WO2016041257A1 - 膜厚传感器及其制备方法 - Google Patents

膜厚传感器及其制备方法 Download PDF

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Publication number
WO2016041257A1
WO2016041257A1 PCT/CN2014/092901 CN2014092901W WO2016041257A1 WO 2016041257 A1 WO2016041257 A1 WO 2016041257A1 CN 2014092901 W CN2014092901 W CN 2014092901W WO 2016041257 A1 WO2016041257 A1 WO 2016041257A1
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WIPO (PCT)
Prior art keywords
thickness sensor
mgo
film thickness
film
film layer
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PCT/CN2014/092901
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English (en)
French (fr)
Inventor
肖昂
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BOE Technology Group Co Ltd
Ordos Yuansheng Optoelectronics Co Ltd
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BOE Technology Group Co Ltd
Ordos Yuansheng Optoelectronics Co Ltd
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Priority to US14/769,293 priority Critical patent/US20160252347A1/en
Publication of WO2016041257A1 publication Critical patent/WO2016041257A1/zh
Anticipated expiration legal-status Critical
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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
    • G01B21/02—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness
    • G01B21/08—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness for measuring thickness
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • 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
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • 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
    • 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
    • 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
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/542—Controlling the film thickness or evaporation rate
    • C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
    • C23C14/546—Controlling the film thickness or evaporation rate using measurement on deposited material using crystal oscillators
    • 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
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment
    • C23C14/5853—Oxidation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B1/00—Measuring instruments characterised by the selection of material therefor

Definitions

  • Embodiments of the present invention relate to a film thickness sensor for vapor deposition and a method of fabricating the same.
  • a Mg/Ag alloy is generally selected as a cathode material, and the cathode material is vapor-deposited onto the substrate glass by an evaporation method.
  • a film thickness sensor is usually provided on the Mg and Ag evaporation sources.
  • the film thickness sensor selected is a quartz film thickness sensor.
  • Mg evaporation sources In general, in order to meet the needs of continuous production, two evaporation sources are usually designed in the same metal evaporation chamber, one is the main Mg evaporation source, and the other is the standby Mg evaporation source (the two evaporation sources contain two). Corresponding film thickness sensor). However, it is difficult for Mg vapor to adhere to the quartz film thickness sensor. In other words, the speed at which Mg vapor adheres to the quartz film thickness sensor is very slow. Generally, Mg vapor starts to evaporate to the film thickness sensor until its evaporation rate reaches a stable stage. It takes 1 hour, not only is it too long, it will undoubtedly cause a great waste of Mg material.
  • Embodiments of the present invention provide a film thickness sensor in which a surface of the film thickness sensor is coated with a Mg or Mg/MgO film layer.
  • the Mg or Mg/MgO film layer has a thickness of 5-10 nm.
  • the Mg or Mg/MgO film layer has a thickness of about 8 nm.
  • the thickness of the MgO film layer in the Mg/MgO film layer is 2-3 nm.
  • the thickness ratio of the Mg and MgO film layers in the Mg/MgO film layer is 1:0.25-1.5.
  • the thickness ratio of the Mg and MgO film layers is 1:0.67-1.5; or when the thickness of the Mg/MgO film layer is 8 nm, the Mg The thickness ratio of the MgO film layer is 1:0.3-0.6; or, when the thickness of the Mg/MgO film layer is 10 nm, the thickness ratio of the Mg and MgO film layers is 1:0.25-0.45.
  • Another embodiment of the present invention provides a method for fabricating a film thickness sensor, including:
  • the Mg material is evaporated on the film thickness sensor under high vacuum and anaerobic conditions at a temperature of 600-700 ° C to form a film thickness sensor of the Mg film layer;
  • the Mg material is evaporated on the film thickness sensor under high vacuum and anaerobic conditions at a temperature of 600-700 ° C to form a film thickness sensor of the Mg film layer; the film thickness sensor of the Mg film layer is continuously placed at a temperature of 30-45 ° C After 60-70 seconds in the oxygen-containing argon gas, the surface of the Mg film layer is partially oxidized to MgO to form a film thickness sensor of the Mg/MgO film layer.
  • the oxygen-containing argon has an oxygen concentration of 5-6%.
  • Embodiments of the present invention provide a film thickness sensor on which a surface of a film thickness sensor is coated with a Mg or Mg/MgO film layer.
  • the film thickness sensor provided by the embodiment of the present invention is a quartz film thickness sensor. Since the main component of quartz is silicon dioxide, it belongs to non-metallic minerals, and the vapor deposition material Mg belongs to a metal element, and the Mg has a different property, so that Mg is made. The material is difficult to adhere to the surface of the quartz film thickness sensor during vapor deposition. Under such conditions, if the stable evaporation rate of the Mg material is to be achieved, the time must be long and the Mg material is largely wasted.
  • a film of Mg or Mg/MgO (i.e., Mg layer and MgO layer) is preliminarily deposited on the surface of the quartz film thickness sensor, thus, due to the vapor deposition material Mg and Mg or Mg/MgO film.
  • the elemental properties of the layer are the same, which makes it easier for the Mg material to adhere to the Mg or Mg/MgO film layer coated on the surface of the quartz film thickness sensor during evaporation, thereby reducing the evaporation of the Mg material to its stable evaporation.
  • the time of the rate which in turn reduces the amount of Mg material that is wasted.
  • another film layer which is easy to adhere to the Mg material may be pre-evaporated on the surface of the quartz film thickness sensor, such as pre-evaporation of other element materials belonging to Group IIA of Mg, and IA. And elemental materials in the IIIA family.
  • Embodiments of the present invention provide a film thickness sensor, the main improvement of which is in the film thickness sensor
  • the surface is coated with a layer of Mg or Mg/MgO film.
  • the film thickness sensor selected is mostly a quartz film thickness sensor. Due to the difference in properties of quartz and Mg atoms, it is difficult for the vapor deposition material Mg to adhere to the quartz material.
  • the Mg/Mg/MgO film layer is preliminarily coated on the surface of the film thickness sensor, so that the vapor deposition material Mg is more easily attached to the Mg or Mg/MgO film layer, thereby not only reducing the Mg vapor. From the time of evaporation to the film thickness sensor to the time when the evaporation rate is stabilized, the waste of material caused by the Mg material before the rate stabilization phase is reached can also be avoided.
  • the Mg or Mg/MgO film layer has a thickness of 5-10 nm.
  • the surface of the film thickness sensor may be coated with a Mg film layer or a Mg/MgO film layer, but regardless of which of the above film layers, the coating thickness is 5-10 nm. This is because if the thickness of the applied film layer is larger than 10 nm, the service life of the film thickness sensor is remarkably reduced, and if the film layer thickness is less than 5 nm, it is difficult to form a uniform film layer on the film thickness sensor when the Mg material is evaporated.
  • the Mg or Mg/MgO film layer has a thickness of 8 nm.
  • the thickness of the Mg or Mg/MgO film layer is set to 8 nm, on the one hand, a uniform film layer can be formed, and on the other hand, the Mg material used can be reduced while ensuring the service life of the quartz film thickness sensor.
  • the MgO film layer in the Mg/MgO film layer has a thickness of 2-3 nm.
  • the MgO film layer in the Mg/MgO film layer is further oxidized on the basis of the Mg film layer.
  • the thickness of the MgO film layer is 2-3 nm. Oxidation on the basis of the Mg film layer to obtain the MgO film layer can facilitate the operation of the film thickness sensor attached to the Mg film layer in any environment such as production, storage, transportation, etc., without worrying that the metal Mg will be oxidized by oxygen to MgO, thereby Reduce the process complexity and production cost of the Mg film thickness sensor.
  • the thickness ratio of the Mg and MgO film layers in the Mg/MgO film layer is 1:0.25-1.5.
  • the thickness of the Mg/MgO film layer provided by the present invention is 5-10 nm, and the thickness of the formed MgO film layer is 2-3 nm, so that within this range, the Mg and MgO film layers in the Mg/MgO film layer are The thickness ratio is approximately 1:0.25-1.5.
  • the thickness ratio of the Mg and MgO film layers when the thickness of the Mg/MgO film layer is 5 nm, the thickness ratio of the Mg and MgO film layers is 1:0.67-1.5; In an embodiment, when the thickness of the Mg/MgO film layer is 8 nm, the thickness ratio of the Mg and MgO film layers is 1:0.3-0.6; in an optional embodiment of the invention, the Mg/MgO When the thickness of the film layer is 10 nm, the thickness ratio of the Mg and MgO film layers is 1:0.25-0.45.
  • the thickness ratio of the Mg/MgO film layer can not only form a uniform film layer, but also avoid the waste of the Mg material used under the premise of ensuring the service life of the quartz film thickness sensor.
  • the embodiment of the invention further provides a method for preparing a film thickness sensor as provided in the above embodiments, comprising:
  • the Mg material is evaporated on the film thickness sensor under high vacuum and anaerobic conditions at a temperature of 600-700 ° C to form a film thickness sensor of the Mg film layer;
  • the Mg material is evaporated on the film thickness sensor under high vacuum and anaerobic conditions at a temperature of 600-700 ° C to form a film thickness sensor of the Mg film layer; the film thickness sensor of the Mg film layer is continuously placed at a temperature of 30-45 ° C After 60-70 seconds in the oxygen-containing argon gas, the surface of the Mg film layer is partially oxidized to MgO to form a film thickness sensor of the Mg/MgO film layer.
  • the Mg material is evaporated on the film thickness sensor under anaerobic conditions, and the conditions are harsh, and it is required to be carried out under high vacuum and anaerobic conditions at a temperature of 600-700 ° C, wherein The high vacuum is 10-7Pa; in the process of preparing the Mg/MgO film thickness sensor, the oxidation reaction of Mg mainly occurs, and the oxidation reaction can occur at normal temperature, and the temperature is controlled to ensure the oxidation reaction occurs. In the embodiment of the invention, the temperature is set at 30-45 °C.
  • the Mg/MgO film thickness sensor is more advantageous in actual production and application than the film thickness sensor of the Mg film layer, because it is easy to operate in an environment of production, storage, transportation, etc., and the process. Both complexity and production costs are low.
  • Embodiments of the present invention provide a method for preparing a film thickness sensor, which is coated with a Mg or Mg/MgO film layer on the surface of the film thickness sensor, so that the vapor deposition material Mg is more easily attached to Mg or Mg/ On the MgO film layer, this not only reduces the time from the start of evaporation of the Mg vapor to the film thickness sensor until the evaporation rate is stabilized, but also avoids material waste caused by the Mg material before the rate stabilization phase is reached.
  • the method is simple in operation, low in production cost, and easy to be applied in the preparation of a large-scale film thickness sensor.
  • the oxygen-containing argon has an oxygen concentration of 5-6%.
  • 5-6% oxygen is mixed in the working gas argon.
  • the purpose of oxidizing the MgO film layer on the basis of the Mg film layer is to ensure that the film thickness sensor coated with the Mg material is not easily oxidized in an environment of production, storage, transportation, etc., and mainly functions as a protective layer, so that it is formed.
  • the MgO film layer does not need to be too thick, and thus the amount of oxygen mixed in the working gas argon gas may be sufficient.
  • Mg is evaporated on the film thickness sensor under high vacuum and anaerobic conditions at a temperature of 600 ° C to form a Mg-film thickness sensor;
  • the Mg-film thickness sensor was continuously placed in argon gas containing 5% oxygen at a temperature of 30 ° C for 60 seconds, the surface of the Mg film layer was partially oxidized to MgO to form a Mg/MgO-film thickness sensor 1.
  • Mg is evaporated on the film thickness sensor under high vacuum and anaerobic conditions at a temperature of 650 ° C to form a Mg-film thickness sensor;
  • the Mg-film thickness sensor was continuously placed in an argon gas containing 5.5% oxygen at a temperature of 40 ° C for 65 seconds, the surface of the Mg film layer was partially oxidized to MgO to form a Mg/MgO-film thickness sensor 2.
  • Mg is evaporated on the film thickness sensor under high vacuum and anaerobic conditions at a temperature of 700 ° C to form a Mg-film thickness sensor;
  • the Mg-film thickness sensor was continuously placed in argon gas containing 6% oxygen at a temperature of 45 ° C for 70 seconds, the surface of the Mg film layer was partially oxidized to MgO to form a Mg/MgO-film thickness sensor 3.
  • the film thickness sensor in the above Examples 1-3 and a quartz film thickness sensor (referred to as Comparative Example 1) having no Mg or MgO film layer on the surface were placed in an evaporation apparatus to carry out a Mg evaporation rate stabilization test, and the measurement was performed from the Mg material.
  • the time required to begin evaporation to the evaporation rate stabilization phase (the difference between the four test rate target values ⁇ +-3%) is shown in Table 1.
  • Example 1 Example 2
  • Example 3 Comparative example 1 needs time 17min 15min 18min 52min
  • the surface of the film thickness sensor provided by the embodiment of the present invention is coated with a Mg/MgO film layer, so that the Mg material is more easily attached to the surface of the quartz film thickness sensor during vapor deposition.
  • this not only reduces the time during which the Mg material evaporates to its stable evaporation rate, ie, from the existing 52 minutes to 15-18 minutes, but also further reduces the waste material thus lost.

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Abstract

公开了一种膜厚传感器，在所述膜厚传感器的表面上涂覆有Mg或Mg/MgO膜层，以使Mg材料易于附着在膜厚传感器上，从而避免Mg材料的浪费。

Description

膜厚传感器及其制备方法 技术领域
本发明实施例涉及一种蒸镀用膜厚传感器及其制备方法。
背景技术
在现有的OLED面板生产中，通常选用Mg/Ag合金作为阴极材料，并通过蒸镀的方法将阴极材料蒸镀到基板玻璃上。为了精确地监控蒸镀到基板上的阴极材料的膜厚度，通常会在Mg和Ag蒸发源上设有膜厚传感器，一般情况下，所选用的膜厚传感器为石英膜厚传感器。
一般来说，为了满足连续生产的需要，通常会在同一金属蒸镀腔室内设计有两个蒸发源，一个为主Mg蒸发源，另一个则为备用Mg蒸发源(两个蒸发源包含两个与之相对应的膜厚传感器)。但Mg蒸汽很难附着在石英膜厚传感器上，换言之，Mg蒸汽附着在石英膜厚传感器上的速度非常慢，通常情况下Mg蒸汽从开始蒸发到膜厚传感器上到其蒸发速率达到稳定阶段大概需要1小时，不仅时间过长，还无疑会造成Mg材料在很大程度上的浪费。
发明内容
本发明实施例提供了一种膜厚传感器，其中在所述膜厚传感器的表面上涂覆有Mg或Mg/MgO膜层。
在一个示例中，所述Mg或Mg/MgO膜层的厚度为5-10nm。例如，所述Mg或Mg/MgO膜层的厚度约为8nm。
在一个示例中，所述Mg/MgO膜层中MgO膜层的厚度为2-3nm。
在一个示例中，所述Mg/MgO膜层中Mg和MgO膜层的厚度比为1:0.25-1.5。例如，所述Mg/MgO膜层的厚度为5nm时，所述Mg和MgO膜层的厚度比为1:0.67-1.5；或者，所述Mg/MgO膜层的厚度为8nm时，所述Mg和MgO膜层的厚度比为1:0.3-0.6；或者，所述Mg/MgO膜层的厚度为10nm时，所述Mg和MgO膜层的厚度比为1:0.25-0.45。
本发明另一实施例提供了一种膜厚传感器的制备方法，包括：
在温度600-700℃的高真空无氧条件下，将Mg材料蒸镀在膜厚传感器上，形成Mg膜层膜厚传感器；或
在温度600-700℃的高真空无氧条件下，将Mg材料蒸镀在膜厚传感器上，形成Mg膜层膜厚传感器；将所述Mg膜层膜厚传感器继续放置在温度30-45℃的含氧氩气中60-70秒后，Mg膜层表面部分氧化成MgO，形成Mg/MgO膜层膜厚传感器。
在一个示例中，所述含氧氩气中氧气浓度为5-6％。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例的附图，对本发明实施例的技术方案进行清楚、完整地描述。显然，所描述的实施例是本发明的一部分实施例，而不是全部的实施例。基于所描述的本发明的实施例，本领域普通技术人员在无需创造性劳动的前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明实施例提供了一种膜厚传感器，在所述膜厚传感器的表面上涂覆有Mg或Mg/MgO膜层。
本发明实施例提供的膜厚传感器为石英膜厚传感器，由于石英的主要成分为二氧化硅，属于非金属矿物质，而蒸镀材料Mg属于金属元素，由于二者的自身属性不同，使得Mg材料在蒸镀时很难附着在石英膜厚传感器的表面上，在该条件下，如要达到Mg材料稳定的蒸发速率，则时间必定会很长，也会在很大程度上浪费Mg材料。在本实施例中，通过在石英膜厚传感器的表面上预先蒸镀一层Mg或Mg/MgO(即Mg层和MgO层)膜层，这样，由于蒸镀材料Mg与Mg或Mg/MgO膜层的元素性质一致，这就可使Mg材料在蒸镀时较容易地附着在石英膜厚传感器表面上所涂覆的Mg或Mg/MgO膜层上，从而减少Mg材料在蒸发至其稳定蒸发速率的时间，进而减少由此而浪费的Mg材料。
可以理解的是，在本发明实施例中，在石英膜厚传感器表面上还可预先蒸镀其它易于Mg材料附着的膜层，如可预先蒸镀与Mg同属ⅡA族的其它元素材料，以及ⅠA和ⅢA族中的元素材料。
本发明实施例提供了一种膜厚传感器，其主要改进点在于在膜厚传感器 的表面涂覆有Mg或Mg/MgO膜层。一般情况下所选用的膜厚传感器多为石英膜厚传感器，由于石英与Mg原子自身属性差异，使得蒸镀材料Mg很难附着在石英材料上。本发明实施例通过在膜厚传感器的表面上预先涂覆一层Mg或Mg/MgO膜层，使得蒸镀材料Mg更容易地附着在Mg或Mg/MgO膜层上，这样不仅可减少Mg蒸汽从开始蒸发到膜厚传感器上到其蒸发速率达到稳定时的时间，还可避免Mg材料在达到速率稳定阶段前造成的材料浪费。
在本发明的一实施例中，所述Mg或Mg/MgO膜层的厚度为5-10nm。在本发明实施例中，在膜厚传感器的表面上可涂覆有Mg膜层或Mg/MgO膜层，但无论是上述膜层中的哪一种，其涂覆厚度均为5-10nm。这是因为如若涂覆的膜层厚度大于10nm，会显著减少膜厚传感器的使用寿命，而如若膜层厚度小于5nm，则在Mg材料蒸发时很难在膜厚传感器上形成均一的膜层。在本发明的一优选实施例中，所述Mg或Mg/MgO膜层的厚度为8nm。将所述Mg或Mg/MgO膜层的厚度设置为8nm，一方面可形成均一的膜层，另一方面还可在保证石英膜厚传感器的使用寿命的前提下，减少所使用的Mg材料。
在本发明的另一实施例中，所述Mg/MgO膜层中MgO膜层的厚度为2-3nm。其中，Mg/MgO膜层中的MgO膜层是在Mg膜层的基础上进一步氧化得到的，在本实施例中，MgO膜层的厚度为2-3nm。在Mg膜层的基础上氧化得到MgO膜层可有利于附着有Mg膜层的膜厚传感器在生产、储存、运输等任意环境下操作，而无需担心金属Mg会被氧气氧化为MgO，从而可降低Mg膜层膜厚传感器的工艺复杂度以及生产成本。
在本发明的又一实施例中，所述Mg/MgO膜层中Mg和MgO膜层的厚度比为1:0.25-1.5。本发明所提供的Mg/MgO膜层的厚度为5-10nm，所形成的MgO膜层的厚度为2-3nm，这样，在该范围内，Mg/MgO膜层中的Mg和MgO膜层的厚度比约为1:0.25-1.5。其中，在本发明的一可选实施例中，所述Mg/MgO膜层的厚度为5nm时，所述Mg和MgO膜层的厚度比为1:0.67-1.5；在本发明的一可选实施例中，所述Mg/MgO膜层的厚度为8nm时，所述Mg和MgO膜层的厚度比为1:0.3-0.6；在本发明的一可选实施例中，所述Mg/MgO膜层的厚度为10nm时，所述Mg和MgO膜层的厚度比为1:0.25-0.45。在上述Mg/MgO膜层的厚度范围内，根据上述Mg和MgO膜层 的厚度比制备Mg/MgO膜层，不但可形成均一的膜层，还可在保证石英膜厚传感器的使用寿命的前提下，避免所使用的Mg材料浪费。
本发明实施例还提供了一种如上述实施例所提供的膜厚传感器的制备方法，包括：
在温度600-700℃的高真空无氧条件下，将Mg材料蒸镀在膜厚传感器上，形成Mg膜层膜厚传感器；或
在温度600-700℃的高真空无氧条件下，将Mg材料蒸镀在膜厚传感器上，形成Mg膜层膜厚传感器；将所述Mg膜层膜厚传感器继续放置在温度30-45℃的含氧氩气中60-70秒后，Mg膜层表面部分氧化成MgO，形成Mg/MgO膜层膜厚传感器。
在制备Mg膜层膜厚传感器的过程中，需在无氧条件下将Mg材料蒸镀在膜厚传感器上，条件较为苛刻，需在温度600-700℃的高真空无氧条件下进行，其中高真空为10-7Pa；而在制备Mg/MgO膜层膜厚传感器的过程中，主要发生的是Mg的氧化反应，该氧化反应在常温下即可发生，为了确保发生氧化反应的温度可控，本发明实施例将该温度设置在30-45℃。可以理解的是，相对于Mg膜层膜厚传感器而言，Mg/MgO膜层膜厚传感器在实际生产、应用中更具有优越性，因为其生产、储存、运输等环境中易于操作，且工艺复杂程度以及生产成本均较低。
本发明实施例提供了一种膜厚传感器的制备方法，由于该方法在膜厚传感器的表面上涂覆了Mg或Mg/MgO膜层，使得蒸镀材料Mg更容易地附着在Mg或Mg/MgO膜层上，这样不仅可减少Mg蒸汽从开始蒸发到膜厚传感器上到其蒸发速率达到稳定时的时间，还可避免Mg材料在达到速率稳定阶段前造成的材料浪费。该方法操作简单，生产成本较低，易于应用在规模化的膜厚传感器的制备中。
在本发明的一实施例中，所述含氧氩气中氧气浓度为5-6％。为了保证Mg可发生氧化反应生成MgO，在工作气体氩气中混有5-6％的氧气。由于在Mg膜层的基础上氧化形成MgO膜层的目的在于保证涂覆有Mg材料的膜厚传感器在生产、储存、运输等环境中不易被氧化，主要起到保护层的作用，所以形成的MgO膜层不需要太厚，进而在工作气体氩气中混有的氧气适量即可。
现将结合具体示例来更好地说明本发明实施例所提供的膜厚传感器。
示例1
在温度600℃的高真空无氧条件下，将Mg蒸镀在膜厚传感器上，形成Mg-膜厚传感器；
将所述Mg-膜厚传感器继续放置在温度30℃的含有5％氧气的氩气中60秒后，Mg膜层表面部分氧化成MgO，形成Mg/MgO-膜厚传感器1。
示例2
在温度650℃的高真空无氧条件下，将Mg蒸镀在膜厚传感器上，形成Mg-膜厚传感器；
将所述Mg-膜厚传感器继续放置在温度40℃的含有5.5％氧气的氩气中65秒后，Mg膜层表面部分氧化成MgO，形成Mg/MgO-膜厚传感器2。
示例3
在温度700℃的高真空无氧条件下，将Mg蒸镀在膜厚传感器上，形成Mg-膜厚传感器；
将所述Mg-膜厚传感器继续放置在温度45℃的含有6％氧气的氩气中70秒后，Mg膜层表面部分氧化成MgO，形成Mg/MgO-膜厚传感器3。
性能测试
将上述示例1-3中的膜厚传感器与表面没有Mg或MgO膜层的石英膜厚传感器(记为对比例1)放入蒸镀设备里进行Mg蒸镀速率稳定实验，并测定从Mg材料开始蒸发到其蒸发速率稳定阶段(四个测试的速率目标值相差<+-3％)所需要的时间，具体结果见表1。
表1
  示例1 示例2 示例3 对比例1
需要时间 17min 15min 18min 52min
由上述结果可明显看出，由于本发明实施例所提供的膜厚传感器的表面涂覆有Mg/MgO膜层，使得Mg材料在蒸镀时较容易地附着在石英膜厚传感器表面上的Mg/MgO膜层上，这不仅可减少Mg材料在蒸发至其稳定蒸发速率的时间，即由现有的52分钟减少至15-18分钟，还可进一步减少由此而浪费的Mg材料。
以上所述仅是本发明的示范性实施方式，而非用于限制本发明的保护范 围，本发明的保护范围由所附的权利要求确定。
本申请基于并且要求于2014年9月18日递交的中国专利申请第201410479802.5号的优先权，在此全文引用上述中国专利申请公开的内容。

Claims (10)

  1. 一种膜厚传感器，其中在所述膜厚传感器的表面上涂覆有Mg或Mg/MgO膜层。
  2. 根据权利要求1所述的膜厚传感器，其中所述Mg或Mg/MgO膜层的厚度为5-10nm。
  3. 根据权利要求2所述的膜厚传感器，其中所述Mg或Mg/MgO膜层的厚度为8nm。
  4. 根据权利要求1所述的膜厚传感器，其中所述Mg/MgO膜层中MgO膜层的厚度为2-3nm。
  5. 根据权利要求2-4任一项所述的膜厚传感器，其中所述Mg/MgO膜层中Mg和MgO膜层的厚度比为1:0.25-1.5。
  6. 根据权利要求5所述的膜厚传感器，其中所述Mg/MgO膜层的厚度为5nm时，所述Mg和MgO膜层的厚度比为1:0.67-1.5。
  7. 根据权利要求5所述的膜厚传感器，其中所述Mg/MgO膜层的厚度为8nm时，所述Mg和MgO膜层的厚度比为1:0.3-0.6。
  8. 根据权利要求5所述的膜厚传感器，其中所述Mg/MgO膜层的厚度为10nm时，所述Mg和MgO膜层的厚度比为1:0.25-0.45。
  9. 一种膜厚传感器的制备方法，包括：
    在温度600-700℃的高真空无氧条件下，将Mg材料蒸镀在膜厚传感器上，形成Mg膜层膜厚传感器；或
    在温度600-700℃的高真空无氧条件下，将Mg材料蒸镀在膜厚传感器上，形成Mg膜层膜厚传感器；将所述Mg膜层膜厚传感器继续放置在温度30-45℃的含氧氩气中60-70秒后，Mg膜层表面部分氧化成MgO，形成Mg/MgO膜层膜厚传感器。
  10. 根据权利要求9所述的制备方法，其中所述含氧氩气中氧气浓度为5-6％。
PCT/CN2014/092901 2014-09-18 2014-12-03 膜厚传感器及其制备方法 Ceased WO2016041257A1 (zh)

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