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CN118147578A - Aluminum nitride coating with different preferred orientations and preparation method thereof - Google Patents

Aluminum nitride coating with different preferred orientations and preparation method thereof Download PDF

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CN118147578A
CN118147578A CN202311827538.5A CN202311827538A CN118147578A CN 118147578 A CN118147578 A CN 118147578A CN 202311827538 A CN202311827538 A CN 202311827538A CN 118147578 A CN118147578 A CN 118147578A
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aluminum nitride
substrate
nitride coating
preferred
coating
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CN118147578B (en
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肖舒
吴熠
刘健诚
黄勇
范舒瑜
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South China University of Technology SCUT
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0617AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • C23C14/5826Treatment with charged particles
    • C23C14/5833Ion beam bombardment

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  • Engineering & Computer Science (AREA)
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  • Physical Vapour Deposition (AREA)

Abstract

An aluminum nitride coating containing different preferred orientations and a preparation method thereof, wherein the preparation method comprises the following steps: feeding the substrate cleaned by the plasma into a reaction cavity, and depositing a first preferred orientation aluminum nitride coating on the surface of the substrate by adopting a magnetron sputtering mode; feeding the deposited substrate into a static placing chamber, and cooling to a preset temperature; delivering the cooled substrate into a transition chamber in vacuum pumping, bombarding the first preferred orientation aluminum nitride coating by adopting a gas ion source, and depositing the first preferred orientation aluminum nitride coating to form an amorphous aluminum nitride transition layer; and (3) sending the substrate after amorphization into a reaction cavity, and depositing a second preferred orientation aluminum nitride coating on the surface of the amorphous aluminum nitride transition layer by adopting a magnetron sputtering mode. According to the invention, aluminum nitride coatings with different preferred orientations are compounded on the same substrate by adopting an ion source bombardment technology to replace a single aluminum oxide coating, so that the performance compounding is realized, and the mechanical property, the insulation barrier property and the corrosion resistance of the CVD Mask are improved.

Description

一种含有不同择优取向的氮化铝涂层及制备方法Aluminum nitride coating with different preferred orientations and preparation method thereof

技术领域Technical Field

本发明涉及材料表面处理技术领域,特别涉及一种含有不同择优取向的氮化铝涂层及制备方法。The invention relates to the technical field of material surface treatment, and in particular to an aluminum nitride coating containing different preferred orientations and a preparation method thereof.

背景技术Background technique

近年来,柔性OLED显示技术正逐步成为主流显示技术,而高质量的化学气相沉积用掩膜板(CVD Mask)是实现OLED高质量封装性能的关键。因CVD Mask对位置精度要求十分严格,为了避免因温度变化导致的位置变形,一般采用因瓦合金制备CVD Mask。而为了提高CVD Mask的阻隔绝缘耐腐蚀特性,通常在其表面制备一层Al2O3薄膜,但因瓦合金的热膨胀系数与Al2O3差异大,沉积薄膜过程中易引起CVD Mask变形,无法保证CVD Mask精度,且较大的内应力甚至会导致脱膜失效。In recent years, flexible OLED display technology is gradually becoming the mainstream display technology, and high-quality chemical vapor deposition mask (CVD Mask) is the key to achieving high-quality OLED packaging performance. Because CVD Mask has very strict requirements on position accuracy, in order to avoid position deformation caused by temperature changes, CVD Mask is generally prepared using Invar alloy. In order to improve the barrier insulation and corrosion resistance of CVD Mask, a layer of Al 2 O 3 film is usually prepared on its surface, but the thermal expansion coefficient of Invar alloy is very different from that of Al 2 O 3 , which can easily cause deformation of CVD Mask during the deposition of thin films, and the accuracy of CVD Mask cannot be guaranteed. In addition, the large internal stress may even lead to demolding failure.

发明内容Summary of the invention

基于此,本发明的目的是提供一种含有不同择优取向的氮化铝涂层及制备方法,通过采用含有不同择优取向的氮化铝涂层复合结构,替换单一的氧化铝涂层,以提高CVDMask的力学性能、绝缘阻隔性和耐腐蚀性。Based on this, the purpose of the present invention is to provide an aluminum nitride coating containing different preferred orientations and a preparation method, by adopting a composite structure of aluminum nitride coating containing different preferred orientations to replace the single aluminum oxide coating, so as to improve the mechanical properties, insulation barrier properties and corrosion resistance of CVDMask.

第一方面,本发明提供一种含有不同择优取向的氮化铝涂层,成形于基材的表面,包括位于所述基材表面上的第一择优取向氮化铝涂层,位于所述第一择优取向氮化铝涂层表面上的非晶氮化铝过渡层,以及位于所述非晶氮化铝过渡层表面上的第二择优取向氮化铝涂层,所述第二择优取向氮化铝涂层和所述第一择优取向氮化铝涂层的择优取向不相同。In a first aspect, the present invention provides an aluminum nitride coating containing different preferred orientations, formed on the surface of a substrate, including a first preferred orientation aluminum nitride coating located on the surface of the substrate, an amorphous aluminum nitride transition layer located on the surface of the first preferred orientation aluminum nitride coating, and a second preferred orientation aluminum nitride coating located on the surface of the amorphous aluminum nitride transition layer, wherein the preferred orientations of the second preferred orientation aluminum nitride coating and the first preferred orientation aluminum nitride coating are different.

进一步地,所述第一择优取向氮化铝涂层的厚度为1~3um,所述非晶氮化铝过渡层的厚度为50~200nm;所述第二择优取向氮化铝涂层的厚度为1~3um。Furthermore, the thickness of the first preferentially oriented aluminum nitride coating is 1 to 3 um, the thickness of the amorphous aluminum nitride transition layer is 50 to 200 nm; and the thickness of the second preferentially oriented aluminum nitride coating is 1 to 3 um.

进一步地,该氮化铝涂层的择优取向为氧化铝晶体的首选晶面取向。Furthermore, the preferred orientation of the aluminum nitride coating is the preferred crystal plane orientation of aluminum oxide crystals.

进一步地,该首选晶面以纤锌矿为主要晶体结构,表现出a轴方向生长或c轴方向生长。Furthermore, the preferred crystal plane has wurtzite as a main crystal structure, showing growth in the a-axis direction or the c-axis direction.

第二方面,本发明提供一种含有不同择优取向的氮化铝涂层的制备方法,包括以下步骤:In a second aspect, the present invention provides a method for preparing an aluminum nitride coating having different preferred orientations, comprising the following steps:

步骤S10,将等离子体清洗后的基材送入反应腔中,采用磁控溅射方式在所述基材的表面上沉积第一择优取向氮化铝涂层,所述基材以第一预设速度运动;Step S10, placing the plasma-cleaned substrate into a reaction chamber, and depositing a first preferentially oriented aluminum nitride coating on the surface of the substrate by magnetron sputtering, with the substrate moving at a first preset speed;

步骤S11,将沉积后的基材送入静放室中,进行冷却至预设温度;Step S11, sending the deposited substrate into a static chamber to cool it to a preset temperature;

步骤S12,将冷却后的基材送入抽真空的过渡腔室内,采用气体离子源轰击所述第一择优取向氮化铝涂层,以在所述第一择优取向氮化铝涂层沉积形成非晶氮化铝过渡层;Step S12, sending the cooled substrate into a vacuum transition chamber, bombarding the first preferentially oriented aluminum nitride coating with a gas ion source, so as to deposit an amorphous aluminum nitride transition layer on the first preferentially oriented aluminum nitride coating;

步骤S13,将非晶化后的基材送入反应腔中,采用磁控溅射方式在所述非晶氮化铝过渡层的表面沉积形成第二择优取向氮化铝涂层,所述基材以第二预设速度运动,所述第二预设速度与所述第一预设速度不相同。In step S13, the amorphized substrate is fed into a reaction chamber, and a second preferentially oriented aluminum nitride coating is deposited on the surface of the amorphous aluminum nitride transition layer by magnetron sputtering. The substrate moves at a second preset speed, which is different from the first preset speed.

进一步地,在步骤S10和步骤S13中,磁控溅射所采用的电源为中频电源,电压为300~600V,工作气体为氩气,反应气体为氮气。Furthermore, in step S10 and step S13, the power source used for magnetron sputtering is a medium frequency power source, the voltage is 300-600V, the working gas is argon, and the reaction gas is nitrogen.

进一步地,在步骤S11中,预设温度为20~50℃。Furthermore, in step S11, the preset temperature is 20-50°C.

进一步地,在步骤S12中,气体离子源为线性阳极离子源,工作气体为氩气,电压可调范围为50~300V,轰击时间为10~30min。Further, in step S12, the gas ion source is a linear anode ion source, the working gas is argon, the voltage is adjustable in the range of 50 to 300 V, and the bombardment time is 10 to 30 minutes.

进一步地,在步骤S10中,所述基材安装在反应腔中的平动轨道上,所述平动轨道带动所述基材做往复移动;Further, in step S10, the substrate is mounted on a translation track in the reaction chamber, and the translation track drives the substrate to reciprocate;

所述平动轨道上设有对所述基材通入负偏置电压的脉冲偏压电源,和对所述基材加热的加热装置。The translation track is provided with a pulse bias power supply for applying a negative bias voltage to the substrate and a heating device for heating the substrate.

进一步地,所述脉冲偏压电源的电压范围为0~500V,所述加热装置的加热温度范围为50~200℃,所述平动轨道的运动速度范围为0~200mm/s。Furthermore, the voltage range of the pulse bias power supply is 0-500V, the heating temperature range of the heating device is 50-200°C, and the movement speed range of the translation track is 0-200mm/s.

进一步地,在步骤S10之前,该制备方法还包括:Furthermore, before step S10, the preparation method further comprises:

采用软接触电动叉车将基材转运至定位台架上,通过机械手自动将基材送至清洗设备中进行超声波清洗,并干燥;The substrate is transferred to the positioning stand by a soft-contact electric forklift, and the substrate is automatically sent to the cleaning equipment for ultrasonic cleaning and drying by a manipulator;

将干燥后的基材通过机械手自动转运至真空腔内,进行抽真空达到预设真空度后,持续通入工作气体;The dried substrate is automatically transferred to the vacuum chamber by a robot, and after the vacuum is evacuated to a preset vacuum degree, the working gas is continuously introduced;

采用气体离子源轰击基材表面,以对基材进行等离子体清洗。A gas ion source is used to bombard the substrate surface to perform plasma cleaning on the substrate.

进一步地,气体离子源为线性阳极离子源,工作气体为氩气,电压可调范围为800~1000V,轰击时间为10~30min。Furthermore, the gas ion source is a linear anode ion source, the working gas is argon, the voltage can be adjusted in the range of 800 to 1000 V, and the bombardment time is 10 to 30 minutes.

相较现有技术,本发明中,通过采用离子源轰击技术将不同择优取向的氮化铝涂层复合在同一基材上,替换单一的氧化铝涂层,实现性能的复合,以提高CVD Mask的力学性能、绝缘阻隔性和耐腐蚀性。Compared with the prior art, in the present invention, aluminum nitride coatings with different preferential orientations are composited on the same substrate by adopting ion source bombardment technology to replace the single aluminum oxide coating, thereby achieving performance composite, so as to improve the mechanical properties, insulation barrier properties and corrosion resistance of the CVD Mask.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

图1为本发明中含有不同择优取向的氮化铝涂层的结构示意图;FIG1 is a schematic diagram of the structure of an aluminum nitride coating having different preferred orientations in the present invention;

图2为本发明中含有不同择优取向的氮化铝涂层制备方法的结流程图;FIG2 is a flow chart of a method for preparing aluminum nitride coatings having different preferred orientations according to the present invention;

图3为本发明中hcp-AlN晶体结构示意图;FIG3 is a schematic diagram of the hcp-AlN crystal structure of the present invention;

图4为本发明中不同的平动轨道运动速度(0mm/s、5mm/s和200mm/s,试样分别命名为AlN-0,AlN-5,AlN-20)下制备的氮化铝涂层基材和涂层的XRD衍射图谱;FIG4 is an XRD diffraction pattern of the aluminum nitride coating substrate and coating prepared at different translational orbital motion speeds (0 mm/s, 5 mm/s and 200 mm/s, the samples are named AlN-0, AlN-5, AlN-20, respectively) in the present invention;

图5为本发明中不同的平动轨道运动速度(0mm/s、5mm/s和200mm/s,试样分别命名为AlN-0,AlN-5,AlN-20)下制备试样的表面和界面形貌图;FIG5 is a surface and interface morphology of samples prepared at different translational orbital motion speeds (0 mm/s, 5 mm/s and 200 mm/s, the samples are named AlN-0, AlN-5, AlN-20, respectively) in the present invention;

图6为发明中因瓦合金表面制备的不同择优取向氮化铝涂层的表面电阻率和介电强度测试结果图;FIG6 is a graph showing the surface resistivity and dielectric strength test results of aluminum nitride coatings with different preferred orientations prepared on the surface of Invar alloy in the present invention;

图7为本发明中因瓦合金表面制备的不同择优取向氮化铝涂层在1mol/LNaF溶液中的Tafel曲线及拟合的腐蚀电位和腐蚀电流密度曲线图;FIG7 is a Tafel curve of aluminum nitride coatings with different preferred orientations prepared on the surface of Invar alloy in the present invention in a 1 mol/L NaF solution and a fitted corrosion potential and corrosion current density curve;

图8为本发明中因瓦合金表面不同择优取向氮化铝涂层复合、上层及下层的XRD衍射图谱;FIG8 is an XRD diffraction spectrum of the composite, upper and lower layers of aluminum nitride coatings with different preferred orientations on the surface of Invar alloy in the present invention;

图9为本发明中因瓦合金表面不同择优取向氮化铝涂层两种不同复合顺序的截面形貌图。FIG. 9 is a cross-sectional morphology diagram of two different composite sequences of aluminum nitride coatings with different preferred orientations on the surface of Invar alloy in the present invention.

如下具体实施方式将结合上述附图进一步说明本发明。The following specific implementation manner will further illustrate the present invention in conjunction with the above-mentioned drawings.

具体实施方式Detailed ways

为了便于理解本发明,下面将参照相关附图对本发明进行更全面的描述。附图中给出了本发明的若干实施例。但是,本发明可以以许多不同的形式来实现,并不限于本文所描述的实施例。相反地,提供这些实施例的目的是使对本发明的公开内容更加透彻全面。In order to facilitate understanding of the present invention, the present invention will be described more fully below with reference to the relevant drawings. Several embodiments of the present invention are given in the drawings. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thorough and comprehensive.

请参阅图1,第一方面,本发明提供一种含有不同择优取向的氮化铝涂层,成形于基材的表面,包括位于所述基材表面上的第一择优取向氮化铝涂层,位于所述第一择优取向氮化铝涂层表面上的非晶氮化铝过渡层,以及位于所述非晶氮化铝过渡层表面上的第二择优取向氮化铝涂层,所述第二择优取向氮化铝涂层和所述第一择优取向氮化铝涂层的择优取向不相同,以便于两种不同择优取向的氮化铝涂层能够结合。Please refer to Figure 1. In the first aspect, the present invention provides an aluminum nitride coating containing different preferred orientations, which is formed on the surface of a substrate, including a first preferred orientation aluminum nitride coating located on the surface of the substrate, an amorphous aluminum nitride transition layer located on the surface of the first preferred orientation aluminum nitride coating, and a second preferred orientation aluminum nitride coating located on the surface of the amorphous aluminum nitride transition layer. The preferred orientations of the second preferred orientation aluminum nitride coating and the first preferred orientation aluminum nitride coating are different, so that the two aluminum nitride coatings with different preferred orientations can be combined.

需要说明的是,本申请中,所述第一择优取向氮化铝涂层的厚度为1~3um,所述非晶氮化铝过渡层的厚度为20~200nm;所述第二择优取向氮化铝涂层的厚度为1~3um。It should be noted that, in the present application, the thickness of the first preferentially oriented aluminum nitride coating is 1 to 3 um, the thickness of the amorphous aluminum nitride transition layer is 20 to 200 nm; the thickness of the second preferentially oriented aluminum nitride coating is 1 to 3 um.

进一步地,该氮化铝涂层的择优取向为氧化铝晶体的首选晶面取向。且该首选晶面以纤锌矿为主要晶体结构,表现出a轴方向生长或c轴方向生长。Furthermore, the preferred orientation of the aluminum nitride coating is the preferred crystal plane orientation of the aluminum oxide crystal, and the preferred crystal plane has wurtzite as the main crystal structure, showing growth in the a-axis direction or the c-axis direction.

请参阅图2,第二方面,本发明提供一种含有不同择优取向的氮化铝涂层的制备方法,包括以下步骤:Referring to FIG. 2 , in a second aspect, the present invention provides a method for preparing an aluminum nitride coating having different preferred orientations, comprising the following steps:

步骤S10,将等离子体清洗后的基材送入反应腔中,采用磁控溅射方式在所述基材的表面上沉积第一择优取向氮化铝涂层,所述基材以第一预设速度运动;Step S10, placing the plasma-cleaned substrate into a reaction chamber, and depositing a first preferentially oriented aluminum nitride coating on the surface of the substrate by magnetron sputtering, with the substrate moving at a first preset speed;

在本步骤中,磁控溅射所采用的电源为中频电源,电压为300~600V,工作气体为氩气,反应气体为氮气。In this step, the power source used for magnetron sputtering is a medium frequency power source with a voltage of 300-600V, the working gas is argon, and the reaction gas is nitrogen.

需要说明的是,本步骤中,所述基材安装在反应腔中的平动轨道上,所述平动轨道带动所述基材做往复移动,以进行往复式镀膜,且所述第一预设速度根据所需氮化铝涂层的择优取向进行设置;It should be noted that in this step, the substrate is mounted on a translation track in the reaction chamber, and the translation track drives the substrate to reciprocate to perform reciprocating coating, and the first preset speed is set according to the preferred orientation of the desired aluminum nitride coating;

所述平动轨道上设有对所述基材通入负偏置电压的脉冲偏压电源,和对所述基材加热的加热装置。The translation track is provided with a pulse bias power supply for applying a negative bias voltage to the substrate and a heating device for heating the substrate.

其中,所述脉冲偏压电源的电压范围为0~500V,所述加热装置的加热温度范围为50~200℃,所述平动轨道的运动速度范围为0~200mm/s。溅射电压优选为400~500V,通入的反应气体的标准流率优选为10sccm以上且20sccm以下,以确保溅射过程是在过渡条件下进行以得到标准化学计量比的氮化铝涂层。The voltage range of the pulse bias power supply is 0-500V, the heating temperature range of the heating device is 50-200°C, and the movement speed range of the translation track is 0-200mm/s. The sputtering voltage is preferably 400-500V, and the standard flow rate of the introduced reaction gas is preferably 10sccm or more and 20sccm or less to ensure that the sputtering process is carried out under transition conditions to obtain an aluminum nitride coating with a standard stoichiometric ratio.

步骤S11,将沉积后的基材送入静放室中,进行冷却至预设温度;Step S11, sending the deposited substrate into a static chamber to cool it to a preset temperature;

在本步骤中,预设温度为20~50℃。In this step, the preset temperature is 20-50°C.

步骤S12,将冷却后的基材送入抽真空的过渡腔室内,采用气体离子源轰击所述第一择优取向氮化铝涂层,以在所述第一择优取向氮化铝涂层沉积形成非晶氮化铝过渡层;Step S12, sending the cooled substrate into a vacuum transition chamber, bombarding the first preferentially oriented aluminum nitride coating with a gas ion source, so as to deposit an amorphous aluminum nitride transition layer on the first preferentially oriented aluminum nitride coating;

需要说明的是,本步骤中,采用气体离子源轰击第一择优取向氮化铝涂层是为了形成非晶氮化铝过渡层,以实现不同择优取向的氮化铝涂层在同一基材上的复合。It should be noted that, in this step, the gas ion source is used to bombard the first preferentially oriented aluminum nitride coating in order to form an amorphous aluminum nitride transition layer, so as to realize the composite of aluminum nitride coatings with different preferential orientations on the same substrate.

具体的,本步骤中,气体离子源为线性阳极离子源,工作气体为氩气,电压可调范围为50~300V,轰击时间为10~30min。Specifically, in this step, the gas ion source is a linear anode ion source, the working gas is argon, the voltage is adjustable in the range of 50 to 300 V, and the bombardment time is 10 to 30 minutes.

步骤S13,将非晶化后的基材送入反应腔中,采用磁控溅射方式在所述非晶氮化铝过渡层的表面沉积形成第二择优取向氮化铝涂层,所述基材以第二预设速度运动,所述第二预设速度与所述第一预设速度不相同。In step S13, the amorphized substrate is fed into a reaction chamber, and a second preferentially oriented aluminum nitride coating is deposited on the surface of the amorphous aluminum nitride transition layer by magnetron sputtering. The substrate moves at a second preset speed, which is different from the first preset speed.

进一步地,在步骤S10之前,该制备方法还包括:Furthermore, before step S10, the preparation method further comprises:

采用软接触电动叉车将基材转运至定位台架上,通过机械手自动将基材送至清洗设备中进行超声波清洗,并干燥;The substrate is transferred to the positioning stand by a soft-contact electric forklift, and the substrate is automatically sent to the cleaning equipment for ultrasonic cleaning and drying by a manipulator;

将干燥后的基材通过机械手自动转运至真空腔内,进行抽真空达到预设真空度后,持续通入工作气体;The dried substrate is automatically transferred to the vacuum chamber by a robot, and after the vacuum is evacuated to a preset vacuum degree, the working gas is continuously introduced;

需要说明的是,本步骤中,需要预先将真空腔内的真空度抽到8×10-4Pa以下,目的是尽可能减小背景残余气体对后续反应溅射过程的影响。It should be noted that in this step, the vacuum degree in the vacuum chamber needs to be evacuated to below 8×10 −4 Pa in advance, in order to minimize the influence of background residual gas on the subsequent reactive sputtering process.

采用气体离子源轰击基材表面,以对基材进行等离子体清洗。A gas ion source is used to bombard the substrate surface to perform plasma cleaning on the substrate.

需要说明的是,所用气体离子源为线性阳离子源,工作气体为氩气。离子源电压优选为800~1000V,离子源轰击时间优选为10~30min,其目的是去除基材的待镀膜区域残留的水分子膜以及有机物,起到活化基材、提高膜基结合力的作用。It should be noted that the gas ion source used is a linear cation source, and the working gas is argon. The ion source voltage is preferably 800-1000V, and the ion source bombardment time is preferably 10-30min, the purpose of which is to remove the residual water molecule film and organic matter in the substrate to be coated area, to activate the substrate and improve the film-substrate bonding force.

综合上述,本发明中,通过采用离子源轰击技术将不同择优取向的氮化铝涂层复合在同一基材上,替换单一的氧化铝涂层,实现性能的复合,以提高CVD Mask的力学性能、绝缘阻隔性和耐腐蚀性。In summary, in the present invention, aluminum nitride coatings with different preferential orientations are composited on the same substrate by adopting ion source bombardment technology to replace the single aluminum oxide coating, thereby achieving performance composite, so as to improve the mechanical properties, insulation barrier properties and corrosion resistance of the CVD Mask.

需要说明的是,本申请的制备方法可应用于不同基材的表面,并且适用于氧化铝涂层、氧化钇涂层等。It should be noted that the preparation method of the present application can be applied to the surfaces of different substrates, and is suitable for aluminum oxide coatings, yttrium oxide coatings, and the like.

下面以实施例进行具体说明:The following is a specific description with examples:

第一、预处理:First, preprocessing:

在千级无尘车间采用软接触电动叉车将CVD Mask基材转运至定位台架上,基材调整至合适位置后采用叉车将基材转运至清洗设备处;In the Class 1000 dust-free workshop, a soft-contact electric forklift is used to transfer the CVD Mask substrate to the positioning stand. After the substrate is adjusted to the appropriate position, a forklift is used to transfer the substrate to the cleaning equipment.

采用扫码器提取产品外形尺寸信息,自动化清洗及传输段根据产品尺寸信息,自适应调整机械手、提升夹具及传输轮等位置。叉车将基材提升至清洗机前段机械手抓取位置,机械手自动将基材传输至清洗设备中进行清洗,具体包括:超声波药液清洗——1道超声波漂洗——2道超声波漂洗——扫描式喷淋——洁净风切除水——真空脱水——洁净度检查;The barcode scanner is used to extract the product's external dimensions. The automated cleaning and transmission section adaptively adjusts the positions of the manipulator, lifting fixture, and transmission wheel according to the product's dimensions. The forklift lifts the substrate to the front section of the cleaning machine where the manipulator grabs it. The manipulator automatically transfers the substrate to the cleaning equipment for cleaning, which includes: ultrasonic liquid cleaning - 1 ultrasonic rinse - 2 ultrasonic rinses - scanning spray - clean air removal of water - vacuum dehydration - cleanliness inspection;

为了避免清洗后的CVD Mask基材被微小颗粒附着,该阶段转入全自动转运过程,包括:托盘接片——托盘传输——机械手抓取——基材架接收基材——基材架传输至真空腔内的清洗区域。In order to prevent the cleaned CVD Mask substrate from being attached by tiny particles, this stage is transferred to a fully automatic transfer process, including: tray connection - tray transmission - robot grabbing - substrate rack receiving substrate - substrate rack transmission to the cleaning area in the vacuum chamber.

第二、不同择优取向的氮化铝涂层制备Second, preparation of aluminum nitride coatings with different preferred orientations

第一种择优取向氮化铝涂层沉积:抽真空——气体等离子体表面清洗——颗粒物高速在线检测(≥10um)——调整溅射阴极与基材的距离为8cm,设定基材所在平动轨道移动速度为200mm/s,溅射氮化铝——氮化铝涂层厚度及温度在线监测,达到1um厚度后,转运至静放室冷却、冷却至25℃;The first type of preferentially oriented aluminum nitride coating deposition: vacuuming - gas plasma surface cleaning - high-speed online detection of particles (≥10um) - adjusting the distance between the sputtering cathode and the substrate to 8cm, setting the moving speed of the translational track where the substrate is located to 200mm/s, sputtering aluminum nitride - online monitoring of the thickness and temperature of the aluminum nitride coating, after reaching a thickness of 1um, transporting it to a static room for cooling and cooling it to 25°C;

非晶氮化铝过渡层沉积:基材由静放室传输至过渡腔室——抽真空——线性离子源低能氩离子轰击;Amorphous aluminum nitride transition layer deposition: the substrate is transferred from the static chamber to the transition chamber - vacuum pumping - linear ion source low-energy argon ion bombardment;

第二种择优取向氮化铝涂层沉积:再次送至反应腔中——调整基材架移动速度为0mm/s,其余参数保持不变,正对溅射靶沉积第二种择优取向的氮化铝涂层——静置10小时后的CVD Mask产品经过渡室转运至自动化传输段——由基材架传输至下料机械手位置——机械手抓取产品——叉车移动至固定位置接产品——机械手脱离产品,叉车接收。The second preferentially oriented aluminum nitride coating deposition: sent to the reaction chamber again - adjust the substrate rack moving speed to 0mm/s, and keep other parameters unchanged, and deposit the second preferentially oriented aluminum nitride coating facing the sputtering target - after standing for 10 hours, the CVD Mask product is transferred to the automated transmission section through the transition chamber - transferred from the substrate rack to the unloading robot position - the robot grabs the product - the forklift moves to the fixed position to receive the product - the robot detaches from the product, and the forklift receives it.

第三、出货检测Third, shipment inspection

检查sheet面是否褶皱、Cell位置精度、Sheet下垂量、边缘氮化铝涂层完整性、氮化铝涂层电阻是否达到要求,检查合格后转入氮气保护储存箱出货。Check whether the sheet surface is wrinkled, the cell position accuracy, the sheet droop, the edge aluminum nitride coating integrity, and whether the aluminum nitride coating resistance meets the requirements. After passing the inspection, transfer it into the nitrogen protection storage box for shipment.

具体的,采用中频反应磁控溅射在因瓦合金表面制备AlN薄膜,设定中频电源功率为500W,频率为20kHz,占空比为40%,通入的工作气体Ar与反应气体N2流量比值为32:12sccm,加热基材温度至200℃,在此温度下持续溅射60min。将基材运动速度作为变量,控制基材在孪生阴极溅射靶之间做往复移动,基材运动速度分别设置为0、5和200mm/s,分别进行AlN薄膜制备并命名为:AlN-0,AlN-5,AlN-20。Specifically, AlN thin film was prepared on the surface of Invar alloy by medium frequency reactive magnetron sputtering, the medium frequency power supply power was set to 500W, the frequency was set to 20kHz, the duty cycle was set to 40%, the flow ratio of the introduced working gas Ar to the reactive gas N2 was set to 32:12sccm, the substrate temperature was heated to 200℃, and sputtering was continued for 60min at this temperature. The substrate movement speed was used as a variable to control the substrate to move back and forth between the twin cathode sputtering targets. The substrate movement speed was set to 0, 5 and 200mm/s respectively, and AlN thin films were prepared and named: AlN-0, AlN-5, AlN-20.

请参阅图3,需要说明的是,晶态AlN以六方纤锌矿(hcp)为主,晶格常数hcp-AlN中存在两种类型的Al-N键:即B1型和B2型键。B1型共价键的键长为/>其形成能小于键长为/>的B2型的离子键。在hcp-AlN晶体结构中,单个Al(或N)原子同时和4个相邻的N(或Al)原子相结合形成正四面体,以B2键为共轴进一步形成原子相异的具有C3V对称的三棱柱(如4所示)。B2键的方向为c轴,当c轴垂直于基底时,AlN呈现出c轴取向,平行于基底的是紧密堆积面,如(002)面;而当c轴平行于基底时,则呈现出a轴取向,平行于基底的则是松散堆积面,如(100)面。(002)平面由B1和B2型键组成,(100)平面仅由B1型键组成。研究证实,吸附原子的动能很大程度上会影响取向的形成,且B1和B2键组合的形成需要高能量。这也是形成(002)平面需要高能量的沉积条件,而较低能量的条件则适合于(100)平面的形成的原因。Please refer to Figure 3. It should be noted that crystalline AlN is mainly hexagonal wurtzite (hcp), with a lattice constant of There are two types of Al-N bonds in hcp-AlN: B1 type and B2 type. The bond length of B1 type covalent bond is/> Its formation energy is less than the bond length / > B2 -type ionic bonds. In the hcp-AlN crystal structure, a single Al (or N) atom combines with four adjacent N (or Al) atoms to form a regular tetrahedron, and further forms a triangular prism with C3V symmetry with different atoms with the B2 bond as the coaxis (as shown in 4). The direction of the B2 bond is the c - axis. When the c-axis is perpendicular to the substrate, AlN presents a c-axis orientation, and the surface parallel to the substrate is a close-packed surface, such as the (002) surface; when the c-axis is parallel to the substrate, it presents an a-axis orientation, and the surface parallel to the substrate is a loosely packed surface, such as the (100) surface. The (002) plane is composed of B1 and B2 type bonds, and the (100) plane is composed only of B1 type bonds. Studies have confirmed that the kinetic energy of the adsorbed atoms will greatly affect the formation of the orientation, and the formation of the combination of B1 and B2 bonds requires high energy. This is also the reason why high-energy deposition conditions are required to form the (002) plane, while lower energy conditions are suitable for the formation of the (100) plane.

请参阅图4,虚线框内为AlN的衍射峰,而未被标出的衍射峰属于因瓦合金基材,框线内XRD衍射峰均与标准ICSD(00-025-1133)相匹配,表明晶体结构属于hcp-AlN,其2θ值为33.2°、36.0°、59.4°的衍射峰分别对应于(100)、(002)和(110)取向。从XRD衍射图谱中看出,当基底运动速度为200mm/s时,AlN-20在2θ=33.2°具有最高强度衍射峰,表明该薄膜择优取向为(100),属a轴取向;当运动速度下降到5mm/s时,AlN-5以(002)为择优取向,且具有一定强度的(100)衍射峰;当运动速度为0mm/s时,AlN-0以(002)为择优取向,强度较5mm/s有所提高,表明结晶度有所提高。可以看出,在制备AlN薄膜时,静止有利于(002)取向的生长,而运动速度的提高将有利于(100)取向的生长而抑制(002)取向。Please refer to Figure 4. The dotted box contains the diffraction peaks of AlN, while the unmarked diffraction peaks belong to the Invar alloy substrate. The XRD diffraction peaks in the box all match the standard ICSD (00-025-1133), indicating that the crystal structure belongs to hcp-AlN. The diffraction peaks with 2θ values of 33.2°, 36.0°, and 59.4° correspond to the (100), (002), and (110) orientations, respectively. From the XRD diffraction spectrum, it can be seen that when the substrate movement speed is 200mm/s, AlN-20 has the highest intensity diffraction peak at 2θ=33.2°, indicating that the preferred orientation of the film is (100), which belongs to the a-axis orientation; when the movement speed drops to 5mm/s, AlN-5 has a preferred orientation of (002) and a certain intensity of (100) diffraction peak; when the movement speed is 0mm/s, AlN-0 has a preferred orientation of (002), and the intensity is higher than that of 5mm/s, indicating that the crystallinity is improved. It can be seen that when preparing AlN film, stillness is conducive to the growth of (002) orientation, while the increase of movement speed will be conducive to the growth of (100) orientation and inhibit the (002) orientation.

基于XRD衍射图谱,采用Scherrer公式对所制备的AlN薄膜晶粒尺寸进行计算,得到不同转速下制备的氮化铝薄膜的晶粒尺寸计算结果,结果显示0mm/s下制备的氮化铝薄膜的晶粒尺寸为25.31nm;5mm/s下制备的氮化铝薄膜中(002)取向对应的晶粒尺寸为30.20nm,而(100)取向对应的晶粒尺寸为32.19nm;20mm/s下制备的氧化铝薄膜的晶粒尺寸为40.06nm。因此,得出结论:移动速度的提高会增大AlN薄膜的晶粒尺寸,且(002)取向的晶粒尺寸要小于(100)取向的晶粒尺寸。Based on the XRD diffraction pattern, the grain size of the prepared AlN film was calculated using the Scherrer formula, and the grain size calculation results of the aluminum nitride film prepared at different rotation speeds were obtained. The results showed that the grain size of the aluminum nitride film prepared at 0 mm/s was 25.31 nm; the grain size corresponding to the (002) orientation in the aluminum nitride film prepared at 5 mm/s was 30.20 nm, and the grain size corresponding to the (100) orientation was 32.19 nm; the grain size of the aluminum oxide film prepared at 20 mm/s was 40.06 nm. Therefore, it is concluded that the increase in the moving speed will increase the grain size of the AlN film, and the grain size of the (002) orientation is smaller than the grain size of the (100) orientation.

请参阅图5,AlN薄膜表面致密无明显的裂痕或孔隙。可以看出,随着基材运动速度的提高,所制备的氮化铝薄膜的晶粒更加粗大不均匀,200mm/s条件下氮化铝薄膜结构呈柱状晶状态,0mm/s和5mm/s条件下制备的氮化铝薄膜结构致密无明显柱状晶结构。Please refer to Figure 5, the surface of the AlN film is dense without obvious cracks or pores. It can be seen that with the increase of the substrate movement speed, the grains of the prepared aluminum nitride film become coarser and more uneven. The aluminum nitride film structure under the condition of 200mm/s is in a columnar crystal state, and the aluminum nitride film structure prepared under the conditions of 0mm/s and 5mm/s is dense without obvious columnar crystal structure.

结合XRD与SEM结果分析,以(100)为择优取向的薄膜表面的晶粒尺寸较大,截面具有较为明显的柱状晶结构;而以(002)为择优取向的薄膜表面晶粒尺寸较小,截面的柱状晶结构不明显,膜层更加致密。SEM的表征结果与基于XRD计算得出的晶粒尺寸趋势相匹配,同时表明以(002)为择优取向的AlN薄膜膜层质量相较(100)择优取向的薄膜要好。对AlN薄膜进行EDS能谱分析,得到不同运动速度下制备的氮化铝薄膜的膜层厚度和铝氮比:AlN-0,AlN-5,AlN-20的膜层厚度分别为1050、1180和1060nm,对应的沉积速率为17.5、19.7和17.7nm/min;AlN-0,AlN-5,AlN-20的铝氮原子百分比分别为48.23:51.77、51.35:48.65和50.54:49.46,表明该沉积条件所制备的AlN薄膜基本符合标准化学计量比铝氮比1:1。Combining the XRD and SEM results, the surface grain size of the film with (100) preferred orientation is larger, and the cross section has a more obvious columnar crystal structure; while the surface grain size of the film with (002) preferred orientation is smaller, the columnar crystal structure of the cross section is not obvious, and the film layer is more dense. The SEM characterization results match the grain size trend calculated based on XRD, and also show that the film quality of the AlN film with (002) preferred orientation is better than that of the film with (100) preferred orientation. EDS energy spectrum analysis was performed on the AlN film, and the film thickness and aluminum-nitrogen ratio of the aluminum nitride films prepared at different movement speeds were obtained: the film thicknesses of AlN-0, AlN-5, and AlN-20 were 1050, 1180, and 1060 nm, respectively, and the corresponding deposition rates were 17.5, 19.7, and 17.7 nm/min; the aluminum-nitrogen atomic percentages of AlN-0, AlN-5, and AlN-20 were 48.23:51.77, 51.35:48.65, and 50.54:49.46, respectively, indicating that the AlN film prepared under this deposition condition basically meets the standard stoichiometric aluminum-nitrogen ratio of 1:1.

请参阅图6,AlN薄膜作为Mask的防护涂层,良好的绝缘性能是保障其与导电玻璃接触时不发生打火击穿的重要条件,采用同心圆重锤电极测量表面电阻并转化为表面电阻率。如图6所示,AlN(100)的平均表面电阻率为2.1×1013Ω,AlN(002)为1.3×1014Ω,(002)取向平均表面电阻率是(100)取向的6.2倍,AlN薄膜的两种不同取向的相较于因瓦合金表面Al2O3的表面电阻率2×1012Ω均有数量级的提升。因瓦合金表面AlN薄膜的介电强度测试结果则表明两种择优取向的介电强度相差不大,对比因瓦合金表面Al2O3薄膜的介电强度45V/μm,AlN薄膜绝缘性能及耐击穿性能有明显提高。结果表明,(002)择优取向的AlN薄膜具有更好的绝缘性能,更适合作为绝缘屏障。Please refer to Figure 6. As the protective coating of the Mask, the good insulation performance of the AlN film is an important condition to ensure that it does not spark and break down when in contact with the conductive glass. The surface resistance is measured using a concentric hammer electrode and converted into surface resistivity. As shown in Figure 6, the average surface resistivity of AlN (100) is 2.1×10 13 Ω, and that of AlN (002) is 1.3×10 14 Ω. The average surface resistivity of the (002) orientation is 6.2 times that of the (100) orientation. The two different orientations of the AlN film are both orders of magnitude higher than the surface resistivity of 2×10 12 Ω of Al 2 O 3 on the surface of Invar alloy. The dielectric strength test results of the AlN film on the surface of Invar alloy show that the dielectric strength of the two preferred orientations is not much different. Compared with the dielectric strength of 45V/μm of the Al 2 O 3 film on the surface of Invar alloy, the insulation performance and breakdown resistance of the AlN film are significantly improved. The results show that (002) preferred oriented AlN films have better insulation properties and are more suitable as insulating barriers.

请参阅图7,测得在1mol/L的NaF溶液体系下AlN动电位极化的Tafel极化曲线,对曲线进行拟合得到腐蚀电位和腐蚀电流密度结果,结果显示因瓦合金基材的腐蚀电位Ecorr为0.2663V,腐蚀电流密度Icorr为1.62×10-9A/cm2;(100)择优取向AlN薄膜的腐蚀电位Ecorr为0.3411V,腐蚀电流密度Icorr为5.49×10-7A/cm2;(002)择优取向AlN薄膜的腐蚀电位Ecorr为0.3191V,腐蚀电流密度Icorr为1.95×10-8A/cm2;从图6中明显看出AlN薄膜的制备有效提升了因瓦合金的耐蚀性,且AlN(100)的耐蚀性能明显优于AlN(002)。通过分析拟合后的腐蚀电流密度和腐蚀电位数据结果,AlN(002)的腐蚀电流密度是AlN(100)的12倍,结果表明,(100)择优取向的AlN薄膜具有更好的耐F-腐蚀性能。Please refer to Figure 7. The Tafel polarization curve of AlN potentiodynamic polarization in 1 mol/L NaF solution system was measured, and the corrosion potential and corrosion current density results were obtained by fitting the curve. The results show that the corrosion potential E corr of the Invar alloy substrate is 0.2663V, and the corrosion current density I corr is 1.62× 10-9 A/ cm2 ; the corrosion potential E corr of the (100) preferentially oriented AlN film is 0.3411V, and the corrosion current density I corr is 5.49× 10-7 A/ cm2 ; the corrosion potential E corr of the (002) preferentially oriented AlN film is 0.3191V, and the corrosion current density I corr is 1.95× 10-8 A/ cm2 ; It can be clearly seen from Figure 6 that the preparation of AlN film effectively improves the corrosion resistance of Invar alloy, and the corrosion resistance of AlN(100) is significantly better than that of AlN(002). By analyzing the fitted corrosion current density and corrosion potential data results, the corrosion current density of AlN (002) is 12 times that of AlN (100). The results show that the (100) preferred orientation AlN film has better F - corrosion resistance.

请参阅图1,考虑到不同择优取向的AlN薄膜的性能优势侧重点有所区别,结合离子源轰击技术,在因瓦合金基材上沉积(100)和(002)择优取向的AlN复合涂层从而实现其优势性能的复合,(002)择优取向提高耐磨性能和绝缘性能,(100)择优取向提高耐腐蚀性能。Please refer to Figure 1. Considering that the performance advantages of AlN films with different preferred orientations have different focuses, combined with ion source bombardment technology, a composite AlN coating with (100) and (002) preferred orientations is deposited on an Invar alloy substrate to achieve a combination of their advantageous properties. The (002) preferred orientation improves wear resistance and insulation properties, and the (100) preferred orientation improves corrosion resistance.

请参阅图8,在本申请一优选实施方式中,在因瓦合金基材上沉积不同择优取向的AlN复合涂层的XRD衍射图谱表明该方案实现了(100)和(002)择优取向AlN薄膜在同一基体上的复合制备。Please refer to FIG8 . In a preferred embodiment of the present application, the XRD diffraction pattern of the AlN composite coating with different preferred orientations deposited on the Invar alloy substrate shows that the scheme achieves the composite preparation of (100) and (002) preferred oriented AlN films on the same substrate.

请参阅图9,在本申请另一优选实施方式中,可根据不同应用场景对AlN薄膜性能要求的不同,采用不同的复合顺序制备同时具有(100)和(002)择优取向的AlN薄膜。Please refer to FIG. 9 . In another preferred embodiment of the present application, different composite sequences may be used to prepare AlN films having both (100) and (002) preferred orientations according to different application scenarios and requirements for AlN film performance.

综上,本发明耦合并调控基底的制备参数以实现氮化铝涂层择优取向的调控,实现因瓦合金表面氮化铝涂层c轴取向和a轴取向的转换,并结合离子源轰击技术将同种材料不同择优取向的涂层复合在同一基底上,实现性能的复合,为OLED蒸镀制程中掩膜板防护涂层制备技术提供新的方案和理论指导。In summary, the present invention couples and regulates the preparation parameters of the substrate to achieve the regulation of the preferred orientation of the aluminum nitride coating, realizes the conversion of the c-axis orientation and the a-axis orientation of the aluminum nitride coating on the surface of Invar alloy, and combines the ion source bombardment technology to composite coatings of the same material with different preferred orientations on the same substrate to achieve performance composite, providing a new solution and theoretical guidance for the preparation technology of the mask protective coating in the OLED evaporation process.

本说明书中,各个实施例采用递进的方式描述,每个实施例重点说明的都是与其它实施例的不同之处,各个实施例之间相同或相似部分互相参见即可。且以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。In this specification, each embodiment is described in a progressive manner, and each embodiment focuses on the differences from other embodiments, and the same or similar parts between the embodiments can be referred to each other. The above-mentioned embodiments only express several implementation methods of the present invention, and their descriptions are relatively specific and detailed, but they cannot be understood as limiting the scope of the patent of the present invention. It should be pointed out that for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be based on the attached claims.

Claims (10)

1.一种含有不同择优取向的氮化铝涂层,成形于基材的表面,其特征在于:包括位于所述基材表面上的第一择优取向氮化铝涂层,位于所述第一择优取向氮化铝涂层表面上的非晶氮化铝过渡层,以及位于所述非晶氮化铝过渡层表面上的第二择优取向氮化铝涂层,所述第二择优取向氮化铝涂层和所述第一择优取向氮化铝涂层的择优取向不相同。1. An aluminum nitride coating containing different preferred orientations, formed on the surface of a substrate, characterized in that it includes a first preferred orientation aluminum nitride coating located on the surface of the substrate, an amorphous aluminum nitride transition layer located on the surface of the first preferred orientation aluminum nitride coating, and a second preferred orientation aluminum nitride coating located on the surface of the amorphous aluminum nitride transition layer, wherein the preferred orientations of the second preferred orientation aluminum nitride coating and the first preferred orientation aluminum nitride coating are different. 2.根据权利要求1所述的含有不同择优取向的氮化铝涂层,其特征在于,所述第一择优取向氮化铝涂层的厚度为1~3um,所述非晶氮化铝过渡层的厚度为50 ~ 200nm;所述第二择优取向氮化铝涂层的厚度为1~3um。2. The aluminum nitride coating containing different preferred orientations according to claim 1 is characterized in that the thickness of the first preferred orientation aluminum nitride coating is 1~3um, the thickness of the amorphous aluminum nitride transition layer is 50~200nm; the thickness of the second preferred orientation aluminum nitride coating is 1~3um. 3.根据权利要求1所述的含有不同择优取向的氮化铝涂层,其特征在于,该氮化铝涂层的择优取向为氧化铝晶体的首选晶面取向。3. The aluminum nitride coating with different preferred orientations according to claim 1, characterized in that the preferred orientation of the aluminum nitride coating is the preferred crystal plane orientation of the aluminum oxide crystal. 4.根据权利要求3所述的含有不同择优取向的氮化铝涂层,其特征在于,该首选晶面以纤锌矿为主要晶体结构,表现出a轴方向生长或c轴方向生长。4. The aluminum nitride coating with different preferred orientations according to claim 3 is characterized in that the preferred crystal plane has wurtzite as the main crystal structure and exhibits growth in the a-axis direction or the c-axis direction. 5.一种含有不同择优取向的氮化铝涂层的制备方法,其特征在于,包括以下步骤:5. A method for preparing an aluminum nitride coating having different preferred orientations, characterized in that it comprises the following steps: 步骤S10,将等离子体清洗后的基材送入反应腔中,采用磁控溅射方式在所述基材的表面上沉积第一择优取向氮化铝涂层,所述基材以第一预设速度运动;Step S10, placing the plasma-cleaned substrate into a reaction chamber, and depositing a first preferentially oriented aluminum nitride coating on the surface of the substrate by magnetron sputtering, with the substrate moving at a first preset speed; 步骤S11,将沉积后的基材送入静放室中,进行冷却至预设温度;Step S11, sending the deposited substrate into a static chamber to cool it to a preset temperature; 步骤S12,将冷却后的基材送入抽真空的过渡腔室内,采用气体离子源轰击所述第一择优取向氮化铝涂层,以在所述第一择优取向氮化铝涂层沉积形成非晶氮化铝过渡层;Step S12, sending the cooled substrate into a vacuum transition chamber, bombarding the first preferentially oriented aluminum nitride coating with a gas ion source, so as to deposit an amorphous aluminum nitride transition layer on the first preferentially oriented aluminum nitride coating; 步骤S13,将非晶化后的基材送入反应腔中,采用磁控溅射方式在所述非晶氮化铝过渡层的表面沉积形成第二择优取向氮化铝涂层,所述基材以第二预设速度运动,所述第二预设速度与所述第一预设速度不相同。In step S13, the amorphized substrate is fed into a reaction chamber, and a second preferentially oriented aluminum nitride coating is deposited on the surface of the amorphous aluminum nitride transition layer by magnetron sputtering. The substrate moves at a second preset speed, which is different from the first preset speed. 6.根据权利要求5所述的含有不同择优取向的氮化铝涂层的制备方法,其特征在于,在步骤S10和步骤S13中,磁控溅射所采用的电源为中频电源,电压为300 ~ 600V,工作气体为氩气,反应气体为氮气;6. The method for preparing an aluminum nitride coating having different preferred orientations according to claim 5, characterized in that, in step S10 and step S13, the power source used for magnetron sputtering is a medium frequency power source, the voltage is 300-600V, the working gas is argon, and the reaction gas is nitrogen; 在步骤S11中,预设温度为20 ~ 50℃;In step S11, the preset temperature is 20 to 50°C; 在步骤S12中,气体离子源为线性阳极离子源,工作气体为氩气,电压可调范围为50 ~300 V,轰击时间为10 ~ 30 min。In step S12, the gas ion source is a linear anode ion source, the working gas is argon, the voltage is adjustable in the range of 50 to 300 V, and the bombardment time is 10 to 30 min. 7.根据权利要求5所述的含有不同择优取向的氮化铝涂层的制备方法,其特征在于,在步骤S10中,所述基材安装在反应腔中的平动轨道上,所述平动轨道带动所述基材做往复移动;7. The method for preparing an aluminum nitride coating having different preferred orientations according to claim 5, characterized in that, in step S10, the substrate is mounted on a translation track in a reaction chamber, and the translation track drives the substrate to reciprocate; 所述平动轨道上设有对所述基材通入负偏置电压的脉冲偏压电源,和对所述基材加热的加热装置。The translation track is provided with a pulse bias power supply for applying a negative bias voltage to the substrate and a heating device for heating the substrate. 8.根据权利要求7所述的含有不同择优取向的氮化铝涂层的制备方法,其特征在于,所述脉冲偏压电源的电压范围为0 ~ 500 V,所述加热装置的加热温度范围为50 ~ 200℃,所述平动轨道的运动速度范围为0 ~ 200 mm/s。8. The method for preparing an aluminum nitride coating with different preferred orientations according to claim 7, characterized in that the voltage range of the pulse bias power supply is 0 ~ 500 V, the heating temperature range of the heating device is 50 ~ 200 ° C, and the movement speed range of the translation track is 0 ~ 200 mm/s. 9.根据权利要求5所述的含有不同择优取向的氮化铝涂层的制备方法,其特征在于,在步骤S10之前,该制备方法还包括:9. The method for preparing an aluminum nitride coating having different preferred orientations according to claim 5, characterized in that before step S10, the method further comprises: 采用软接触电动叉车将基材转运至定位台架上,通过机械手自动将基材送至清洗设备中进行超声波清洗,并干燥;The substrate is transferred to the positioning stand by a soft-contact electric forklift, and the substrate is automatically sent to the cleaning equipment for ultrasonic cleaning and drying by a manipulator; 将干燥后的基材通过机械手自动转运至真空腔内,进行抽真空达到预设真空度后,持续通入工作气体;The dried substrate is automatically transferred to the vacuum chamber by a robot, and after the vacuum is evacuated to a preset vacuum degree, the working gas is continuously introduced; 采用气体离子源轰击基材表面,以对基材进行等离子体清洗。A gas ion source is used to bombard the substrate surface to perform plasma cleaning on the substrate. 10.根据权利要求9所述的含有不同择优取向的氮化铝涂层的制备方法,其特征在于,气体离子源为线性阳极离子源,工作气体为氩气,电压可调范围为800 ~ 1000 V,轰击时间为10 ~ 30 min。10. The method for preparing an aluminum nitride coating with different preferred orientations according to claim 9, characterized in that the gas ion source is a linear anode ion source, the working gas is argon, the voltage is adjustable in the range of 800 to 1000 V, and the bombardment time is 10 to 30 min.
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