CN115974589A - Composite burning bearing plate and preparation method thereof - Google Patents
Composite burning bearing plate and preparation method thereof Download PDFInfo
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- CN115974589A CN115974589A CN202211519833.XA CN202211519833A CN115974589A CN 115974589 A CN115974589 A CN 115974589A CN 202211519833 A CN202211519833 A CN 202211519833A CN 115974589 A CN115974589 A CN 115974589A
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Abstract
The embodiment of the application discloses a composite setter plate and a preparation method thereof; the composite setter plate comprises a ceramic substrate and a coating arranged on at least one side of the ceramic substrate, wherein the coating is formed by coating in a plasma thermal spraying manner; the coating comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria. The composite setter plate provided by the embodiment of the application has the advantages that the bonding strength between the coating and the ceramic substrate is high, the surface of the whole composite setter plate is compact, the high-temperature stability is good, the composite setter plate is particularly suitable for being applied to high-temperature sintering of titanium products, and the coating is not easy to generate chemical reaction of titanium alloy.
Description
Technical Field
The application relates to the technical field of ceramic material production and processing, in particular to a composite setter plate and a preparation method thereof.
Background
Metal powder injection molding (MIM) titanium alloy products are finding increasingly wider applications in the fields of consumer electronics, automotive industry, and medical hygiene. Sintering is an important process in the metal powder injection molding process, and plays a decisive role in the organization, the densification performance and the chemical property uniformity of products.
For common stainless steel parts, the traditional alumina or corundum-mullite material is usually used as a burning bearing plate during sintering, while for titanium or titanium alloy parts, because the titanium or titanium alloy parts have active chemical properties and high chemical affinity with elements such as O, C and the like, trace impurity elements can cause great influence on the mechanical properties of sintered titanium or titanium alloy. Specifically, in the high-temperature sintering process, the titanium or titanium alloy material is easy to chemically react with the setter plates made of traditional materials and generate brittle compounds, so that the product is poor.
Disclosure of Invention
The application aims to provide a novel technical scheme of a composite setter plate and a preparation method thereof.
In a first aspect, an embodiment of the present application provides a composite setter plate. The composite setter plate comprises: the plasma thermal spraying coating comprises a ceramic substrate and a coating arranged on at least one side of the ceramic substrate, wherein the coating is formed by a coating in a plasma thermal spraying mode;
the coating comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria.
Optionally, the thickness of the coating is set to be more than or equal to 0.12mm.
Optionally, the ceramic matrix has at least one first surface, and a rough structure with a roughness Ra ≥ 10 μm is formed at least in part of the first surface, and the rough structure has rugged pits.
Optionally, the coating is embedded into the concave pits with the rough structure and the unevenness, so that an embedded structure can be formed between the coating and the ceramic substrate, and the bonding force between the coating and the ceramic substrate is not less than 15MPa.
Optionally, the composite setter plate further includes an intermediate transition layer, the intermediate transition layer is formed on the ceramic substrate by means of plasma thermal spraying, and the intermediate transition layer is interposed between the ceramic substrate and the coating, and is used for connecting the ceramic substrate and the coating;
the thermal expansion coefficient of the intermediate transition layer is set to be between that of the ceramic substrate and that of the coating.
Optionally, the intermediate transition layer is a single crystal aluminum oxide layer.
Optionally, the intermediate transition layer is a bi-phase layer formed by yttrium-stabilized zirconia and alumina; wherein the mass fraction of the yttrium-stabilized zirconia is 60-80%, and the mass fraction of the alumina is 20-40%.
Optionally, the thickness of the intermediate transition layer is set to be 0.02mm to 0.1mm.
Optionally, the thickness of the coating is set to be 0.12 mm-0.2 mm, and the thickness of the composite setter plate is set to be 0.14 mm-0.3 mm.
Optionally, the ceramic matrix comprises 99-Al 2 O 3 A ceramic matrix or a corundum-mullite ceramic matrix.
In a second aspect, an embodiment of the present application provides a method for preparing a composite setter plate. The preparation method comprises the following steps:
providing a ceramic matrix;
spraying a coating on at least one side of the ceramic matrix in a plasma thermal spraying manner to form a coating on the ceramic matrix to obtain a blank; wherein the coating comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria;
and carrying out heat treatment on the obtained blank, and naturally cooling to obtain the composite setter plate.
Optionally, the preparation method further comprises: the ceramic substrate is provided with at least one first surface, the first surface is subjected to sand blasting treatment, and a rough structure with the roughness Ra being more than or equal to 10 mu m is formed on the first surface; wherein the roughness structure has rugged pits.
Optionally, the preparation method further comprises: the ceramic substrate is provided with at least one first surface, an intermediate transition layer is formed on the first surface in a plasma thermal spraying mode, and the intermediate transition layer is a single crystal alumina layer or a two-phase layer formed by yttrium-stabilized zirconia and alumina.
Optionally, the plasma thermal spray comprises: the method comprises the following steps of (1) driving by adopting a direct-current power supply, generating a direct-current arc between a cathode and an anode, respectively introducing main gas and auxiliary gas, and heating and ionizing the main gas and the auxiliary gas into high-temperature plasma serving as a heat source; the main gas comprises argon, helium or nitrogen, the flow rate of the main gas is 70-75L/min, the auxiliary gas is hydrogen, and the flow rate of the auxiliary gas is 2-3L/min;
the current is 500A-640A, the voltage is 38V-75V, the spraying distance is 6 cm-10 cm, and the spraying speed is 10 cm/s-20 cm/s.
Optionally, the heat treatment comprises: annealing at 650-800 deg.c to form high temperature stable structure.
The beneficial effect of this application lies in:
the composite burning bearing plate provided by the embodiment of the application is a composite structure, a ceramic matrix is used as a base material, at least one side of the ceramic matrix is sprayed to form a coating with good high-temperature stability, and the coating has excellent wetting resistance and erosion resistance to the titanium alloy at high temperature and is not easy to chemically react with the titanium alloy; in addition, the composite setter plate finally formed based on the spraying process has the advantages of high bonding strength, high density, few micro-defects, good high-temperature stability and low cost. The composite setter plate provided by the embodiment of the application can effectively replace an MIM titanium alloy sintering conventional bulk zirconia or yttria setter plate.
Further features of the present application and advantages thereof will become apparent from the following detailed description of exemplary embodiments thereof, which is to be read in connection with the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate embodiments of the application and together with the description, serve to explain the principles of the application.
FIG. 1 is one of the schematic structural diagrams of a composite setter plate of the present application;
FIG. 2 is a second schematic structural view of the composite setter plate according to the embodiment of the present application;
FIG. 3 is a flow chart of a method of making a composite setter plate according to an embodiment of the present application.
Description of reference numerals:
1. a ceramic substrate; 11. a first surface; 2. coating; 3. and an intermediate transition layer.
Detailed Description
Various exemplary embodiments of the present application will now be described in detail with reference to the accompanying drawings. It should be noted that: the relative arrangement of the components and steps, the numerical expressions, and numerical values set forth in these embodiments do not limit the scope of the present application unless specifically stated otherwise.
The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the application, its application, or uses.
Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate.
In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be discussed further in subsequent figures.
The composite setter plates provided in the embodiments of the present application and the methods for manufacturing the composite setter plates are described in detail below with reference to fig. 1 to 3.
In the processing of powder injection molded (MIM) titanium alloy products it was found that: the traditional setter plates made of alumina and corundum-mullite materials are poor in high-temperature stability, and are easy to pollute titanium products, so that the setter plates cannot be applied to sintering of the titanium products. The reason for this is that: the titanium alloy material has active chemical property and high chemical affinity with elements such as O, C and the like, and trace impurity elements can cause great influence on the mechanical property of the sintered titanium alloy. In the high-temperature sintering process, the titanium alloy material is easy to chemically react with the sintering bearing plate made of the traditional material to generate a brittle compound, so that the product is poor.
The sintering process of MIM titanium alloy can adopt zirconium oxide (ZrO) with better high-temperature stability 2 ) Or yttrium oxide (Y) 2 O 3 ) The material is used as a burning bearing plate, but the two materials are expensive, the expansion coefficient of the product is large, and the thermal shock resistance is poor. Therefore, if a bulk ZrO is simply used 2 Or Y 2 O 3 The sintering bearing plate not only can greatly increase the process cost of the MIM titanium alloy, but also has short service life and can not obtain good economic benefit.
The embodiment of the application provides a composite setter plate, which can be applied to a processing procedure of metal powder injection molding (MIM), is particularly suitable for MIM titanium alloy, can overcome the defect that the traditional alumina or corundum-mullite material is used as the setter plate, and cannot excessively increase the process cost of the MIM titanium alloy. The composite setter plates proposed in the embodiments of the present application are described in detail below.
Referring to fig. 1, the composite setter plate provided in the embodiment of the present application includes a ceramic substrate 1 and a coating 2 disposed on at least one side of the ceramic substrate 1, where the coating 2 may be formed by a coating material through plasma thermal spraying; wherein the coating may comprise at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria.
In the composite setter plate proposed in the above embodiment, the coating layer 2 may be formed on one side of the ceramic substrate 1 as one of the components of the composite setter plate, and the coating layer 2 may be, for example, a coating layer including an yttria material or a coating layer including a zirconia material, or may be, for example, a composite coating layer formed of an yttria material and a zirconia material.
The composite setter plate provided by the embodiment of the application is a composite material structure. Specifically, the composite setter plate includes, for example, a ceramic base 1 and a coating layer 2 provided on the ceramic base 1. In particular, the coating material forming the coating layer 2 includes, but is not limited to, pure zirconia powder or yttria powder. For example, the coating may be selected from magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria, in combination with one or more of these.
The coating 2 may be made of a material containing at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, and alumina-stabilized zirconia, and these materials are more stable. Can convert the unstable zirconia phase at room temperature into a stable state or a metastable state, and the formed coating 2 has the characteristics of more excellent heat resistance, corrosion resistance, ceramic toughening and the like. The material with good stability is used in the coating 2, so that the cubic or tetragonal zirconia can be stabilized in a wider temperature range, the stability of the performance of the formed whole composite setter plate is well improved, and the composite setter plate is suitable for the processing technology of the MIM titanium alloy.
In the embodiment of the present application, the coating 2 is formed on the ceramic substrate 1 by, for example, plasma thermal spraying, and the plasma thermal spraying can increase the bonding strength between the coating 2 and the ceramic substrate 1, and the formed composite setter plate has the characteristics of low surface porosity and compactness; meanwhile, based on the material property of the coating 2, the high-temperature stability of the whole composite setter plate is better. By using the composite setter plate provided by the embodiment of the application, in the high-temperature sintering process, the titanium alloy material does not react with the coating 2, and meanwhile, the coating 2 can well separate the titanium alloy material from the ceramic substrate 1, so that a brittle compound generated by the chemical reaction between the titanium alloy material and the ceramic substrate 1 in the high-temperature sintering process is avoided, and the product yield can be improved.
In the composite setter plate provided in the embodiment of the present application, a layer containing zirconium oxide (ZrO) is formed on the ceramic substrate 1 2 ) And/or yttria (Y) 2 O 3 ) Coating 2, as compared to the direct use of only bulk zirconia (ZrO) 2 ) Or yttrium oxide (Y) 2 O 3 ) As for the material setter plate, the process cost can be lower, the service life of the setter plate can be longer, good economic benefits can be obtained, and the setter plate is more suitable for industrial production.
The composite setter plate provided by the embodiment of the application is a composite structure, a ceramic substrate 1 is used as a base material, a coating 2 with good high-temperature stability is formed by spraying on at least one side of the base material, and the coating 2 has excellent wetting resistance and erosion resistance to titanium alloy at high temperature; the formed composite setter plate has the advantages of high bonding strength, low porosity, high density, few micro-defects, good high-temperature stability, simple structure and low cost.
The composite setter plate provided by the embodiment of the application can effectively replace the MIM titanium alloy sintering conventional bulk zirconia or yttria setter plate.
In some examples of the present application, the thickness of the coating 2 is set to ≧ 0.12mm.
The composite setter plate provided by the embodiment of the application is characterized in that a layer of the coating 2 is formed on the ceramic substrate 1, wherein the thickness of the coating 2 can be controlled to be not less than 0.12mm. In addition, the coating 2 is prepared on the ceramic substrate 1 by, for example, plasma thermal spraying, and can improve the surface performance of the formed composite sintered plate to a certain extent, for example, improve the surface compactness.
Wherein the thickness of the coating 2 cannot easily be designed too thin. For example, when the thickness of the coating 2 is less than 0.12mm, the coating 2 may be easily peeled off due to its thin thickness, and may not function to well isolate the titanium alloy material from the ceramic substrate 1.
Of course, the thickness of the coating 2 need not be made too large either. For example, when the thickness of the coating layer 2 is set to be greater than 0.2mm, the manufacturing cost of the composite setter may be increased, which results in no advantage of low cost.
Therefore, it is preferable that the thickness of the coating layer 2 is controlled to be, for example, 0.12mm to 0.2mm, and the use requirement can be satisfied while ensuring a small thickness range, and at the same time, the cost is not increased.
In some examples of the present application, referring to FIG. 1, the ceramic substrate 1 has at least one first surface 11, and a roughness structure having a roughness Ra ≧ 10 μm is formed at least in a part of the first surface 11, the roughness structure having recesses and projections.
The coating is embedded into the concave pits with the rough structures and the rough structures, so that an embedded structure can be formed between the coating 2 and the ceramic matrix 1, and the bonding force between the coating 2 and the ceramic matrix 1 is not less than 15MPa.
In the composite setter plate provided in the embodiment of the present application, a surface (for example, the first surface 11 shown in fig. 1) where the ceramic substrate 1 and the coating layer 2 are bonded to each other may be subjected to a sand blasting process in advance, which facilitates powdering when a paint is sprayed on the ceramic substrate 1, thereby facilitating the firm adhesion of the coating layer 2 to the ceramic substrate 1.
For example, the ceramic substrate 1 is a corundum-mullite substrate or 99-Al 2 O 3 The surface of the substrate and the ceramic substrate 1 is smooth, which is not beneficial to applying powder during spraying. In this case, a rough surface morphology may be obtained by sandblasting and abrasion, and a specific surface area may be enlarged, thereby improving a bonding force between the coating layer 2 and the ceramic substrate 1. In the examples of the present application, for exampleIf the bonding strength between the coating 2 and the ceramic substrate 1 is not less than 15MPa, the coating 2 can firmly cover the ceramic substrate 1 without easily falling off.
Specifically, the first surface 11 of the ceramic substrate 1 may be uniformly sand-blasted with white corundum sand grains to achieve a roughness Ra of 10 μm to 15 μm of the first surface 11.
Preferably, the ceramic substrate 1 has a first surface 11, and a roughness structure having recesses and protrusions with a roughness Ra of 10 to 15 μm is formed on the first surface 11. Thus, when the coating is sprayed and powdered, the coating can be partially embedded into the concave pits with the rough structure and the unevenness, so that the coating 2 and the ceramic matrix 1 can form an embedded state, and the bonding strength between the coating 2 and the ceramic matrix 1 can reach 15MPa or even higher. The formed composite setter plate has good integrity and is not easy to separate each layer.
It should be noted that the rough structure may be directly formed on the first surface 11 and is an uneven micron-scale structure, so that a plurality of micron-scale recesses may be formed on the first surface 11, and a part of the sprayed coating powder may enter the micron-scale recesses when falling onto the first surface 11, so as to increase the connection strength between the coating 2 and the ceramic substrate 1.
In the composite setter plate according to the embodiment of the present application, only the one coating layer 2 is not limited to be formed on the ceramic base 1, that is, other layered structures may be formed on the ceramic base 1.
In some examples of the present application, referring to fig. 2, the composite setter plate further includes an intermediate transition layer 3, the intermediate transition layer 3 is formed on the ceramic substrate 1 by means of plasma thermal spraying, and the intermediate transition layer 3 is interposed between the ceramic substrate 1 and the coating 2 to connect the ceramic substrate 1 and the coating 2; the thermal expansion coefficient of the intermediate transition layer 3 is set to be between that of the ceramic substrate 1 and that of the coating 2.
For example, a two-layer composite structure is disposed on the ceramic substrate 1, and includes the outermost coating layer 2 and an intermediate transition layer 3 in direct contact with the ceramic substrate 1, that is, an intermediate transition layer 3 may be further introduced between the coating layer 2 and the ceramic substrate 1. The intermediate transition layer 3 can be used to improve the bonding force between the coating 2 and the ceramic substrate 1.
In the above example, referring to fig. 2, the composition of the specially formulated intermediate transition layer 3 is designed to be between the coating layer 2 and the ceramic substrate 1, and the thermal expansion coefficient thereof is also between the coating layer 2 and the ceramic substrate 1, so that a transition of the thermal expansion coefficient can be formed between the coating layer 2 and the ceramic substrate 1, which acts to reduce the difference between the thermal expansion coefficients, thereby reducing the thermal stress of the material of the coating layer 2 and the material of the ceramic substrate 1 under high temperature conditions, and enhancing the spalling resistance of the coating layer 2.
Alternatively, before the intermediate transition layer 3 is formed on the ceramic substrate 1, a certain roughness Ra may be formed on the first surface 11 of the ceramic substrate 1 bonded to the intermediate transition layer 3 by sand blasting. Wherein the roughness can also reach 10-15 μm. Thus, the bonding strength between the intermediate transition layer 3 and the ceramic matrix 1 is improved.
The intermediate transition layer 3 may be fitted to the roughness structure formed on the first surface layer 11.
In the above example, in the process of preparing the composite setter plate, before the plasma thermal spray coating on the ceramic substrate 1 forms the coating 2, the intermediate transition layer 3 may be sprayed on, for example, the first surface 11 of the ceramic substrate 1, so as to increase the bonding force between the coating 2 and the ceramic substrate 1, and meanwhile, the double-layer spraying may better block the impurity infiltration pollution in the ceramic substrate 1.
Optionally, the intermediate transition layer 3 is a single crystal alumina layer.
Optionally, the intermediate transition layer 3 is a two-phase layer formed by yttrium-stabilized zirconia and alumina; wherein the mass fraction of the yttrium-stabilized zirconia is 60-80%, and the mass fraction of the alumina is 20-40%.
That is, the intermediate transition layer 3 may be a single-crystal alumina layer. Of course, the intermediate transition layer 3 may also be a two-phase composite material layer formed by mixing yttrium-stabilized zirconia and alumina, wherein the mass ratio of the yttrium-stabilized alumina is 60% to 80%, and the mass ratio of the alumina is 20% to 40%. It can be seen that the composition of the intermediate transition layer 3 is specifically formulated to be interposed between the coating 2 and the ceramic substrate 1, and thus to have a coefficient of thermal expansion also interposed between the coating 2 and the ceramic substrate 1, so that a transition in coefficient of thermal expansion can be formed between the coating 2 and the ceramic substrate 1, which serves to reduce the difference in coefficient of thermal expansion.
The intermediate transition layer 3 is added between the ceramic substrate 1 and the coating 2, so that the bonding strength between the ceramic substrate 1 and the coating 2 is improved. Meanwhile, based on a double-layer spraying process, the surface of the formed composite setter plate has extremely low porosity, fewer micro-defects and higher surface compactness. Meanwhile, the composite setter plate has the characteristic of good high-temperature stability. The whole composite setter plate is simple in manufacturing process, simple in structure and remarkable in cost benefit. Can effectively replace the conventional bulk zirconia or yttria setter plates used in MIM titanium alloy sintering.
Optionally, the thickness of the intermediate transition layer 3 is set to be 0.02mm to 0.1mm.
When the thickness of the intermediate transition layer 3 is within the above range, the manufacturing cost of the composite setter plate can be well controlled, and meanwhile, the bonding strength between the ceramic substrate 1 and the coating 2 can reach a better value, and the thickness of the whole composite setter plate cannot be too large.
Preferably, the thickness of the intermediate transition layer 3 may be set to 0.05mm to 0.08mm. The cost of the composite setter plate can be better controlled, and the bonding strength between the ceramic substrate 1 and the coating 2 can be ensured.
In some examples of the present application, the thickness of the coating layer 2 is set to 0.12mm to 0.2mm, and the thickness of the composite setter is set to 0.14mm to 0.3mm.
On the basis, the thickness of the intermediate transition layer 3 can be controlled to be 0.02 mm-0.1 mm.
It should be noted that the thickness of the coating 2 is not easily designed to be too thin or too thick. When the thickness of the coating 2 is less than 0.12mm, the coating 2 may easily fall off during the high-temperature sintering process, and cannot perform a good function of isolating the titanium alloy material from the ceramic substrate 1. When the thickness of the coating layer 2 is set to be greater than 0.2mm, the manufacturing cost of the composite setter plate is increased, which results in no advantage of low cost.
The thickness of the whole composite setter plate should be reasonably controlled, otherwise the process cost is increased.
The thickness of the ceramic substrate 1 may be reasonably adjusted according to the thickness of the composite setter plate, the thickness of the coating 2, and the thickness of the intermediate transition layer 3, which is not limited in the present application.
In the composite setter plate provided in the embodiment of the present application, the ceramic base 1 includes, for example, 99-Al 2 O 3 A ceramic matrix or a corundum-mullite ceramic matrix.
The composite setter plate provided by the embodiment of the application takes the traditional alumina or corundum-mullite material as a base material, and a coating 2 with prominent anti-erosion performance is formed on the base material by spraying. The ceramic substrate 1 is widely available. The finally formed composite setter plate has a series of advantages of high bonding strength, low porosity, few micro-defects, high density, good high-temperature stability, simple structure, outstanding cost benefit and the like, and can effectively replace the conventional bulk zirconia or yttria setter plate sintered by MIM titanium alloy.
According to another aspect of the embodiment of the application, a preparation method of the composite setter plate is further provided, and the preparation method can be used for manufacturing the composite setter plate.
Referring to fig. 3, the method for preparing a composite setter plate provided in the embodiment of the present application at least includes the following steps 301 to 303:
the ceramic matrix 1 is, for example, 99-Al 2 O 3 A ceramic matrix or a corundum-mullite ceramic matrix.
302, spraying a coating on at least one side of the ceramic substrate 1 by adopting a plasma thermal spraying mode to form a coating 2 on the ceramic substrate 1 to obtain a blank;
wherein the coating comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria.
And 303, carrying out heat treatment on the blank obtained in the step 302, and naturally cooling to obtain the composite setter plate.
Optionally, the preparation method further comprises the following steps:
referring to FIG. 1, the ceramic substrate 1 has at least one first surface 11, and the first surface 11 is subjected to sand blasting to form a rough structure with a roughness Ra of more than or equal to 10 μm on the first surface 11; wherein the roughness structure has rugged pits.
Specifically, the ceramic substrate 1 is, for example, 99-Al 2 O 3 Ceramic substrates or corundum-mullite ceramic substrates, which have a relatively smooth surface of the ceramic substrate 1, are not advantageous for applying powder during spraying. Based on this, before the step 302 is performed, the roughness of the surface of the ceramic substrate 1 may be increased by sandblasting and abrasion, so as to enlarge the specific surface area, facilitate the powdering during spraying, and improve the bonding force between the formed coating 2 and the ceramic substrate 1.
When the coating powder is sprayed, the powder can partially enter the concave pits with the rough structures and the rough structures, so that the coating 2 and the ceramic matrix 1 are mutually embedded, and the coating and the ceramic matrix naturally have stronger bonding fastness. It can be ensured that the coating 2 does not easily fall off in long-term use.
In a specific example, the first surface 11 of the ceramic substrate 1 may be uniformly blasted with a white corundum grit to achieve a roughness Ra of the first surface 11 of 10-15 μm.
In some examples of the present application, the method of making a composite setter plate further comprises:
referring to fig. 2, the ceramic substrate 1 has at least one first surface 11, and an intermediate transition layer 3 is formed on the first surface 11 by means of plasma thermal spraying, wherein the intermediate transition layer 3 may be provided as a single crystal alumina layer or a bi-phase layer formed from yttrium-stabilized zirconia and alumina.
As an optimized preparation method provided by the present application, before the coating 2 is sprayed, an intermediate transition layer 3 may be sprayed on the first surface 11 of the ceramic substrate 1, and the intermediate transition layer 3 is made of alumina or a composite material of zirconia and alumina. The double-layer spraying is carried out on the ceramic matrix 1, so that the impurity permeation pollution in the ceramic matrix 1 can be better prevented.
The material components of the intermediate transition layer 3 with a specific formula are between the coating 2 and the ceramic matrix 1, the intermediate transition layer 3 can increase the bonding force between the coating 2 and the ceramic matrix 1, and the three can be firmly combined into a whole to form a multilayer composite structure material; meanwhile, the thermal expansion coefficient of the material of the intermediate transition layer 3 is also between that of the coating 2 and that of the ceramic substrate 1, so that the difference of the thermal expansion coefficients can be reduced, the thermal stress of the coating material and that of the ceramic substrate material under the high-temperature condition can be reduced, and the anti-stripping capability of the coating 2 can be enhanced.
In some examples of the present application, the plasma thermal spray comprises: the method comprises the following steps of adopting a direct-current power supply for driving, generating a direct-current arc between a cathode and an anode, respectively introducing main gas and auxiliary gas, and heating and ionizing the main gas and the auxiliary gas into high-temperature plasma serving as a heat source; the main gas comprises argon, helium or nitrogen, the flow rate of the main gas is 70L/min-75L/min, the auxiliary gas is hydrogen, and the flow rate of the auxiliary gas is 2L/min-3L/min; the current is 500A-640A, the voltage is 38V-75V, the spraying distance is 6 cm-10 cm, and the spraying speed is 10 cm/s-20 cm/s.
The coating 2 and the intermediate transition layer 3 can be prepared by adopting a plasma thermal spraying technology. The thickness of the formed coating layer 2 is set to 0.12mm to 0.2mm, for example. The intermediate transition layer 3 is formed to have a thickness of, for example, 0.02mm to 0.1mm.
The plasma thermal spraying is driven by a direct current power supply, a direct current electric arc is generated between a cathode and an anode, introduced argon and hydrogen are heated and ionized into high-temperature plasma which serves as a heat source, coating powder fed by powder feeding gas is heated and melted, and then the coating powder is sprayed onto a ceramic substrate 1 subjected to sand blasting treatment in an accelerating mode through plasma flame to form a coating 2, and the formed coating 2 has the advantages of being good in flatness, high in density and the like.
In one specific example, the step of preparing the coating 2 by the plasma spraying technology comprises the following steps: drying and sand blasting (preprocessing) the first surface 11 of the ceramic substrate 1 to make the roughness Ra of the first surface 11 reach 10-15 μm; loading zirconia powder to be sprayed into a powder feeding device of special equipment, and feeding the zirconia powder into a spray gun nozzle during working; the ceramic matrix 1 is arranged on a special spraying workbench, special plasma spraying equipment is started, gas is sent into a spray gun, the spray gun is ignited to generate plasma flame flow, the ceramic matrix 1 starts to be subjected to spray coating, and the thickness of the coating 2 is controlled to be more than or equal to 0.12mm. Wherein, the main gas used in the spraying process is Ar or He or N2, the gas flow is controlled to be 70L/min to 75L/min, and the auxiliary gas is H 2 The gas flow is 2L/min-3L/min; the current is 500A-640A, the voltage is 38-75V, the spraying distance is 6 cm-10 cm, and the spraying speed is 10 cm/s-20 cm/s.
The above-described plasma thermal spray process is equally applicable to the intermediate transition layer, and may be distinguished only by the powder being sprayed.
In some examples of the present application, the heat treatment in step 303 includes: annealing at 650-800 deg.c to form high temperature stable structure.
After the spraying is finished (only the coating 2 can be sprayed, or the intermediate transition layer 3 and the coating 2 can be sprayed), the obtained blank needs to be subjected to heat treatment. Specifically, the medium temperature annealing may be performed at a temperature of 650 ℃ to 800 ℃ for 2 hours, for example, to reoxidize an oxygen-deficient phase generated in the plasma flame stream including the yttria-stabilized zirconia coating to form a high temperature stable structure.
And after the heat treatment is finished, naturally cooling to obtain the composite setter plate.
The composite setter plate provided by the embodiment of the application comprises 99-Al 2 O 3 The ceramic base or corundum-mullite ceramic base is coated with a coating 2 with a specific component by single-layer spraying, or a middle transition layer 3 and the coating 2 are formed by double-layer spraying. Compared with the titanium alloy sintered bulk zirconia or yttria setter plates used in the current market, the titanium alloy sintered bulk zirconia or yttria setter plates have the advantages of low cost, long service life, good high-temperature stability, no product pollution and the like.
Example 1
Referring to fig. 1, the preparation method of the composite setter plate includes:
wherein the ceramic matrix 1 is 99-Al 2 O 3 Ceramic matrix or corundum-mullite ceramic matrix.
wherein the plasma thermal spray comprises: the method comprises the following steps of adopting a direct-current power supply for driving, generating a direct-current arc between a cathode and an anode, respectively introducing main gas and auxiliary gas, and heating and ionizing the main gas and the auxiliary gas into high-temperature plasma serving as a heat source; the main gas comprises argon, helium or nitrogen, the flow rate of the main gas is 70-75L/min, the auxiliary gas is hydrogen, and the flow rate of the auxiliary gas is 2-3L/min; the current is 500A-640A, the voltage is 38V-75V, the spraying distance is 6 cm-10 cm, and the spraying speed is 10 cm/s-20 cm/s.
Step 4, carrying out heat treatment on the blank obtained in the step 3, and naturally cooling to obtain a composite setter plate; wherein the heat treatment is carried out at 650-800 ℃ for annealing treatment to form a high-temperature stable structure.
Example 2
Referring to fig. 2, the preparation method of the composite setter plate includes:
wherein the ceramic matrix 1 is 99-Al 2 O 3 A ceramic matrix or a corundum-mullite ceramic matrix.
And 3, forming an intermediate transition layer 3 on the first surface 11 in a plasma thermal spraying manner after the step 2, wherein the intermediate transition layer is a single crystal alumina layer or a two-phase layer formed by yttrium-stabilized zirconia and alumina.
Step 4, spraying a coating on the intermediate transition layer 3 by adopting a plasma thermal spraying mode to form a coating 2 on the intermediate transition layer 3 to obtain a blank; wherein the coating comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria;
in step 3 and step 4, the plasma thermal spraying includes: the method comprises the following steps of (1) driving by adopting a direct-current power supply, generating a direct-current arc between a cathode and an anode, respectively introducing main gas and auxiliary gas, and heating and ionizing the main gas and the auxiliary gas into high-temperature plasma serving as a heat source; the main gas comprises argon, helium or nitrogen, the flow rate of the main gas is 70L/min-75L/min, the auxiliary gas is hydrogen, and the flow rate of the auxiliary gas is 2L/min-3L/min; the current is 500A-640A, the voltage is 38V-75V, the spraying distance is 6 cm-10 cm, and the spraying speed is 10 cm/s-20 cm/s.
Step 5, carrying out heat treatment on the blank obtained in the step 4, and naturally cooling to obtain a composite setter plate; wherein the heat treatment is carried out at 650-800 ℃ for annealing treatment to form a high-temperature stable structure.
The difference between the above embodiment 1 and embodiment 2 is that the composite setter plate provided in embodiment 2 is added with the intermediate transition layer 3. The bonding strength between the coating 2 and the ceramic matrix 1 can be better improved by additionally arranging the intermediate transition layer 3 before the coating 2 is sprayed on the surface of the ceramic matrix 1, and the impurity permeation pollution in the ceramic matrix 1 can be better prevented by double-layer spraying. The components of the intermediate transition layer 3 with a specific formula are between the coating 2 on the surface layer and the ceramic substrate 1 on the bottom layer, and the thermal expansion coefficients are also between the two, so that the effect of reducing the difference of the thermal expansion coefficients can be achieved, the thermal stress of the coating material and the substrate material under the high-temperature condition is reduced, and the anti-stripping capability of the coating is enhanced.
In the above embodiments, the differences between the embodiments are described in emphasis, and different optimization features between the embodiments can be combined to form a better embodiment as long as the differences are not contradictory, and further description is omitted here in consideration of brevity of the text.
Although some specific embodiments of the present application have been described in detail by way of illustration, it should be understood by those skilled in the art that the above illustration is only for purposes of illustration and is not intended to limit the scope of the present application. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the present application. The scope of the application is defined by the appended claims.
Claims (15)
1. The composite setter plate is characterized by comprising a ceramic substrate (1) and a coating (2) arranged on at least one side of the ceramic substrate (1), wherein the coating (2) is formed by coating in a plasma thermal spraying manner;
the coating comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria.
2. The composite setter plate of claim 1, wherein the thickness of the coating (2) is set to 0.12mm or more.
3. The composite setter plate as set forth in claim 1, wherein the ceramic substrate (1) has at least one first surface (11), and a coarse structure having a roughness Ra of 10 μm or more is formed at least in a part of the first surface (11), the coarse structure having concave and convex pits.
4. The composite setter plate as set forth in claim 3, wherein the paint is embedded in the recesses having the rugged coarse structure to enable the coating (2) and the ceramic base (1) to form an embedded structure therebetween, and the bonding force between the coating (2) and the ceramic base (1) is equal to or greater than 15MPa.
5. The composite setter plate as set forth in claim 1, further comprising an intermediate transition layer (3), the intermediate transition layer (3) being formed on the ceramic base (1) by means of plasma thermal spraying, and the intermediate transition layer (3) being interposed between the ceramic base (1) and the coating (2) for connecting the ceramic base (1) and the coating (2);
the thermal expansion coefficient of the intermediate transition layer (3) is set to be between that of the ceramic substrate (1) and that of the coating (2).
6. Composite setter plate according to claim 5, characterized in that the intermediate transition layer (3) is a layer of monocrystalline alumina.
7. The composite setter plate of claim 5, wherein the intermediate transition layer (3) is a bi-phase layer formed from yttrium stabilized zirconia and alumina; wherein the mass fraction of the yttrium-stabilized zirconia is 60-80%, and the mass fraction of the alumina is 20-40%.
8. The composite setter plate of claim 5, wherein the thickness of the intermediate transition layer (3) is set to 0.02mm to 0.1mm.
9. The composite setter plate of any one of claims 1 to 8, wherein the thickness of the coating layer (2) is set to 0.12mm to 0.2mm, and the thickness of the composite setter plate is set to 0.14mm to 0.3mm.
10. The composite setter plate of claim 9, wherein the ceramic matrix (1) comprises 99-Al 2 O 3 Ceramic matrix or corundum-mullite ceramic matrix.
11. A method of making a composite setter plate as set forth in any one of claims 1 to 10, comprising:
providing a ceramic substrate;
spraying a coating on at least one side of the ceramic matrix in a plasma thermal spraying manner to form a coating on the ceramic matrix to obtain a blank; wherein the coating comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria;
and carrying out heat treatment on the obtained blank, and naturally cooling to obtain the composite setter plate.
12. The method of making a composite setter plate of claim 11, further comprising: the ceramic substrate is provided with at least one first surface, and the first surface is subjected to sand blasting treatment to form a rough structure with the roughness Ra being more than or equal to 10 mu m on the first surface; wherein the roughness structure has rugged pits.
13. The method of making a composite setter plate of claim 11, further comprising: the ceramic substrate is provided with at least one first surface, an intermediate transition layer is formed on the first surface in a plasma thermal spraying mode, and the intermediate transition layer is a single crystal alumina layer or a two-phase layer formed by yttrium-stabilized zirconia and alumina.
14. The method of making a composite setter plate of claim 11, wherein the plasma thermal spraying includes: the method comprises the following steps of (1) driving by adopting a direct-current power supply, generating a direct-current arc between a cathode and an anode, respectively introducing main gas and auxiliary gas, and heating and ionizing the main gas and the auxiliary gas into high-temperature plasma serving as a heat source; the main gas comprises argon, helium or nitrogen, the flow rate of the main gas is 70L/min-75L/min, the auxiliary gas is hydrogen, and the flow rate of the auxiliary gas is 2L/min-3L/min;
the current is 500A-640A, the voltage is 38V-75V, the spraying distance is 6 cm-10 cm, and the spraying speed is 10 cm/s-20 cm/s.
15. The method of making a composite setter plate of claim 11, wherein the heat treating includes: annealing at 650-800 deg.c to form high temperature stable structure.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113913727A (en) * | 2021-09-28 | 2022-01-11 | 德清创智科技股份有限公司 | Preparation method of thermal spraying ceramic coating of sagger burning board |
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