-formed diamond-like film layer to the base layer.
In some embodiments, the diamond-like film layer has a thickness of 0.9 to 1.4 μm; although the thickness of the diamond-like film layer is increased to improve the acoustic performance of the prepared loudspeaker diaphragm, after the thickness of the diamond-like film layer is increased, the increase of the elastic modulus and the hardness is small, so that the production cost is increased, and meanwhile, more excellent performance cannot be obtained, so that the performance such as the elastic modulus, the hardness and the like of the diamond-like film layer with the thickness of 0.9-1.4 μm can be ensured, and meanwhile, the acoustic performance of the loudspeaker diaphragm prepared by the diamond-like film layer is also ensured.
The thickness of the diamond film layer may be selected from the range of one or both of 0.9 μm, 1 μm, 1.1 μm, 1.2 μm, 1.3 μm, 1.4 μm.
In some embodiments, the step of providing a magnesium aluminum alloy substrate comprises:
providing a magnesium-aluminum alloy raw material;
and carrying out ultrasonic cleaning on the magnesium aluminum alloy raw material to obtain a magnesium aluminum alloy matrix.
In this embodiment, ultrasonic cleaning can diversely wash magnadure raw materials, and cleaning efficiency is high, and the cleaning performance is good.
In some embodiments, the step of ultrasonically cleaning the magnesium aluminum alloy feedstock comprises:
and after performing first ultrasonic cleaning treatment on the magnesium-aluminum alloy raw material for 10 to 50 minutes through an acetone solution or a sodium hydroxide solution, performing second ultrasonic cleaning treatment on the magnesium-aluminum alloy raw material subjected to the first ultrasonic cleaning treatment for 10 to 50 minutes through deionized water or absolute ethyl alcohol.
In this embodiment, the surface oil stain of the magnesium-aluminum alloy raw material is removed by an acetone solution or a sodium hydroxide solution, the magnesium-aluminum alloy raw material is primarily cleaned, and then the magnesium-aluminum alloy raw material which is cleaned by the acetone solution or the sodium hydroxide solution is secondarily cleaned by deionized water or absolute ethyl alcohol, so as to remove organic impurities and residual ions on the surface of the magnesium-aluminum alloy raw material.
Further, the magnesium-aluminum alloy raw material is subjected to the first ultrasonic cleaning treatment for one or more range values selected from 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min and 50min by an acetone solution or a sodium hydroxide solution.
Further, the magnesium-aluminum alloy raw material subjected to the first ultrasonic cleaning treatment is subjected to the second ultrasonic cleaning treatment for one or more range values selected from 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min and 50min by deionized water or absolute ethyl alcohol.
In some embodiments, the step S102, before the step of using argon and tetramethylsilane as the first working gas, further includes:
and forming a rough surface on the magnesium-aluminum alloy substrate by taking inert gas as third working gas under the preset cavity pressure condition.
In this embodiment, the rough surface is used to improve the bonding strength between the magnesium-aluminum alloy substrate and the substrate layer formed by subsequent deposition thereon, so as to improve the structural stability of the magnesium-aluminum alloy substrate and the substrate layer; meanwhile, the frequency curve of the finally formed composite vibrating diaphragm is smooth, and the hearing effect is enhanced.
In some embodiments, the inert gas is at least one of helium, neon, argon, krypton, xenon, radon, og. Optionally, the inert gas is argon, and because the first working gas in S102 and the second working gas in S103 also contain argon, the preparation of the operator gas is facilitated, and the preparation steps are simplified.
In some embodiments, the volume flow of the inert gas in the third working gas is 100 to 300sccm.
The volume flow rate of the inert gas in the third working gas is selected from one or two of 100sccm, 110sccm, 120sccm, 130sccm, 140sccm, 150sccm, 160sccm, 170sccm, 180sccm, 190sccm, 200sccm, 210sccm, 220sccm, 230sccm, 240sccm, 250sccm, 260sccm, 270sccm, 280sccm, 290sccm, and 300sccm.
In this embodiment, the volume flow of the inert gas in the third working gas is 100 to 300sccm, so as to ensure that the magnesium-aluminum alloy substrate forms a rough surface, and avoid damage to the surface of the magnesium-aluminum alloy substrate caused by excessive argon in the third working gas.
In some embodiments, the rough surface is formed on the magnesium aluminum alloy substrate under a third pulse magnetron sputtering condition, wherein the third pulse magnetron sputtering condition comprises at least one of an excitation voltage of 1200 to 2200V, an excitation current of 50 to 150A, a pulse width of 10 to 30 μs, a pulse frequency of 1000 to 1500Hz, a bias voltage of-500 to-200V, and an operating gas pressure of 0.6 to 1.6 Pa.
The excitation voltage in the third pulse magnetron sputtering condition is selected from one or two of 1200V, 1300V, 1400V, 1500V, 1600V, 1700V, 1800V, 1900V, 2000V, 2100V, 2200V.
The excitation current in the third pulse magnetron sputtering condition is selected from a range of values between one or two of 50A, 60A, 70A, 80A, 90A, 100A, 110A, 120A, 130A, 140A, 150A.
The pulse width in the third pulse magnetron sputtering condition is selected from one or two of 10 μs, 15 μs, 20 μs, 25 μs and 30 μs.
The pulse frequency in the third pulse magnetron sputtering condition is selected from one or two of 1000Hz, 1100Hz, 1200Hz, 1300Hz, 1400Hz and 1500 Hz.
The operating air pressure in the third pulse magnetron sputtering condition is selected from one or two of 0.6Pa, 0.7Pa, 0.8Pa, 0.9Pa, 1Pa, 1.1Pa, 1.2Pa, 1.3Pa, 1.4Pa, 1.5Pa and 1.6 Pa.
The pulse plasma in the pulse magnetron sputtering is used for enhancing the chemical vapor deposition rate, has large and uniform deposition area and low cost, and is easy for industrialized mass production.
In some embodiments, the rough surface is formed on the magnesium aluminum alloy substrate for 10 to 50 minutes.
The time for forming the rough surface on the magnesium-aluminum alloy matrix is selected from one or two of 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min and 50min.
In order to better understand the technical solutions of the present application, the following description will clearly and completely describe the technical solutions in the embodiments of the present application with reference to the accompanying drawings.
Example 1-1:
the preparation method of the composite loudspeaker diaphragm of the embodiment 1-1 is as follows:
step S101, providing a magnesium-aluminum alloy matrix;
step S102, at a vacuum level of 1×10 -3 Under the preset cavity pressure condition, taking argon with the volume flow of 100sccm and tetramethylsilane with the volume flow of 10sccm as first working gases, and depositing and forming a substrate layer on the magnesium-aluminum alloy substrate;
step S103, at a vacuum degree of 1×10 -3 Under the preset cavity pressure condition, taking argon with the volume flow of 100sccm, tetramethylsilane with the volume flow of 10sccm and acetylene with the volume flow of 100sccm as second working gases, and depositing a diamond-like film layer with the thickness of 0.9 μm on the substrate layer to obtain the composite diaphragm.
Example 2-1:
the preparation method of the composite loudspeaker diaphragm of the embodiment 2-1 is as follows:
step S101, providing a magnesium-aluminum alloy matrix;
step S102, at a vacuum level of 1×10 -3 Under the preset cavity pressure condition, taking argon with the volume flow of 200sccm and tetramethylsilane with the volume flow of 25sccm as first working gases, and depositing and forming a substrate layer on the magnesium-aluminum alloy substrate;
step S103, at a vacuum degree of 1×10 -3 Under the preset cavity pressure condition, argon with the volume flow of 200sccm, tetramethylsilane with the volume flow of 25sccm and acetylene with the volume flow of 200sccm are used as second working gases, and a diamond-like film layer with the thickness of 1.2 μm is deposited on the substrate layer, so that the composite diaphragm is obtained.
Example 3-1:
the preparation method of the composite loudspeaker diaphragm of the embodiment 3-1 is as follows:
step S101, providing a magnesium-aluminum alloy matrix;
step S102, at a vacuum level of 1×10 -3 Under the preset cavity pressure condition, taking argon with the volume flow of 300sccm and tetramethylsilane with the volume flow of 40sccm as first working gases, and depositing and forming a substrate layer on the magnesium-aluminum alloy substrate;
step S103, at a vacuum degree of 1×10 -3 Under the preset cavity pressure condition, argon with the volume flow of 300sccm and tetranychium with the volume flow of 40sccm are used for preparing the high-pressure liquid crystal displayAnd (3) taking the silane and 300sccm of acetylene as a second working gas, and depositing a diamond-like film layer with the thickness of 1.4 mu m on the substrate layer to obtain the composite diaphragm.
Comparative examples 1-1:
the preparation method of the composite loudspeaker diaphragm of the comparative example 1-1 is as follows:
providing a magnesium-aluminum alloy matrix;
at a vacuum degree of 1X 10 -3 Under the preset cavity pressure condition, argon with the volume flow of 200sccm, tetramethylsilane with the volume flow of 25sccm and acetylene with the volume flow of 200sccm are used as second working gases, and a diamond-like film layer with the thickness of 0.96 μm is deposited on the substrate layer, so that the composite diaphragm is obtained.
Comparative example 2-1:
comparative example 2-1 provides a magnesium aluminum alloy substrate with the magnesium aluminum alloy substrate as a loudspeaker diaphragm.
Test one:
1. test sample: examples 1-1 to 3-1, comparative example 1-1 and comparative example 2-1 of the present application.
2. Formal test: the elastic moduli of examples 1-1 to 3-1, comparative example 1-1 and comparative example 2-1 were measured by a nanoindenter; the Vickers hardness of examples 1-1 to 3-1, comparative example 1-1 and comparative example 2-1 were measured by a Vickers hardness tester.
Table one: results of the test for modulus of elasticity and Vickers hardness
Elastic modulus (Unit: GPa) Vickers hardness (Unit: HV)
Example 1-1 185.3 18.85
Example 2-1 193.5 21.64
Example 3-1 202.5 23.62
Comparative examples 1 to 1 122.7 27.34
Comparative example 2-1 56.7 38.48
As can be seen from table one, in embodiments 1-1 to 3-1 of the present application, before depositing the diamond-like film layer, the surface oxide film of the magnesium-aluminum alloy substrate is removed by argon in step S102, and the substrate layer is deposited on the magnesium-aluminum alloy substrate by tetramethylsilane, so as to effectively reduce the internal stress of the magnesium-aluminum alloy substrate and the diamond-like film layer in the subsequent step, and then the surface oxide film of the magnesium-aluminum alloy substrate is further removed by argon in step S103, so as to further improve the bonding force between the substrate layer formed by depositing tetramethylsilane on the magnesium-aluminum alloy substrate and the magnesium-aluminum alloy substrate, and meanwhile, the diamond-like film layer is formed on the substrate layer by acetylene matching, so as to obtain the composite diaphragm, thereby effectively improving the bonding force between the magnesium-aluminum alloy substrate and the diamond-like film layer; therefore, the composite diaphragms prepared in examples 1-1 to 3-1 of the present application have a larger elastic modulus and Vickers hardness than those of comparative examples 1-1 and 2-1, so that the amplitude of bending vibration of the loudspeaker diaphragms in operation is suppressed, the frequency response curve can be flattened more, and the playback frequency band can be widened appropriately.
Further, raman spectra of example 2-1 and comparative example 1-1 of the present application were detected by a Raman spectrometer, respectively; FIG. 2 is a Raman spectrum of example 2-1 of the present application, FIG. 3 is a Raman spectrum of comparative example 1-1, wherein the Raman spectrum can characterize sp in the diamond-like film 2 And sp (sp) 3 Content of hybridized carbon atoms. In Raman spectroscopy, I D /I G Representing the graphitization degree of carbon, the smaller the ratio, the sp in the sample 3 The higher the content, the hardness of the diamond-like film layer and sp in the diamond-like film layer 3 The content of bonds being related to sp 3 The higher the bond content, the higher the hardness of the diamond-like film layer, so that the embodiment 2-1 of the present application has more step S102 than the comparative example 1-1, and this step can further remove the oxide film on the surface of the magnesium-aluminum alloy, and improve the film-base binding force between the diamond-like film layer and the magnesium-aluminum alloy substrate, so that the composite diaphragm prepared in the embodiment 2-1 of the present application has the I D /I G Smaller, the corresponding modulus of elasticity and vickers hardness are high (see table one).
Further, examples 1-2:
at a vacuum degree of 1X 10 -3 Under the preset cavity pressure condition, taking inert gas of argon with the volume flow of 100sccm as third working gas, and forming a rough surface on the magnesium aluminum alloy substrate.
Example 2-2:
at a vacuum degree of 1X 10 -3 Under the preset cavity pressure condition, taking inert gas of argon with the volume flow of 200sccm as third working gas, and forming a rough surface on the magnesium aluminum alloy substrate.
Example 3-2:
at a vacuum degree of 1X 10 -3 Under the preset cavity pressure condition, taking inert gas of argon with the volume flow of 300sccm as third working gas, and forming a rough surface on the magnesium aluminum alloy substrate.
Comparative examples 1 to 2
At a vacuum degree of 1X 10 -3 Under the preset cavity pressure condition, inert gas of argon with the volume flow of 200sccm is used as third working gasAnd forming a rough surface on the magnesium-aluminum alloy substrate.
And (2) testing II:
1. test sample: examples 1-2 to 3-2, comparative examples 1-2 and comparative examples 2-1 of the present application.
2. Formal test: the roughness of examples 1-2 to 3-2, comparative examples 1-2 and comparative example 2-1 was measured by atomic microscopy.
And (II) table: roughness test results
As can be obtained from table two, the surface roughness of each of the embodiments 1-2 to 3-2 of the present application is smaller than that of the comparative examples 1-2 and 2-1, so that the frequency response transitions of the embodiments 1-2 to 3-2 of the present application are flatter, and the sound effect of the composite diaphragm is effectively improved; by way of example, referring to fig. 4, fig. 4 is a graph comparing the frequency response curves of examples 2-2, comparative examples 1-2 and comparative examples 2-1 of the present application, and it can be seen that the frequency response curve of example 2-2 has a reduced dip, enhancing the smoothness of the curve.
The application also provides a composite loudspeaker diaphragm, which is prepared by the preparation method of the composite loudspeaker diaphragm.
According to the method, argon and tetramethylsilane are used as first working gases, the surface oxide film of the magnesium aluminum alloy substrate is removed through the argon, the substrate layer is deposited on the magnesium aluminum alloy substrate through the tetramethylsilane, so that the internal stress of the magnesium aluminum alloy substrate and the diamond-like carbon film layer in the follow-up process is effectively reduced, then argon, tetramethylsilane and acetylene are used as second working gases, the surface oxide film of the magnesium aluminum alloy substrate is further removed through the argon, the bonding force between the substrate layer formed by the deposition of the tetramethylsilane on the magnesium aluminum alloy substrate and the magnesium aluminum alloy substrate is further improved, and meanwhile, the diamond-like carbon film layer is formed on the substrate layer through the cooperation of the acetylene, so that the composite diaphragm is obtained, the film base bonding force between the magnesium aluminum alloy substrate and the diamond-like carbon film layer can be effectively improved, the prepared composite diaphragm is further improved to have higher elastic modulus and Vickers hardness, the bending vibration amplitude of the loudspeaker diaphragm is restrained in working, the frequency response curve is relatively flat, the replay frequency band is widened, and the tone quality of the loudspeaker diaphragm is effectively improved.
The application also provides a loudspeaker, which comprises the composite loudspeaker diaphragm prepared by the preparation method of the composite loudspeaker diaphragm or the composite loudspeaker diaphragm.
According to the method, argon and tetramethylsilane are used as first working gases, the surface oxide film of the magnesium aluminum alloy substrate is removed through the argon, the substrate layer is deposited on the magnesium aluminum alloy substrate through the tetramethylsilane, so that the internal stress of the magnesium aluminum alloy substrate and the diamond-like carbon film layer in the follow-up process is effectively reduced, then argon, tetramethylsilane and acetylene are used as second working gases, the surface oxide film of the magnesium aluminum alloy substrate is further removed through the argon, the bonding force between the substrate layer formed by the deposition of the tetramethylsilane on the magnesium aluminum alloy substrate and the magnesium aluminum alloy substrate is further improved, and meanwhile, the diamond-like carbon film layer is formed on the substrate layer through the cooperation of the acetylene, so that the composite diaphragm is obtained, the film base bonding force between the magnesium aluminum alloy substrate and the diamond-like carbon film layer can be effectively improved, the prepared composite diaphragm is further improved to have higher elastic modulus and Vickers hardness, the bending vibration amplitude of the loudspeaker diaphragm is restrained in working, the frequency response curve is relatively flat, the replay frequency band is widened, and the tone quality of the loudspeaker diaphragm is effectively improved.
The application also provides an electronic device comprising the loudspeaker.
In this embodiment, the electronic device may be a mobile phone, a tablet, a television, a display, a speaker, or the like with a speaker built therein.
The loudspeaker that this electronic equipment adopted is as above-mentioned compound loudspeaker vibrating diaphragm, this compound loudspeaker vibrating diaphragm uses argon gas and tetramethyl silane as first working gas earlier, with get rid of the top layer oxide film of magnalium base member through the argon gas, and deposit the stratum basale on the magnalium base member through tetramethyl silane, with the internal stress that effectively reduces magnalium base member and diamond-like carbon rete in follow-up, afterwards use argon gas, tetramethyl silane and acetylene as second working gas, with the top layer oxide film of getting rid of the magnalium base member through the argon gas, further promote the cohesion of stratum basale and the magnalium base member that tetramethyl silane deposit formed on the magnalium base member, form diamond-like carbon rete on the stratum basale through the cooperation of acetylene simultaneously, obtain compound vibrating diaphragm, so can effectively improve the membrane base cohesion of magnalium base member and diamond-like carbon rete, and then the compound vibrating diaphragm that the preparation obtained has higher elastic modulus and vickers hardness, make the bending vibration range of speaker at the during operation obtain the suppression, the frequency response curve relatively becomes flatter, and the tone quality of playback frequency band has effectively promoted the vibrating diaphragm.
It is apparent that the embodiments described above are only some embodiments of the present application, but not all embodiments, the preferred embodiments of the present application are given in the drawings, but not limiting the patent scope of the present application. This application may be embodied in many different forms, but rather, embodiments are provided in order to provide a more thorough understanding of the present disclosure. Although the present application has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing, or equivalents may be substituted for elements thereof. All equivalent structures made by the specification and the drawings of the application are directly or indirectly applied to other related technical fields, and are also within the protection scope of the application.

Claims (9)

1. The preparation method of the composite loudspeaker diaphragm is characterized by comprising the following steps:
providing a magnesium-aluminum alloy matrix;
under the condition of preset cavity pressure, argon and tetramethylsilane are used as first working gases, and a base layer is formed on the magnesium-aluminum alloy substrate in a deposition mode;
under the preset cavity pressure condition, argon, tetramethylsilane and acetylene are used as second working gases, and a diamond-like film layer is deposited on the substrate layer to obtain a composite vibrating diaphragm;
wherein the volume flow of argon in the first working gas is 100-300 sccm;
and/or the volumetric flow rate of the tetramethylsilane in the first working gas is 10 to 40sccm;
and/or depositing a base layer on the magnesium-aluminum alloy substrate under a first pulse magnetron sputtering condition, wherein the first pulse magnetron sputtering condition comprises at least one of excitation voltage of 1200-2200V, excitation current of 50-150A, pulse width of 10-30 mu s, pulse frequency of 1000-1500 Hz, bias voltage of-300-100V and working air pressure of 0.7-2 Pa;
and/or depositing and forming a basal layer on the magnesium-aluminum alloy matrix for 5 to 30 minutes.
2. The method for preparing a composite loudspeaker diaphragm of claim 1,
the volume flow of the argon in the second working gas is 100-300 sccm;
and/or the volumetric flow rate of the tetramethylsilane in the second working gas is 10 to 40sccm;
and/or the volumetric flow rate of the acetylene in the second working gas is 100 to 300sccm;
and/or depositing a diamond-like film layer on the substrate layer under a second pulse magnetron sputtering condition, wherein the second pulse magnetron sputtering condition comprises at least one of an excitation voltage of 1000 to 2000V, an excitation current of 10 to 70A, a pulse width of 10 to 30 μs, a pulse frequency of 1000 to 1500Hz, a bias voltage of-200 to 0V and an operating pressure of 1 to 4 Pa;
and/or depositing a diamond-like film layer on the substrate layer for 5 to 30 minutes;
and/or the diamond-like film layer has a thickness of 0.9 to 1.4 μm.
3. The method for manufacturing a composite loudspeaker diaphragm according to claim 1 or 2, wherein the step of providing a magnesium aluminum alloy substrate comprises:
providing a magnesium-aluminum alloy raw material;
and carrying out ultrasonic cleaning on the magnesium aluminum alloy raw material to obtain a magnesium aluminum alloy matrix.
4. The method for preparing a composite loudspeaker diaphragm according to claim 3, wherein the step of ultrasonically cleaning the magnesium-aluminum alloy material comprises:
and after performing first ultrasonic cleaning treatment on the magnesium-aluminum alloy raw material for 10 to 50 minutes through an acetone solution or a sodium hydroxide solution, performing second ultrasonic cleaning treatment on the magnesium-aluminum alloy raw material subjected to the first ultrasonic cleaning treatment for 10 to 50 minutes through deionized water or absolute ethyl alcohol.
5. The method for preparing a composite loudspeaker diaphragm according to claim 1 or 2, further comprising, prior to the step of using argon and tetramethylsilane as the first working gas:
and forming a rough surface on the magnesium-aluminum alloy substrate by taking inert gas as third working gas under the preset cavity pressure condition.
6. The method for preparing a composite loudspeaker diaphragm of claim 5,
the inert gas is at least one of helium, neon, argon, krypton, xenon, radon and Og;
and/or the volume flow of the inert gas in the third working gas is 100 to 300sccm;
and/or forming a rough surface on the magnesium-aluminum alloy substrate under a third pulse magnetron sputtering condition, wherein the third pulse magnetron sputtering condition comprises at least one of excitation voltage of 1200-2200V, excitation current of 50-150A, pulse width of 10-30 mu s, pulse frequency of 1000-1500 Hz, bias voltage of-500-200V and working air pressure of 0.6-1.6 Pa;
and/or forming the rough surface on the magnesium-aluminum alloy substrate for 10 to 50 minutes.
7. A composite loudspeaker diaphragm prepared by the method of preparing a composite loudspeaker diaphragm according to any one of claims 1 to 6.
8. A loudspeaker comprising a composite loudspeaker diaphragm produced by the method of producing a composite loudspeaker diaphragm according to any one of claims 1 to 6, or a composite loudspeaker diaphragm according to claim 7.
9. An electronic device comprising the speaker of claim 8.
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