Evaporation boat, preparation method therefor and use thereof
By introducing a tungsten-boron binary compound into the evaporation boat substrate and forming a TiAl3 coating on the surface, 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
- PCT/CN2024/115068
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-05-24
- Filing Date
- 2024-08-28
- Publication Date
- 2025-12-26
AI Technical Summary
In the vacuum coating process, the evaporation boat is easily corroded by molten metal, resulting in a shortened service life and unstable product quality.
An evaporation boat substrate containing a tungsten-boron binary compound is used, and a TiAl3 coating is formed on its surface to improve the substrate density and corrosion resistance, while also enhancing the wettability of the 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 product quality.
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Figure CN2024115068_26122025_PF_FP_ABST
Abstract
Description
Evaporation boat and preparation method and application thereof
[0001] CROSS-REFERENCE TO RELATED APPLICATIONS
[0002] This application claims priority to Chinese Patent Application No. 202410657763.7, filed on May 24, 2024, entitled “Evaporation boat and preparation method and application thereof”, which is incorporated by reference in its entirety. TECHNICAL FIELD
[0003] The present application relates to the technical field of evaporation vessels, in particular to an evaporation boat and a preparation method and application thereof. BACKGROUND
[0004] The statements herein are provided only to complement the application and do not necessarily constitute prior art.
[0005] Currently, when metal evaporation (such as aluminum evaporation) is performed using a vacuum metal coating process, an evaporation boat is usually used as a melter for molten metal liquid. During 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 of corrosion of the evaporation boat by the molten metal liquid (such as aluminum liquid), which shortens the service life of the evaporation boat.
[0006] SUMMARY
[0007] 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.
[0008] To achieve the above-mentioned purpose, the first aspect of the present application provides an evaporation boat, comprising:
[0009] an evaporation boat base; and
[0010] a coating layer covering the surface of the evaporation boat base, wherein the evaporation boat base comprises a tungsten-boron binary compound, the tungsten-boron binary compound comprises one or both of WB and W2B5, and the coating layer comprises TiAl3.
[0011] In some embodiments of the present application, in the evaporation boat base, the mass percentage content of the tungsten-boron binary compound is ω, and 0 < ω ≤ 6%.
[0012] In some embodiments of the present application, in the evaporation boat base, the mass percentage content of the tungsten-boron binary compound is ω, and 1% ≤ ω ≤ 5%.
[0013] In some embodiments of the present application, the evaporation boat base further comprises one or more of Si3N4, Al2O3 and Y2O3.
[0014] In some embodiments of the present application, one or more of the following conditions is met:
[0015] (1) the mass percentage of Si3N4 in the evaporation boat base is 2% to 4%;
[0016] (2) the mass percentage of Al2O3 in the evaporation boat base is 0 to 1%;
[0017] (3) the mass percentage of Y2O3 in the evaporation boat base is 0 to 1%.
[0018] In some embodiments of the present application, the evaporation boat base further comprises BN and TiB2, and optionally AlN.
[0019] In some embodiments of the present application, the mass percentage of BN in the evaporation boat base is 35% to 40%, the mass percentage of TiB2 is 40% to 65%, and the mass percentage of AlN is 0 to 20%.
[0020] In some embodiments of the present application, the thickness of the coating is 300 microns (μm) to 600 μm.
[0021] In some embodiments of the present application, the mass ratio of Al to Ti in the coating is ≥ 2:1.
[0022] The second aspect of the present application also provides a method for preparing an evaporation boat, comprising:
[0023] forming a coating on the surface of an evaporation boat base comprising a tungsten-boron binary compound, so that the coating comprises TiAl3, thereby preparing the evaporation boat, wherein the tungsten-boron binary compound comprises one or both of WB and W2B5.
[0024] In some embodiments of the present application, the method for preparing the evaporation boat base comprises:
[0025] preparing the evaporation boat base from raw materials comprising BN powder, TiB2 powder, and W powder, so that the evaporation boat base comprises the tungsten-boron binary compound.
[0026] In some embodiments of the present application, the mass percentage of W powder in the raw materials is σ, and 0 < σ ≤ 6%.
[0027] In some embodiments of the present application, one or more of the following conditions is met:
[0028] (1) the raw materials further comprise AlN powder;
[0029] (2) the raw material further comprises one or more of Si3N4 powder, Al2O3 powder and Y2O3 powder.
[0030] The second aspect of the present application also provides a 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 evaporating a metal.
[0031] In some embodiments of the present application, the evaporated metal comprises aluminum.
[0032] The evaporation boat provided by the present application contains tungsten boride binary compounds in the evaporation boat substrate, which can improve the density of the evaporation boat substrate, 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. At the same time, the tungsten boride binary compounds contained in the evaporation boat substrate can also improve the wettability of the molten metal liquid. The coating 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 the tungsten boride binary compounds. Moreover, it can further improve the wettability of the evaporation boat to the molten metal liquid.
[0033] The details of one or more embodiments of the present application are presented in the following drawings and description. Other features, objects, and advantages of the present application will become apparent from the description, drawings, and claims. BRIEF DESCRIPTION OF DRAWINGS
[0034] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required to be used in the embodiments of the present application will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application, and other drawings can also be obtained according to the drawings without creative labor for those skilled in the art. In the drawings:
[0035] FIG. 1 is a schematic view of the cross-sectional structure of the evaporation boat according to an embodiment of the present application.
[0036] Reference signs: 11, evaporation boat substrate; 12, coating. DETAILED DESCRIPTION
[0037] Hereinafter, some embodiments of the evaporation boat of the present application, the method for producing the same, and the use thereof will be described in detail with appropriate reference to the accompanying drawings. However, there will be cases where unnecessary detailed description is omitted. For example, there will be cases of omitting detailed description of matters known to those skilled in the art, and repeated description of substantially identical configurations. This is to avoid the following description from becoming unnecessarily lengthy and to facilitate understanding by those skilled in the art. Furthermore, the accompanying drawings and the following description are provided to enable those skilled in the art to fully understand the present application, and are not intended to limit the subject matter recited in the claims.
[0038] "Ranges" disclosed herein can be defined, with respect to a minimum and maximum, by selecting a minimum and a maximum, the selected minimum and maximum defining the boundaries of a particular range. Ranges defined in this way can be inclusive or exclusive of the endpoints, either endpoint can be included or excluded independently, and can be combined in any manner, i.e., any minimum can be combined with any maximum to form a range. For example, if ranges of 60-120 and 80-110 are listed for a particular parameter, it is understood that ranges of 60-110 and 80-120 are also contemplated. Furthermore, if a minimum range value of 1 and 2 are listed, and if a maximum range value of 3, 4, and 5 is also listed, then the following ranges are all contemplated: 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5. In the present application, unless otherwise stated, a numerical range "a-b" indicates a shorthand way of describing each and every intervening real number, a and b being real numbers. For example, the numerical range "0-5" indicates that all real numbers between "0-5" have been listed herein, "0-5" being a shorthand way of describing these numerical combinations. Also, when it is stated that a parameter is an integer ≥ 2, it is equivalent to listing the parameter as, for example, integer 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc. For example, when it is stated that a parameter is an integer selected from "2-10", it is equivalent to listing the integers 2, 3, 4, 5, 6, 7, 8, 9, and 10.
[0039] In the present application, "a plurality of", "a plurality of kinds", and the like, unless otherwise specified, mean greater than or equal to 2 in number. For example, "one or more" means one or more than or equal to two.
[0040] All embodiments and optional embodiments of the present application can be combined with each other to form new technical solutions, if not otherwise specified.
[0041] Reference to "an embodiment" herein means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment or implementation of the application. The appearances of the phrase "in an embodiment" or "in implementations" in various places in the specification are not necessarily all referring to the same embodiment, nor are they necessarily mutually exclusive of one another. Those skilled in the art will appreciate that embodiments described herein can be combined with other embodiments unless otherwise specified. Reference to "implementations" herein has a similar understanding.
[0042] Those skilled in the art can understand that, in the method of each implementation or embodiment, the writing order of each step 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 application can be performed in sequence or randomly, preferably in sequence. For example, the method includes steps (a) and (b), which means that the method can include steps (a) and (b) performed in sequence, or steps (b) and (a) performed in sequence. For example, the method also includes step (c), which means that step (c) can be added to the method in any order, for example, the method can include steps (a), (b) and (c), or steps (a), (c) and (b), or steps (c), (a) and (b), etc.
[0043] In the present application, the open technical features or technical solutions described by the words "containing", "including", "comprising" and the like, if not otherwise specified, do not exclude additional members from the listed members, which can be regarded as providing both a closed feature or solution composed of the listed members, and an open feature or solution including additional members in addition to the listed members. For example, A includes a1, a2 and a3, if not otherwise specified, it can also include other members, or it can not include additional members, which can be regarded as providing the feature or solution that "A is composed of a1, a2 and a3", and also providing the feature or solution that "A includes a1, a2 and a3, and also includes other members". In the present application, if not otherwise specified, 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.
[0044] In the present application, "optionally", "optional" and "optional" mean that it can or can not be present, that is, it means to choose from either of the two parallel solutions "have" or "have not". If there are multiple "options" in a technical solution, if not otherwise specified, and there is no contradictory relationship or mutual restriction, each "option" is independent.
[0045] At present, in the process of metal evaporation (such as aluminum evaporation) by vacuum coating metal, the evaporation boat is usually used as a melter for molten metal liquid. During the evaporation process, due to repeated temperature rise and fall and the erosion of molten metal liquid to the boat body, the evaporation boat 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. At present, the commercially available evaporation boat is usually a composite ceramic evaporation boat sintered by mixing two components BN and TiB2 or three components BN, TiB2 and AlN. That is, after the raw materials are prepared and purified, they are mixed uniformly, cold-pressed into a shape, and sintered by hot pressing to form a ceramic blank. Finally, the evaporation boat with a specific shape is machined by milling and the like.
[0046] 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 temperature field, thereby further intensifying the corrosion reaction, so that the surface quality of the evaporation boat is poor in the later stage of use, and the service life of the evaporation boat is shortened. In addition, the evaporation boat usually needs to be lubricated to improve the surface wettability when it is used for the first time, 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 initial stage of coating, and thus affects the product quality.
[0047] 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 a tungsten-boron binary compound cooperates with the coating layer containing TiAl3 on the surface to effectively improve the corrosion resistance of the evaporation boat to the molten metal liquid, thereby prolonging the service life of the evaporation boat, and the wettability of the evaporation boat to the molten metal liquid.
[0048] In a first aspect, the present application provides an evaporation boat, as shown in FIG. 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 a tungsten-boron binary compound, the tungsten-boron binary compound includes one or both of WB and W2B5, and the coating layer contains TiAl3.
[0049] The evaporation boat provided by the present application contains tungsten-boron binary compounds 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, thus reducing the corrosion of the evaporation boat by the molten metal liquid and prolonging the service life of the evaporation boat. Meanwhile, the tungsten-boron binary compounds 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 evaporation boat base from direct contact with 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 the tungsten-boron binary compounds. Moreover, the coating can further improve the wettability of the evaporation boat to the molten metal liquid.
[0050] Therefore, the evaporation boat containing tungsten-boron binary compounds in the evaporation boat base cooperates with the coating containing TiAl3 on the surface of the evaporation boat base, which can effectively improve the corrosion resistance of the evaporation boat to the molten metal liquid, prolong the service life of the evaporation boat, and improve the wettability of the evaporation boat to the molten metal liquid, so that the evaporation boat has good wettability, reduces the splashing of the molten metal liquid in the evaporation process, and improves the quality of the prepared product. That is, the evaporation boat provided by the present application can balance the corrosion resistance and wettability of the evaporation boat to the molten metal liquid in the evaporation process.
[0051] In some embodiments, the mass percentage content of the tungsten-boron binary compounds in the evaporation boat base is ω, and 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 consisting of any of the above values.
[0052] In some embodiments, the mass percentage content of the tungsten-boron binary compounds in the evaporation boat base is ω, and 1% ≤ ω ≤ 5%. Therefore, the density of the evaporation boat base can be further improved, and the corrosion resistance of the evaporation boat to the molten metal liquid and the service life of the evaporation boat can be further improved.
[0053] In some embodiments, the evaporation boat base further contains one or more of Si3N4, Al2O3, and Y2O3.
[0054] In some embodiments, the mass percentage content of Si3N4 in the evaporation boat base 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 consisting of any of the above values. Therefore, the corrosion resistance of the entire evaporation boat to the molten metal liquid can be further improved, and the service life of the evaporation boat can be further improved.
[0055] In some embodiments, the Al2O3 has a mass percentage content of 0 to 1% in the evaporation boat base. For example, the mass percentage content of Al2O3 can be 0%, 0.5%, 1%, or within a range defined by any of the above values. Alternatively, the mass percentage content of Al2O3 is greater than 0 and not more than 1%. 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.
[0056] In some embodiments, the Y2O3 has a mass percentage content of 0 to 1% in the evaporation boat base. For example, the mass percentage content of Y2O3 can be 0%, 0.5%, 1%, or within a range defined by any of the above values. Alternatively, the mass percentage content of Y2O3 is greater than 0 and not more than 1%. In this way, the density of the evaporation boat base 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.
[0057] In some embodiments, the evaporation boat base further comprises BN and TiB2, and optionally AlN.
[0058] In some embodiments, the BN has a mass percentage content of 35% to 40% in the evaporation boat base. For example, the mass percentage content of BN can be 35%, 37%, 39%, 40%, or within a range defined by any of the above values.
[0059] In some embodiments, the TiB2 has a mass percentage content of 40% to 65% in the evaporation boat base. For example, the mass percentage content of TiB2 can be 40%, 45%, 50%, 55%, 60%, 65%, or within a range defined by any of the above values.
[0060] In some embodiments, the AlN has a mass percentage content of 0 to 20% in the evaporation boat base. For example, the mass percentage content of AlN can be 0%, 5%, 10%, 15%, 20%, or within a range defined by any of the above values. Alternatively, the mass percentage content of AlN is greater than 0 and not more than 20%.
[0061] For example, the mass percentage content of each component in the evaporation boat base can be measured by the following method: the powder of the evaporation boat is scraped and coated, and the XRD (X-ray diffraction) test is performed on the powder, so that the composition and percentage content of the substances in the coating can be measured by the diffraction peaks and peak intensity ratio of the XRD (the test angle is 25° to 80°, and the scanning rate is 10° / min).
[0062] In some embodiments, the coating has a thickness of 300-600 μm. For example, the coating can have a thickness of 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.
[0063] In some embodiments, the mass ratio of Al to Ti in the coating is ≥ 2:1.
[0064] Alternatively, the mass ratio of Al to Ti in the coating is 2:1-4:1. For example, the mass ratio of Al to Ti can be 2:1, 2.5:1, 3:1, 3.5:1, 4:1 or within a range defined by any of the above values. In this way, the corrosion resistance of the coating to molten metal and the wettability of the coating to molten metal are further improved.
[0065] For example, the mass percentage of the components in the coating can be measured by scraping the powder on the surface of the evaporation boat and testing the powder by XRD (X-ray diffraction). The composition and percentage of the components in the coating can be determined by the diffraction peaks and peak intensity ratio of the XRD (the testing angle is 25-80° and the scanning rate is 10° / min).
[0066] 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. The method can comprise the following steps:
[0067] S1, forming a coating on the surface of the evaporation boat body comprising a tungsten-boron binary compound, so that the coating comprises TiAl3, thereby preparing the evaporation boat, wherein the tungsten-boron binary compound comprises one or both of WB and W2B5.
[0068] The evaporation boat body comprising a tungsten-boron binary compound can provide good corrosion resistance and wettability of the evaporation boat to molten metal. On this basis, the coating comprising TiAl3 is further formed on the surface of the evaporation boat body in step S1, which can further improve the corrosion resistance of the evaporation boat to molten metal and the wettability of the evaporation boat to molten metal, so that the evaporation boat has good boat wetting effect, reduces the splashing of molten metal during the evaporation process, and improves the quality of the prepared product.
[0069] In some embodiments, the method for preparing the evaporation boat body can comprise the following steps:
[0070] S1', preparing the evaporation boat body from raw materials comprising BN powder, TiB2 powder and W powder, so that the evaporation boat body comprises a tungsten-boron binary compound.
[0071] In the step S1', the W contained in the raw material can react with the oxide impurities in the raw material or generated during the preparation of the sintering process to form a tungsten boride binary compound (reaction formula as ), which has excellent wettability and can improve the wettability of the evaporation boat to the molten metal liquid, reduce the electrical performance instability caused by local wettability; and the product tungsten oxide is easy to volatilize, thereby reducing the content of boron oxide impurities in the evaporation boat, improving the sintering density, preventing the electrical performance instability caused by local corrosion, and improving the service life.
[0072] It can be understood that the tungsten boride binary compound generated by the reaction in the present application can contain both WB and W2B5, and WB and W2B5 can exist in any mass ratio in the tungsten boride binary compound.
[0073] Compared with the tungsten boride binary compound coating arranged on the surface of the traditional two-component (BN and TiB2) or three-component (BN, TiB2 and AlN) composite ceramic evaporation boat, the W powder is added to the raw material to prepare the evaporation boat substrate, which not only enables the generated tungsten boride binary compound to play a role in improving the wettability, but also enables the evaporation boat substrate to be densified through the reaction of W with oxide impurities (such as B2O3), and this effect is not possessed by directly arranging the tungsten boride binary compound coating on the surface of the traditional composite ceramic evaporation boat.
[0074] In this way, the present application adds W powder to the raw material, and thereby forms a tungsten boride binary compound in the prepared evaporation boat substrate, and at the same time, forms a coating containing TiAl3 on the surface of the evaporation boat substrate, which not only improves the corrosion resistance of the evaporation boat to the molten metal liquid and the service life of the evaporation boat, but also enables the evaporation boat to have good wettability to the evaporated molten metal liquid (such as aluminum liquid). That is, the evaporation boat substrate containing the tungsten boride binary compound cooperates with the coating containing TiAl3 on the surface of the evaporation boat, which can realize the corrosion resistance and wettability of the evaporation boat to the molten metal liquid.
[0075] In some embodiments, the method of preparing the raw material into the evaporation boat substrate can adopt the traditional method of preparing the evaporation boat. For example, after the raw material is prepared and purified, it is mixed uniformly, cold-pressed and formed, hot-pressed and sintered to form a ceramic substrate, and the evaporation boat substrate is prepared.
[0076] As an example, the process of preparing the evaporation boat substrate 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 to 0.4 times the mass of distilled water is added, and stirred uniformly to obtain a green body; then the green body is sent into a mold to be molded to obtain a shaped body, and finally the shaped body is sent to a sealed medium-frequency induction hot-pressing sintering furnace for sintering treatment to obtain the evaporation boat substrate.
[0077] The sintering process is as follows: the sintering furnace is heated, and before the temperature reaches 1200-1300 degrees Celsius (℃), 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 15-18 megapascals (MPa); then the temperature is continuously raised to 2300-2500℃ for isothermal sintering, and the sintering time is 1.5-2 hours (h), and the static pressure is kept at 25-30 MPa during sintering.
[0078] 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.
[0079] 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.
[0080] In some embodiments, the mass percentage of the W powder in the raw material is σ, and 0<σ≤6%. For example, σ can be 0%, 1%, 2%, 3%, 4%, 5%, 6%, or within a range formed by any of the above values. Alternatively, σ is greater than 0 and does not exceed 6%. In this way, the reaction of W with oxide impurities (which can be oxide impurities contained in the BN or TiB2 raw material or oxide impurities generated during sintering, such as B2O3) is facilitated, and the generation of tungsten boron binary compounds is facilitated.
[0081] In some embodiments, the raw material further comprises AlN powder.
[0082] In some embodiments, the raw material further comprises one or more of Si3N4 powder, Al2O3 powder, and Y2O3 powder.
[0083] The Si3N4 and Al2O3 in the raw material can react with AlN and Al2O3 during the preparation of the evaporation boat substrate, thereby improving the corrosion resistance of the entire evaporation boat to molten metal liquid. The reaction equation can be shown as follows:
[0084] 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 reaction raw material particles, and a low-melting-point glassy liquid phase is formed during sintering, which continuously fills the voids in the evaporation boat substrate, thereby densifying the material and further improving the density of the evaporation boat substrate.
[0085] 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.
[0086] In a third aspect, the application provides an application of the evaporation boat of the first aspect of the application or the evaporation boat prepared by the method of the second aspect of the application in evaporation of metal.
[0087] In some embodiments, the evaporation of metal includes evaporation of aluminum.
[0088] It should be noted that the application scenario of the evaporation boat provided by the first aspect of the application or the evaporation boat prepared by the method of the second aspect of the application is not limited, and it can not only be used in evaporation of aluminum, but also be applied to evaporation or preparation of other metals.
[0089] Embodiments
[0090] 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 described in the literature in the art or according to the product manual are used. If the reagents or instruments are not indicated by the manufacturer, they are all conventional products that can be obtained by market purchase.
[0091] Embodiment 1
[0092] (1) Preparation of evaporation boat base body
[0093] 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%).
[0094] 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.
[0095] S30, the shaped body is sent to a sealed medium frequency induction heat pressure sintering furnace for sintering treatment to prepare an evaporation boat base body containing a tungsten-boron binary compound, which includes one or both of WB and W2B5. The sintering process is as follows: the sintering furnace is heated, and before the temperature rises to 1300℃, the sintering furnace is kept in a vacuum state (vacuum degree ≥3×10 -2Pa) ; after the temperature reaches 1300 DEG C, nitrogen is filled into the sintering furnace, and the static pressure is kept at 18 MPa; then the temperature is continuously increased to 2300 DEG C for isothermal sintering, and the sintering time is 2 h, and the static pressure is kept at 30 MPa during the sintering process.
[0096] (2) Preparation of the coating
[0097] S10', surface roughening: the surface of the evaporation boat base is polished by using coarse sandpaper.
[0098] S20', ball milling of ingredients: Ti powder and Al powder (mass ratio of 1:3) are taken, 30% of the total mass of the Ti powder and Al powder is added as alcohol, and the mixture is loaded into a ball mill for ball milling, the ball milling speed is 300 revolutions per minute (rpm), and the ball milling time is 7 h.
[0099] S30', drying of the powder: after the ball milling is completed, the uniformly mixed suspension is dried at 100 DEG C for 2 h;
[0100] S40', thermal spraying coating: the dried powder is sprayed on the surface of the evaporation boat base to form a TiAl3 coating with a thickness of about 300 microns by using plasma arc plating technology, and the evaporation boat is prepared. The spraying mode is plasma arc plating, and the process parameters are as follows: the spraying current is 520 amperes (A), the spraying distance is 110 millimeters (mm), the main gas (argon) flow rate is 45 liters per minute (L / min), the auxiliary gas (hydrogen) flow rate is 7.5 L / min, the spraying gun moving speed is 200 centimeters per second (cm / s), the carrier gas (nitrogen) flow rate is 4.5 L / min, the carrier gas pressure is 0.23 MPa, and the powder feeding rate is 50 grams per minute (g / min).
[0101] Examples 2 to 11
[0102] Similar to the preparation method of Example 1, the main difference is that in step S10, the mass percentage of the tungsten-boron binary compound in the prepared evaporation boat base is changed by adjusting the mass percentage of each component in the raw material, and the results are shown in Table 1 below.
[0103] Comparative Example 1
[0104] Similar to the preparation method of Example 1, the main difference is that steps S10' to S40' are omitted, i.e., the surface of the evaporation boat base is not sprayed with a coating.
[0105] Comparative Example 2
[0106] Similar to the preparation method of Example 1, the main difference is that in step S10, no W powder is added.
[0107] Comparative Example 3
[0108] Similar to the preparation method of Example 1, the main difference is that in step S20', equal mass of Al powder is used to replace Ti powder to prepare an Al coating with equal thickness.
[0109] Comparative Example 4
[0110] Similar to the preparation method of Comparative Example 2, the main difference is that in step S20', W powder and B powder are used to replace Ti powder and Al powder, and the mass ratio of the two is 10:1, to prepare a coating containing tungsten boron binary compound with equal thickness.
[0111] Comparative Example 5
[0112] 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.
[0113] The relevant parameters of the evaporation boat of Examples 1 to 11 and Comparative Examples 1 to 5 are shown in Table 1 below.
[0114] Table 1
[0115] In addition, the evaporation boats obtained in Examples 1 to 11 and Comparative Examples 1 to 5 are subjected to relevant performance tests, and the test results are shown in Table 2 below.
[0116] Test Part
[0117] (1) Corrosion resistance (service life) test
[0118] The evaporation boats prepared in Examples and Comparative Examples are sequentially loaded into a CAS-PVD vacuum coating machine, 2.4 millimeters (mm) of aluminum wire is continuously and uniformly fed to 1 / 3 of the surface of the evaporation boat, the temperature is heated to uniformly evaporate the aluminum liquid, and the evaporation boat is used for about 10 hours of coating, then the evaporation boat is unloaded, the surface aluminum slag and corrosion product impurities are cleaned, and the evaporation boat is continuously loaded 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.
[0119] (2) Wettability test
[0120] The contact angle of the inner surface of the evaporation boat (i.e. the surface containing a single coating) is tested by a contact angle measuring instrument (model CA300) to determine the wettability.
[0121] Table 2
[0122] It can be seen from the comparison of the examples with the comparative examples that the evaporation boat prepared in the examples has a service life much higher than that of the comparative examples, and the contact angle is smaller, which shows that the evaporation boat provided in the application can balance corrosion resistance and wettability.
[0123] The above description of various embodiments tends to emphasize the differences between various embodiments, and the same or similar parts can be referred to each other, and for the sake of brevity, will not be repeated here.
[0124] It should be noted that the present application is not limited to the above-mentioned embodiments. The above-mentioned embodiments are only examples, and embodiments having substantially the same configuration and playing the same role and effect as the technical idea within the scope of the technical solution of the present application are all included in the technical scope of the present application. In addition, within the scope of the gist of the present application, various modifications that can be thought of by those skilled in the art, other modes constructed by combining part of the elements of the embodiments are also included in the scope of the present application.
Claims
1. An evaporation boat comprising: an evaporation boat base; and a coating layer on a surface of the evaporation boat base, wherein the evaporation boat base comprises a tungsten-boron binary compound, the tungsten-boron binary compound comprises one or both of WB and W2B5, and the coating layer comprises TiAl3. The mass percentage of the tungsten-boron binary compound in the evaporation boat base is ω, and 0 < ω ≤ 6%.
2. The evaporation boat according to claim 1, wherein The mass percentage of the tungsten-boron binary compound in the evaporation boat base is ω, and 1% < ω ≤ 5%.
3. The evaporation boat according to claim 1 or 2, wherein The evaporation boat base further comprises one or more of Si3N4, Al2O3 and Y2O3.
4. The evaporation boat according to any one of claims 1 to 3, wherein One or more of the following conditions are satisfied:
5. The evaporation boat according to claim 4, wherein (1) the mass percentage of Si3N4 in the evaporation boat base is 2% to 4%; (2) the mass percentage of Al2O3 in the evaporation boat base is 0 to 1%; (3) the mass percentage of Y2O3 in the evaporation boat base is 0 to 1%. The evaporation boat base further comprises BN and TiB2, and optionally AlN.
6. The vaporization boat according to any one of claims 1 to 5, wherein, The mass percentage of BN in the evaporation boat base is 35% to 40%, the mass percentage of TiB2 in the evaporation boat base is 40% to 65%, and the mass percentage of AlN in the evaporation boat base is 0 to 20%.
7. The evaporation boat according to claim 6, wherein The thickness of the coating layer is 300 μm to 600 μm.
8. The vaporization boat according to any one of claims 1 to 7, wherein, The mass ratio of Al to Ti in the coating layer is ≥ 2:
1.
9. The vaporization boat according to any one of claims 1 to 8, wherein, 10. A method for preparing an evaporation boat, comprising: forming a coating layer on a surface of an evaporation boat base comprising a tungsten-boron binary compound, so that the coating layer comprises TiAl3, to prepare the evaporation boat, wherein the tungsten-boron binary compound comprises one or both of WB and W2B5. The method for preparing the evaporation boat base comprises:
11. The method of claim 10, wherein, preparing the evaporation boat base from raw materials comprising BN powder, TiB2 powder and W powder, so that the evaporation boat base comprises the tungsten-boron binary compound. The mass percentage of the W powder in the raw materials is σ, and 0 < σ ≤ 6%.
12. The method of claim 11, wherein, The raw materials satisfy one or more of the following conditions:
13. The method of claim 11 or 12, wherein, (1) the raw materials further comprise AlN powder; (2) the raw materials further comprise one or more of Si3N4 powder, Al2O3 powder and Y2O3 powder.
14. Use of the evaporation boat according to any one of claims 1 to 9 or prepared by the method according to any one of claims 10 to 13 in evaporation of a metal. The metal to be evaporated comprises aluminum.
15. Use according to claim 14, wherein,