Evaporation boat and preparation method and application thereof
By introducing WB and/or W2B5 into the evaporation boat substrate and coating it with a TiAl3 coating, the problem of easy corrosion of the evaporation boat was solved, resulting in a longer service life and better wettability, and improving the stability of the evaporation process and product quality.
Patent Information
- Application Number
- CN202410657763.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-24
- Publication Date
- 2025-11-25
AI Technical Summary
In vacuum metal coating processes, evaporation boats are easily corroded by molten metal, leading to shortened service life and unstable product quality. In particular, during the vapor deposition process, the matrix components of traditional composite ceramic evaporation boats react severely with the molten metal, and the boat lubrication effect is poor.
An evaporation boat substrate containing WB and/or W2B5 is used, and a TiAl3 coating is formed on its surface to improve the substrate density and corrosion resistance, while enhancing the wettability of molten metal.
It extends the service life of the evaporation boat, improves the corrosion resistance and wettability of molten metal, reduces splashing of molten metal, and improves the quality of vapor-deposited products.
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Figure CN121006512A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of evaporation boat, in particular to an evaporation boat and a preparation method and application thereof. BACKGROUND
[0002] The statements herein are provided only to enhance understanding of the present application and are not necessarily intended to constitute the prior art.
[0003] At present, when metal evaporation (such as aluminum evaporation) is carried out by using a vacuum metal coating process, an evaporation boat is usually used as a melter for molten metal liquid. In the evaporation process, due to repeated temperature rising and falling and the erosion of the molten metal liquid to the boat body, the evaporation boat becomes a key consumable part in the evaporation process, and the performance and service life of the evaporation boat determine the quality and cost of the product. In the traditional evaporation process, there is often a problem that the evaporation boat is corroded by the molten metal liquid (such as aluminum liquid), which shortens the service life of the evaporation boat. SUMMARY
[0004] The present application provides an evaporation boat and a preparation method and application thereof, which can balance the corrosion resistance and wettability of the molten metal liquid in the evaporation process.
[0005] In order to achieve the above-mentioned purpose, the first aspect of the present application provides an evaporation boat, comprising:
[0006] an evaporation boat base; and
[0007] a coating layer covering the surface of the evaporation boat base, wherein the evaporation boat base comprises WB and / or W2B5, and the coating layer comprises TiAl3.
[0008] In some embodiments of the present application, the mass percentage content of the WB and / or W2B5 in the evaporation boat base is ω, and 0 < ω ≤ 6%.
[0009] In some embodiments of the present application, the mass percentage content of the WB and / or W2B5 in the evaporation boat base is ω, and 1% ≤ ω ≤ 5%.
[0010] In some embodiments of the present application, the evaporation boat base further comprises at least one of Si3N4, Al2O3 and Y2O3.
[0011] In some embodiments of the present application, at least one of the following conditions is met:
[0012] (1) the mass percentage content of the Si3N4 in the evaporation boat base is 2% to 4%;
[0013] (2) the mass percentage content of the Al2O3 in the evaporation boat base is 0 to 1%;
[0014] (3) the mass percentage of Y2O3 in the evaporation boat base is 0-1%.
[0015] In some embodiments of the present application, the evaporation boat base further comprises BN and TiB2, and optionally AlN.
[0016] In some embodiments of the present application, the mass percentage of BN in the evaporation boat base is 35%-40%, the mass percentage of TiB2 in the evaporation boat base is 40%-65%, and the mass percentage of AlN in the evaporation boat base is 0-20%.
[0017] In some embodiments of the present application, the thickness of the coating is 300-600 μm.
[0018] In some embodiments of the present application, the mass ratio of Al to Ti in the coating is ≥2:1.
[0019] The second aspect of the present application further provides a method for preparing an evaporation boat, comprising:
[0020] forming a coating on the surface of the evaporation boat base comprising WB and / or W2B5, and making the coating comprise TiAl3, to prepare the evaporation boat.
[0021] In some embodiments of the present application, the method for preparing the evaporation boat base comprises:
[0022] making the evaporation boat base from raw materials comprising BN powder, TiB2 powder and W powder, so that the evaporation boat base comprises the WB and / or W2B5.
[0023] In some embodiments of the present application, the mass percentage of W powder in the raw materials is σ, and 0<σ≤6%.
[0024] In some embodiments of the present application, the raw materials satisfy at least one of the following conditions:
[0025] (1) the raw materials further comprise AlN powder;
[0026] (2) the raw materials further comprise at least one of Si3N4 powder, Al2O3 powder and Y2O3 powder.
[0027] The second aspect of the present application further provides use of the evaporation boat as described in the first aspect of the present application or prepared by the method as described in the second aspect of the present application in evaporation of metal.
[0028] In some embodiments of the present application, the evaporation of metal comprises evaporation of aluminum.
[0029] The evaporation boat provided by the application contains WB and / or W2B5 in the evaporation boat base, which can improve the density of the evaporation boat base, thereby reducing the penetration of the molten metal liquid into the evaporation boat, thereby reducing the corrosion of the evaporation boat, and prolonging the service life of the evaporation boat. Meanwhile, the WB and / or W2B5 contained in the evaporation boat base can also improve the wettability of the molten metal liquid. The coating containing TiAl3 on the surface of the evaporation boat base not only can isolate the direct contact between the evaporation boat base and the molten metal liquid, but also can further improve the corrosion resistance of the evaporation boat to the molten metal liquid and the service life of the evaporation boat on the basis of WB and / or W2B5. Moreover, the coating can further improve the wettability of the evaporation boat to the molten metal liquid.
[0030] The details of one or more embodiments of the application are set forth in the accompanying drawings and the description below. Other features, objects, and advantages of the application will be apparent from the description, drawings, and claims. BRIEF DESCRIPTION OF DRAWINGS
[0031] To better describe and illustrate the embodiments or examples provided by the application, one or more drawings can be referred to. Additional details or examples used to describe the drawings should not be considered as limiting the scope of the disclosed application, the presently described embodiments or examples, and any one of the best modes of these applications currently understood. Moreover, the same reference numbers are used to represent the same components in all the drawings. In the drawings:
[0032] Figure 1 The schematic diagram of the cross-sectional structure of the evaporation boat of an embodiment of the application.
[0033] Explanation of reference signs:
[0034] 11 evaporation boat base; 12 coating. DETAILED DESCRIPTION
[0035] Some embodiments of the evaporation boat, the preparation method and the application thereof of the application are described in detail below with appropriate reference to the drawings. However, there will be cases of omission of unnecessary detailed description. For example, there will be cases of omission of detailed description of matters well known, repeated description of actually identical structures. This is to avoid the following description from becoming unnecessarily lengthy, facilitating the understanding of those skilled in the art. In addition, the drawings and the following description are provided for those skilled in the art to fully understand the application, and are not intended to limit the subject matter recited in the claims.
[0036] The "range" disclosed in this application can be defined in the form of a lower limit and an upper limit. A given range is defined by selecting a lower limit and an upper limit, which define the boundaries of a particular range. Ranges defined in this way can include or exclude endpoints; any endpoint can be independently included or excluded, and they can be combined arbitrarily, meaning any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a specific parameter, it is expected that ranges of 60-110 and 80-120 are also included. Furthermore, if minimum range values 1 and 2 are listed, and maximum range values 3, 4, and 5 are also listed, then the following ranges are all expected: 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5. In this application, unless otherwise stated, the numerical range "ab" represents a shortened representation of any combination of real numbers between a and b, where a and b are real numbers. For example, the numerical range "0-5" indicates that all real numbers between "0" and "5" have been listed in this article; "0-5" is simply a shortened representation of these numerical combinations. Furthermore, when describing a parameter as an integer ≥ 2, it is equivalent to listing integers such as 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, and 12 for that parameter. For instance, when describing a parameter as an integer selected from "2-10", it is equivalent to listing the integers 2, 3, 4, 5, 6, 7, 8, 9, and 10.
[0037] In this application, the terms "multiple" or "various" are used unless otherwise specified, referring to a quantity greater than or equal to 2. For example, "one or more" means one or more types.
[0038] Unless otherwise specified, all embodiments and optional embodiments of this application can be combined to form new technical solutions.
[0039] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment or implementation of this application. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments. The term "implementation" as used herein has a similar understanding.
[0040] Those skilled in the art can understand that the order of writing each step in the method of each embodiment or example does not mean a strict execution order and does not constitute any limitation on the implementation process. The detailed execution order of each step should be determined by its function and possible internal logic. If not specifically stated, all steps of the present application can be performed in sequence or randomly, preferably in sequence. For example, the method comprises steps (a) and (b), which means that the method can comprise steps (a) and (b) in sequence, or steps (b) and (a) in sequence. For example, the method also comprises step (c), which means that step (c) can be added to the method in any order, for example, the method can comprise steps (a), (b) and (c), or steps (a), (c) and (b), or steps (c), (a) and (b), etc.
[0041] In the present application, the open technical features or technical solutions described by "containing", "including", "comprising" and the like are not excluded from additional members unless otherwise stated. It can be considered that both the closed features or solutions composed of the listed members and the open features or solutions including additional members outside the listed members are provided. For example, A includes a1, a2 and a3, unless otherwise stated, which can also include other members or can not include additional members, which can be considered as providing the feature or solution that "A is composed of a1, a2 and a3", and also providing the feature or solution that "A not only includes a1, a2 and a3, but also includes other members". In the present application, unless otherwise stated, A (such as B) means that B is a non-limiting example of A, and it can be understood that A is not limited to B.
[0042] In the present application, "optionally", "optional" and "optional" mean that it can or can not be, that is, it can be selected from either of the two parallel solutions "yes" or "no". If there are multiple "options" in a technical solution, unless otherwise stated, and there is no contradiction or mutual restriction, each "option" is independent.
[0043] Currently, in the process of metal evaporation (such as aluminum evaporation) by vacuum metal coating, an evaporation boat is usually used as a melter for molten metal liquid. During the evaporation process, due to repeated heating and cooling and the erosion of the molten metal liquid to the boat body, it becomes a key consumable part in the evaporation process. The performance and service life of the evaporation boat determine the quality and cost of the product. Currently, commercially available evaporation boats are usually composite ceramic evaporation boats sintered by mixing two components BN / TiB2 or three components BN / TiB2 / AlN. That is, after the raw materials are prepared and purified, they are mixed uniformly, cold-pressed into a shape, and hot-pressed to form a ceramic blank, and finally machined into a specific shape of evaporation boat by milling and other machining methods.
[0044] However, in the current composite ceramic evaporation boat, the components of the evaporation boat substrate (such as BN) often react with the molten metal liquid (such as aluminum liquid) during the evaporation process, so the surface of the evaporation boat is corroded by the molten metal liquid. Moreover, the non-uniformity of surface corrosion easily leads to the non-uniformity of the temperature field, thereby further intensifying the corrosion reaction, making the surface quality of the evaporation boat poor in the later stage of use, and shortening the service life of the evaporation boat. In addition, the evaporation boat usually needs to be lubricated for the first time to improve the surface wettability, but the lubrication effect of the traditional lubrication method is poor, which is not conducive to the stable evaporation of the surface aluminum liquid in the early stage of plating, and thus will affect the product quality.
[0045] To solve the above technical problems, the present application provides an evaporation boat, which comprises an evaporation boat substrate and a coating layer on the surface of the evaporation boat substrate. In the evaporation boat, the evaporation boat substrate containing WB and / or W2B5 cooperates with the coating layer containing TiAl3 on the surface of the evaporation boat substrate, which can effectively improve the corrosion resistance of the evaporation boat to the molten metal liquid, thereby prolonging the service life of the evaporation boat, and improving the wettability of the evaporation boat to the molten metal liquid.
[0046] In a first aspect, the present application provides an evaporation boat, referring to Figure 1 which comprises an evaporation boat substrate 11 and a coating layer 12 on the surface of the evaporation boat substrate 11, wherein the evaporation boat substrate 11 contains WB and / or W2B5, and the coating layer contains TiAl3.
[0047] In the evaporation boat provided by the present application, the WB and / or W2B5 contained in the evaporation boat substrate can improve the density of the evaporation boat substrate, thereby reducing the penetration of the molten metal liquid into the evaporation boat, which is conducive to reducing the corrosion of the molten metal liquid to the evaporation boat, thereby improving the service life of the evaporation boat; at the same time, the WB and / or W2B5 contained in the evaporation boat substrate can also improve the wettability to the molten metal liquid. The coating layer containing TiAl3 on the surface of the evaporation boat substrate not only can isolate the direct contact between the evaporation boat substrate and the molten metal liquid, but also can further improve the corrosion resistance of the evaporation boat to the molten metal liquid and the service life of the evaporation boat on the basis of WB and / or W2B5; and can further improve the wettability of the evaporation boat to the molten metal liquid.
[0048] Therefore, the evaporation boat substrate containing WB and / or W2B5 cooperates with the coating layer containing TiAl3 on the surface of the evaporation boat substrate, which can effectively improve the corrosion resistance of the evaporation boat to the molten metal liquid, thereby prolonging the service life of the evaporation boat, and improving the wettability (wettability) of the evaporation boat to the molten metal liquid, so that the evaporation boat has good lubrication effect, reduces the splashing of the molten metal liquid during the evaporation process, and improves the quality of the prepared product. That is, the evaporation boat provided by the present application can take into account the corrosion resistance and wettability of the molten metal liquid during the evaporation process.
[0049] In some embodiments, the mass percentage content of WB and / or W2B5 in the evaporation boat base body is ω, 0 < ω ≤ 6%. For example, the mass percentage content can be 0.1%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, or within a range formed by any of the above values.
[0050] In some embodiments, the mass percentage content of WB and / or W2B5 in the evaporation boat base body is ω, 1% ≤ ω ≤ 5%. In this way, the density of the evaporation boat base body is further improved, and the corrosion resistance of the evaporation boat to molten metal liquid and the service life of the evaporation boat are further improved.
[0051] In some embodiments, the evaporation boat base body further comprises at least one of Si3N4, Al2O3, and Y2O3.
[0052] In some embodiments, the mass percentage content of Si3N4 in the evaporation boat base body is 2% to 4%. For example, the mass percentage content of Si3N4 can be 2%, 2.5%, 3%, 3.5%, 4%, or within a range formed by any of the above values. In this way, the corrosion resistance of the entire evaporation boat to molten metal liquid is further improved, and the service life of the evaporation boat is further improved.
[0053] In some embodiments, the mass percentage content of Al2O3 in the evaporation boat base body is 0 to 1%. For example, the mass percentage content of Al2O3 can be 0, 0.5%, 1%, or within a range formed by any of the above values. In this way, the corrosion resistance of the entire evaporation boat to molten metal liquid is further improved, and the service life of the evaporation boat is further improved.
[0054] In some embodiments, the mass percentage content of Y2O3 in the evaporation boat base body is 0 to 1%. In this way, the density of the evaporation boat base body is further improved, thereby further improving the corrosion resistance of the entire evaporation boat to molten metal liquid, and further improving the service life of the evaporation boat.
[0055] In some embodiments, the evaporation boat base body further comprises BN and TiB2, and optionally AlN.
[0056] In some embodiments, the mass percentage content of BN in the evaporation boat base body is 35% to 40%, the mass percentage content of TiB2 is 40% to 65%, and the mass percentage content of AlN is 0 to 20%.
[0057] As an example, the mass percentage of each component in the evaporation boat substrate can be measured by the following method: scraping the powder on the surface of the evaporation boat, and performing XRD (X-ray diffraction) test on the powder, so as to measure the composition and percentage of the components in the coating through the diffraction peaks and peak intensity ratio of the XRD (the test angle is 25°-80°, and the scanning rate is 10° / min).
[0058] In some embodiments, the thickness of the coating is 300-600 μm. For example, the thickness of the coating can be 300 μm, 350 μm, 400 μm, 450 μm, 500 μm, 550 μm, 600 μm, or within a range defined by any of the above values.
[0059] In some embodiments, the mass ratio of Al to Ti in the coating is ≥2:1.
[0060] Alternatively, the mass ratio of Al to Ti in the coating is 2:1-4:1. In this way, the corrosion resistance and wettability of the coating to the molten metal liquid are further improved.
[0061] As an example, the mass percentage of each component in the coating can be measured by the following method: scraping the powder on the surface of the evaporation boat, and performing XRD (X-ray diffraction) test on the powder, so as to measure the composition and percentage of the components in the coating through the diffraction peaks and peak intensity ratio of the XRD (the test angle is 25°-80°, and the scanning rate is 10° / min).
[0062] In a second aspect, the present application provides a method for preparing an evaporation boat, which can be used to prepare the evaporation boat of the first aspect of the present application, and can comprise the following steps:
[0063] S1, forming a coating on the surface of the evaporation boat substrate containing WB and / or W2B5, so that the coating contains TiAl3, and preparing the evaporation boat.
[0064] The evaporation boat substrate contains WB and / or W2B5, which can make the evaporation boat substrate have good corrosion resistance and wettability to the molten metal liquid. On this basis, the coating containing TiAl3 is further formed on the surface of the evaporation boat substrate in step S1, which can further improve the corrosion resistance and wettability of the evaporation boat to the molten metal liquid, so that the evaporation boat has good boat wetting effect, reduces the splashing of the molten metal liquid during the evaporation process, and improves the quality of the prepared product.
[0065] In some embodiments, the method for preparing the evaporation boat substrate can comprise the following steps:
[0066] S1', the raw material containing BN powder, TiB2 powder and W powder is made into the evaporation boat matrix, and WB and / or W2B5 is contained in the evaporation boat matrix.
[0067] In the above step S1', the W contained in the raw material can react with the oxide impurities in the raw material or generated in the preparation process of sintering to generate WB and / or W2B5 (reaction formula: 7W + 2B2O3 => 4WB + 3WO2), WB and / or W2B5 has excellent wettability, which can improve the wettability of the evaporation boat to the molten metal liquid and reduce the electrical property instability caused by local wettability; and the product tungsten oxide is volatile, thereby the content of boron oxide impurities in the evaporation boat can be reduced, the sintering density can be improved, the electrical property instability caused by local corrosion can be prevented, and the service life can be improved.
[0068] Compared with the WB and / or W2B5 coating layer arranged on the surface of the traditional two-component (BN / TiB2) or three-component (BN / TiB2 / AlN) composite ceramic evaporation boat, the W powder is added to the raw material to prepare the evaporation boat matrix, which not only enables the generated WB and / or W2B5 to play a role in improving wettability, but also enables the evaporation boat matrix to be densified through the reaction of W with oxide impurities (such as B2O3), and this effect is not possessed by directly arranging the WB and / or W2B5 coating layer on the surface of the traditional composite ceramic evaporation boat.
[0069] Therefore, by adding the W powder to the raw material and thereby forming WB and / or W2B5 in the prepared evaporation boat matrix, and at the same time, forming the coating layer containing TiAl3 on the surface of the evaporation boat matrix, the evaporation boat not only has improved corrosion resistance to the molten metal liquid and service life, but also has good wettability to the evaporation molten metal liquid (such as aluminum liquid). That is, the evaporation boat matrix containing WB and / or W2B5 cooperates with the coating layer containing TiAl3 on the surface, and can realize the corrosion resistance and wettability of the evaporation boat to the molten metal liquid.
[0070] In some embodiments, the method of making the raw material into the evaporation boat matrix can adopt the traditional method of preparing the evaporation boat. For example, after the raw material is prepared and purified, it is uniformly mixed, cold-pressed and formed, hot-pressed and sintered to form a ceramic blank, and the evaporation boat matrix is prepared.
[0071] As an example, the process of preparing the evaporation boat matrix by the traditional method is as follows: first, the raw materials are weighed according to the mass fraction, mixed uniformly in a mixer, and 0.2-0.4 times the mass of distilled water is added, and stirred uniformly to obtain a blank; then the blank is sent into a mold to be molded to obtain a formed body, and finally the formed body is sent to a sealed medium-frequency induction hot-pressing sintering furnace for sintering treatment to obtain the evaporation boat matrix.
[0072] The sintering process is as follows: the sintering furnace is heated, and before the temperature reaches 1200-1300℃, the sintering furnace is kept in a vacuum state; after the temperature reaches 1300-1500℃, nitrogen is filled into the sintering furnace, and the static pressure is kept at 15-18MPa; then the temperature is continuously increased to 2300-2500℃ for constant temperature sintering, and the sintering time is 1.5-2h, and the static pressure is kept at 25-30MPa during the sintering process.
[0073] In some embodiments, the method of forming the coating layer on the surface of the evaporation boat substrate is not limited, and can be selected according to actual needs. For example, the coating layer can be formed by thermal spraying, such as high-velocity oxygen fuel (HVOF) spraying or plasma arc spraying.
[0074] In some embodiments, before the coating layer is prepared, the surface of the evaporation boat substrate can be roughened to enhance the bonding force between the coating layer and the evaporation boat substrate. For example, the surface of the evaporation boat substrate can be polished with coarse sandpaper.
[0075] In some embodiments, the mass percentage of the W powder in the raw material is σ, and 0<σ≤6%. In this way, the reaction between W and oxide impurities (oxide impurities contained in the BN / TiB2 raw material or oxide impurities generated during sintering, such as B2O3) is promoted, and WB and / or W2B5 are generated.
[0076] In some embodiments, the raw material further contains AlN powder.
[0077] In some embodiments, the raw material further contains at least one of Si3N4 powder, Al2O3 powder and Y2O3 powder.
[0078] The Si3N4 and Al2O3 contained in the raw material can react with AlN and Al2O3 during the preparation of the evaporation boat substrate, so that the corrosion resistance of the entire evaporation boat to molten metal liquid is improved. The reaction equation can be shown as follows: (6-x) / 3 Si3N4 + x / 3 Al2O3 + x / 3 AlN ⇒ Si (6-x) Al x O n N (8-n) .
[0079] The Y2O3 contained in the raw material can act as a sintering aid. During the preparation of the evaporation boat substrate, the liquid phase is used to accelerate the directional arrangement and sintering of the raw material particles. During the sintering process, a low-melting-point glassy liquid phase is formed, which continuously fills the voids in the evaporation boat substrate, so as to densify the material, thereby further improving the density of the evaporation boat substrate.
[0080] It should be noted that the shape of the evaporation boat base body is not limited, and any shape can be selected according to actual needs.
[0081] In a third aspect, the application provides an application of the evaporation boat according to the first aspect of the application or prepared by the method according to the second aspect of the application in evaporation of metal.
[0082] In some embodiments, the evaporation of metal includes evaporation of aluminum.
[0083] It should be noted that the application scenario of the evaporation boat according to the first aspect of the application or prepared by the method according to the second aspect of the application is not limited, and it can be used not only in evaporation of aluminum, but also in evaporation or preparation of other metals.
[0084] Embodiments
[0085] Hereinafter, the embodiments of the application are described. The embodiments described below are exemplary and are only used to explain the application, and cannot be understood as a limitation of the application. If the technology or conditions are not indicated in the embodiments, the technology or conditions are described according to the literature in the art or according to the product manual. If the reagents or instruments are not indicated by the manufacturer, they are all conventional products that can be obtained by purchase.
[0086] Embodiment 1
[0087] (1) Preparation of evaporation boat base body
[0088] S10, according to the mass fraction of each raw material, the mass percentage of each component in the raw material is as follows: BN powder (37%), TiB2 powder (37%), AlN powder (18%), Si3N4 powder (2.8%), Al2O3 powder (0.8%), Y2O3 powder (1.2%), W powder (3.2%).
[0089] S20, the ingredients are sent into a mixer for uniform mixing, and 0.3 times the mass of the mixed material of distilled water is added, and the mixture is stirred uniformly to obtain a blank, and then the blank is sent into a mold for molding to obtain a shaped body.
[0090] S30, the shaped body is sent to a sealed medium frequency induction heat pressure sintering furnace for sintering treatment to obtain the evaporation boat base body. The sintering process is as follows: the sintering furnace is heated, before the temperature rises to 1300℃, the sintering furnace is kept in a vacuum state (vacuum degree ≥3*10 -2 Pa); after the temperature reaches 1300℃, nitrogen is filled into the sintering furnace, and the static pressure is kept at 18MPa; then the temperature is continuously raised to 2300℃ for isothermal sintering, and the sintering time is 2h, and the static pressure is kept at 30MPa during the sintering process.
[0091] (2) Preparation of coating
[0092] S10', surface roughening: the surface of the evaporation boat base was polished with coarse sandpaper.
[0093] S20', ball milling: Ti powder and Al powder (mass ratio 1:3) were taken, 30% of the total mass of Ti powder and Al powder was added as alcohol, and the mixture was ball milled at a speed of 300 rpm for 7 h.
[0094] S30', powder drying: after ball milling, the uniformly mixed suspension was dried at 100°C for 2 h;
[0095] S40', thermal spraying coating: the dried powder was sprayed on the surface of the evaporation boat base to form a TiAl3 coating with a thickness of about 300 μm using plasma arc plating technology, and an evaporation boat was prepared. The spraying method was plasma arc plating, and the process parameters were as follows: spraying current was 520 A, spraying distance was 110 mm, main gas (argon) flow rate was 45 L / min, auxiliary gas (hydrogen) flow rate was 7.5 L / min, spraying gun moving speed was 200 cm / s, carrier gas (nitrogen) flow rate was 4.5 L / min, carrier gas pressure was 0.23 MPa, and powder feeding rate was 50 g / min.
[0096] Examples 2-11
[0097] Similar to the preparation method of Example 1, the main difference is that in step S10, the mass percentage of each component in the raw material is adjusted to change the mass percentage of WB and / or W2B5 in the prepared evaporation boat base. The results are shown in Table 1 below.
[0098] Comparative Example 1
[0099] Similar to the preparation method of Example 1, the main difference is that steps S10'-S40' are omitted, i.e. the surface of the evaporation boat base is not sprayed with a coating.
[0100] Comparative Example 2
[0101] Similar to the preparation method of Example 1, the main difference is that in step S10, no W powder is added.
[0102] Comparative Example 3
[0103] Similar to the preparation method of Example 1, the main difference is that in step S20', an equal mass of Al powder is used instead of Ti powder to prepare an Al coating with the same thickness.
[0104] Comparative Example 4
[0105] Similar to the preparation method of Comparative Example 2, the main difference is that in step S20', W powder and B powder are used instead of Ti powder and Al powder, and the mass ratio of the two is 10:1, to prepare an equal-thickness coating containing (WB and / or W2B5).
[0106] Comparative Example 5
[0107] Similar to the preparation method of Comparative Example 4, the main difference is that in step S40', the thickness of the prepared coating is 200 μm; and on the surface of the coating, a layer of Al coating with a thickness of 100 μm is further sprayed.
[0108] The relevant parameters of the evaporation boats of Examples 1-11 and Comparative Examples 1-5 are shown in Table 1 below.
[0109] Table 1
[0110]
[0111] In addition, the evaporation boats obtained in Examples 1-11 and Comparative Examples 1-5 are tested for relevant performance, and the test results are shown in Table 2 below.
[0112] Test section
[0113] (1) Corrosion resistance (service life) test
[0114] The evaporation boats prepared in Examples and Comparative Examples are sequentially loaded into a CAS-PVD vacuum coating machine, and 2.4 mm aluminum wire is continuously and uniformly fed to the surface of the evaporation boat at 1 / 3 of the evaporation boat. The temperature is heated to uniformly evaporate the aluminum liquid, and the evaporation boat is used for about 10 hours. After the aluminum slag and corrosion product impurities on the surface of the evaporation boat are cleaned, the evaporation boat is continuously loaded into the machine and used under the same conditions. When the corrosion pit depth of the boat surface is >5 mm, it is determined that the longest service life of the evaporation boat has been reached.
[0115] The contact angle of the inner surface of the evaporation boat (i.e., the surface containing a single coating) is measured by a contact angle meter (model CA300) to determine the wettability.
[0116] Table 2
[0117]
[0118] Comparing Examples with Comparative Examples, it can be seen that the evaporation boats prepared in Examples have a much longer service life than Comparative Examples, and have a smaller contact angle, indicating that the evaporation boats provided by the present application can have both corrosion resistance and wettability.
[0119] The above description of each embodiment tends to emphasize the differences between each embodiment, and the same or similar parts can be referred to each other. For brevity, the same or similar parts are not described again.
[0120] Note that the present application is not limited to the above-described embodiments. The above-described embodiments are merely examples, and embodiments having substantially the same configuration, function, and effect as the technical idea of the present application are included in the technical scope of the present application. In addition, other modes constructed by combining part of the configurations of the embodiments in a manner that a person skilled in the art can think of within the scope of the gist of the present application are also included in the scope of the present application.
Claims
1. An evaporation boat, characterized in that, include: Evaporation boat substrate; and A coating applied to the surface of the evaporation boat substrate, wherein the evaporation boat substrate contains WB and / or W2B5, and the coating contains TiAl3.
2. The evaporation boat according to claim 1, characterized in that, In the evaporation boat matrix, the mass percentage of WB and / or W2B5 is ω, where 0 < ω ≤ 6%.
3. The evaporation boat according to claim 1, characterized in that, In the evaporation boat matrix, the mass percentage of WB and / or W2B5 is ω, 1%≤ω≤5%.
4. The evaporation boat according to any one of claims 1 to 3, characterized in that, The evaporation boat matrix also contains at least one of Si3N4, Al2O3 and Y2O3.
5. The evaporation boat according to claim 4, characterized in that, At least one of the following conditions must be met: (1) In the evaporation boat substrate, the mass percentage of Si3N4 is 2%~4%; (2) In the evaporation boat substrate, the mass percentage of Al2O3 is 0~1%; (3) The mass percentage of Y2O3 in the evaporation boat substrate is 0~1%.
6. The evaporation boat according to any one of claims 1 to 4, characterized in that, The evaporation boat matrix also contains BN and TiB2, and optionally AlN.
7. The evaporation boat according to claim 6, characterized in that, In the evaporation boat matrix, the mass percentage of BN is 35%~40%, the mass percentage of TiB2 is 40%~65%, and the mass percentage of AlN is 0~20%.
8. The evaporation boat according to any one of claims 1 to 3, characterized in that, The thickness of the coating is 300μm~600μm.
9. The evaporation boat according to any one of claims 1 to 3, characterized in that, In the coating, the mass ratio of Al to Ti is ≥2:
1.
10. A method for preparing an evaporation boat, characterized in that, include: The evaporation boat is prepared by forming a coating on the surface of an evaporation boat substrate containing WB and / or W2B5, wherein the coating contains TiAl3.
11. The method according to claim 10, characterized in that, The method for preparing the evaporation boat substrate includes: The evaporation boat matrix is made from raw materials containing BN powder, TiB2 powder and W powder, such that the evaporation boat matrix contains WB and / or W2B5.
12. The method according to claim 11, characterized in that, In the raw materials, the mass percentage of W powder is σ, where 0 < σ ≤ 6%.
13. The method according to claim 11 or 12, characterized in that, The raw materials satisfy at least one of the following conditions: (1) The raw materials also contain AlN powder; (2) The raw materials also include at least one of Si3N4 powder, Al2O3 powder and Y2O3 powder.
14. The use of an evaporation boat as described in any one of claims 1 to 9 or an evaporation boat prepared by the method according to any one of claims 10 to 13 in the vapor deposition of metal.
15. The application according to claim 14, characterized in that, The vapor-deposited metal includes vapor-deposited aluminum.