CN115947618A - Composite burning bearing plate and preparation method thereof - Google Patents
Composite burning bearing plate and preparation method thereof Download PDFInfo
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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 dispersing a first set material in a sol-gel solution to form composite slurry and then drying and sintering the composite slurry; wherein the first setting material 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 setter plate during sintering, and for titanium or titanium alloy parts, because the titanium or titanium alloy parts have active chemical properties and have 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 a ceramic substrate and a coating arranged on at least one side of the ceramic substrate, wherein the coating is formed by dispersing a first set material in a sol-gel solution to form composite slurry and then drying and sintering the composite slurry;
wherein the first setting material 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 is provided with at least one first surface, and at least part of the first surface is formed with a rough structure with the roughness Ra being more than or equal to 10 mu m, and the rough structure is provided with concave-convex pits;
the composite slurry can be embedded into the concave pits with the rough structure and the unevenness, so that an embedded structure is formed between the coating and the ceramic substrate.
Optionally, the bonding force between the coating and the ceramic matrix is more than or equal to 15MPa.
Optionally, the composite setter plate further includes an intermediate transition layer formed on the surface of the ceramic substrate by a sol-gel method, and the intermediate transition layer is interposed between the ceramic substrate and the coating layer, so that the coating layer and the ceramic substrate are disposed at an interval.
Optionally, the intermediate transition layer is formed in a manner that: dispersing a second set material in the sol-gel solution, then coating the sol-gel solution on the surface of the ceramic substrate, and drying and sintering the sol-gel solution to obtain the ceramic substrate;
wherein the second setting material is single crystal alumina; alternatively, the first and second liquid crystal display panels may be,
the second setting material is formed of yttrium stabilized zirconia and alumina as a dual phase material; wherein the mass fraction of the yttrium-stabilized zirconia is 60-80%, and the mass fraction of the alumina is 20-40%.
Optionally, the intermediate transition layer has a coefficient of thermal expansion set between that of the ceramic substrate and that of the coating.
Optionally, the ceramic matrix comprises 99-Al 2 O 3 A ceramic matrix or a corundum-mullite ceramic matrix.
In a second aspect, embodiments of the present application provide a method for manufacturing a composite setter plate. The preparation method comprises the following steps:
providing a ceramic matrix;
dispersing a first set material in the sol-gel sol, and fully reacting at a set temperature to obtain composite slurry; wherein the first setting material comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria;
and coating the composite slurry on the surface of the ceramic matrix to form a wet blank, and drying and sintering the wet blank to form a coating on the surface of the ceramic matrix to obtain the composite setter plate.
Optionally, the step of preparing the composite slurry comprises:
dissolving zirconium oxide containing crystal water in alcohol or water, and adding a colloidal particle generating agent to obtain a mixed solution; wherein the colloidal particle generating agent is urea;
y with the mass fraction of 2.5 to 3.5 percent 2 O 3 Adding into hydrochloric acid solution, heating until hydrochloric acid is evaporated to dryness, and dissolving the obtained product in deionized water under ultrasonic condition to obtain Y 2 O 3 By YCl 3 Exists in the form of (1);
subjecting the obtained YCl to 3 Dispersing into the mixed solution, and then adding a dispersing agent to obtain yttrium-containing zirconium dioxide sol as composite slurry; wherein the dispersant is polyethylene glycol.
Optionally, the ceramic substrate is pre-machined to a set shape.
Optionally, in the step of preparing the composite slurry, the set temperature is 75 ℃ to 85 ℃.
Optionally, in forming the coating: the drying step comprises natural drying for 2 to 3 hours and drying for 5 to 7 hours at the temperature of between 45 and 65 ℃; the sintering step comprises heat preservation for 3-5 h at 1500-1600 ℃.
Optionally, before the step of coating the composite slurry on the surface of the ceramic substrate, the method further comprises:
firstly forming a rough structure with the roughness Ra of more than or equal to 10 mu m on the surface of the ceramic matrix, wherein the rough structure is provided with rugged pits; and/or the presence of a gas and/or,
and forming an intermediate transition layer on the surface of the ceramic matrix by a sol-gel method.
The beneficial effect of this application lies in:
the composite setter plate provided by the embodiment of the application is a composite structure, a ceramic substrate is used as a base material, and at least one side of the base material is coated in a sol-gel manner to form a coating with good high-temperature stability, wherein 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.
Other features of the present application and advantages thereof will become apparent from the following detailed description of exemplary embodiments thereof, which proceeds with reference to 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 a schematic structural view of a composite setter plate according to an embodiment 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 those 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, further discussion thereof is not required in subsequent figures.
The composite setter plate and the method for manufacturing the composite setter plate according to the embodiment of the present application will be described in detail 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, the chemical affinity with elements such as O, C and the like is high, 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 metal powder injection molding (MIM) processing procedure, 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.
The composite setter plate provided by the embodiment of the application is shown in fig. 1, and comprises: the coating comprises 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 dispersing a first set material in a sol-gel solution to form a composite slurry and then drying and sintering the composite slurry; wherein the first setting material comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria.
In the composite setter plates proposed in the above embodiments, the coating layer 2 may be formed on one side of the ceramic base 1 as one of the components of the composite setter plate. The coating 2 may be, for example, a coating containing an yttria material or a coating containing a zirconia material, or may be, for example, a composite coating formed by 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 stable state or 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 layer 2 is formed by using a sol-gel technique, for example, and may be formed on the ceramic substrate 1 by a coating method such as spraying or painting. Specifically, the coating 2 on the ceramic substrate 1 may be obtained by a sol-gel technique, and the formed composite slurry (or called coating sol) is uniformly coated on the surface of the ceramic substrate 1 by a spraying method, and finally, the coating-ceramic substrate composite structure is formed after drying and sintering.
The ceramic base 1 is, for example, a ceramic substrate processed in advance into a predetermined shape, and a composite setter plate can be finally formed.
In the preparation method provided by the embodiment of the application, the adopted sol-gel method has the advantages of simple and non-harsh reaction conditions, controllable components, low cost and simpler operation. The composite slurry (or called coating sol) prepared by the sol-gel method has certain fluidity, can be coated on the surface of the ceramic matrix 1 in various ways, and has relatively small restriction on the coating way.
For example, the formed composite slurry (or called coating sol) may be formed on the surface of the ceramic substrate 1 by a spraying process, and it may cover the surface of the ceramic substrate 1, so that the formed composite setter plate may have 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.
The embodiments of the present application provideThe composite setter plate of (1) has a zirconia (ZrO) containing layer formed on the ceramic base 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 setter plate made of the material, 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 load bearing plate provided by the embodiment of the application is of a composite structure, a ceramic substrate 1 is used as a base material, at least one side of the base material is coated in a sol-gel manner to form a coating 2 with good high-temperature stability, and the coating 2 has excellent wetting resistance and erosion resistance to the titanium alloy at high temperature and is not easy to react with the titanium alloy chemically; and the composite burning board 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 load bearing plate provided by the application can effectively replace an MIM titanium alloy sintering conventional bulk zirconia or yttria load bearing plate.
In the preparation method of the composite setter plate provided by the embodiment of the application, a sol-gel manner is adopted when the coating 2 is formed, specifically, a first set material (such as fine ceramic powder) is uniformly dispersed in a sol-gel solution to form a composite slurry, and then a spraying technology is adopted to coat the surface of the ceramic substrate 1 to form a pre-coating layer, and then the pre-coating layer is dried and sintered to obtain the coating 2.
The more specific process is as follows: adding a certain content of first set material into the sol, fully stirring and defoaming to obtain a material-composite slurry for preparing the coating 2, coating a pre-coating layer on the surface of the ceramic substrate 1 by adopting a spraying technology, and then drying and sintering to form the coating 2. Because the first setting material is introduced into the sol and ceramic powder is contained in the sol, the volume fraction of the solvent is greatly reduced, and the cracking tendency of the gel film in the subsequent drying and sintering processes is greatly reduced.
In some examples of the present application, the thickness of the coating 2 is set to be ≧ 0.12mm.
The composite setter plate according to the embodiment of the present application has, for example, a coating layer 2 formed on the ceramic substrate 1, wherein the thickness of the coating layer 2 may be designed to be not less than 0.12mm.
The coating 2 is prepared by preparing composite slurry by a sol-gel method, and then coating the composite slurry with certain fluidity on the surface of the ceramic substrate 1 by spraying or the like. The coating 2 can improve the surface properties of the formed composite sintered plate to a certain extent, for example, the compactness of the surface is improved.
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 is too thin and may easily come off, while not functioning well to separate 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 2mm, the manufacturing cost of the composite setter may be increased, which results in no advantage of low cost.
The thickness of the coating layer 2 can be controlled, for example, to 1.5mm to 2mm, based on the fact that the coating layer 2 is formed by adding the first setting material to the sol-gel system.
Of course, the coating 2 is not limited to the above-mentioned 1.5mm to 2mm, and a thin coating can be realized, so that the use requirement can be met while the small thickness range is ensured, and 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, at least a part of the first surface 11 is formed with a roughness Ra ≧ 10 μm, the roughness having rugged pits; the composite slurry can be embedded into the concave pits with the rugged rough structure, so that an embedded structure is formed between the coating 2 and the ceramic matrix 1.
Wherein the binding force between the coating 2 and the ceramic substrate 1 is more than or equal to 15MPa.
In the composite setter plate provided in the embodiment of the present application, a surface (e.g., the first surface 11 shown in fig. 1) of the ceramic substrate 1 and the coating layer 2 may be subjected to a surface etching process in advance, for example, a sand blasting process. This facilitates that when the composite paste is coated on the ceramic substrate 1, the composite paste can be partially embedded into the pits formed on the surface of the ceramic substrate 1 by sand blasting, thereby facilitating that the coating 2 can be firmly attached to the ceramic substrate 1.
Because the composite slurry formed by the sol-gel method is liquid and has certain fluidity, the optional coating process is more. For example, spraying or direct application may be used.
For example, the ceramic substrate 1 is a corundum-mullite substrate or 99-Al 2 O 3 The surface of the ceramic substrate 1 is relatively smooth, which is not favorable for the composite slurry to hang on the surface of the ceramic substrate 1 during coating. At this time, a rough surface morphology is obtained by sandblasting and rubbing, and a specific surface area can be enlarged, so that a bonding force between the coating 2 and the ceramic substrate 1 can be improved.
In the embodiment of the present application, the bonding strength between the coating 2 and the ceramic substrate 1 is not less than 15MPa, and 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.
For example, the ceramic body 1 has a first surface 11, and a rough structure having a roughness Ra of 10 to 15 μm is formed on the first surface 11, the rough structure having concave and convex recesses. When the composite slurry is sprayed, the composite slurry 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, a plurality of micron-scale pits may be formed on the first surface 11, and a part of the sprayed composite slurry may enter the micron-scale pits when falling onto the first surface 11, so as to increase the connection strength between the coating 2 and the ceramic substrate 1.
The surface of the ceramic body 1 may be formed with a roughness having a certain roughness by other means such as chemical etching, and is not limited to the sandblasting treatment in the above example.
In the composite setter plate according to the embodiment of the present application, the ceramic base 1 is not limited to the one-layer coating 2, that is, other layered structures may be formed on the ceramic base 1.
Optionally, referring to fig. 2, the composite setter plate further includes an intermediate transition layer 3, the intermediate transition layer 3 is formed on the surface of the ceramic substrate 1 by a sol-gel method, and the intermediate transition layer 3 is interposed between the ceramic substrate 1 and the coating layer 2, so that the coating layer 2 and the ceramic substrate 1 are arranged at an interval.
Specifically, a double-layer coating 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. The intermediate transition layer 3 can be used to improve the bonding force between the coating 2 and the ceramic substrate 1.
The coating 2 and the intermediate transition layer 3 form a double-coating structure on the ceramic substrate 1; the coating 2 is an external protective coating, and the intermediate transition layer 3 is a bonding layer, and can be used for improving the bonding force between the coating 2 and the ceramic substrate 1.
For example, the intermediate transition layer 3 is formed in the following manner: dispersing a second set material in the sol-gel solution, then coating the sol-gel solution on the surface of the ceramic substrate, and drying and sintering the sol-gel solution to obtain the ceramic substrate;
wherein the second setting material is single crystal alumina; alternatively, the first and second electrodes may be,
the second setting material is formed of yttrium stabilized zirconia and alumina as a dual phase material; wherein the mass fraction of the yttrium-stabilized zirconia is 60-80%, and the mass fraction of the alumina is 20-40%.
In the embodiment of the application, after the intermediate transition layer 3 is introduced, by means of the fine second setting material powder dispersed in the sol-gel solution, the surface cracking condition of the product can be reduced to a certain extent, which is beneficial to improving the yield of the product.
Optionally, 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.
The components of the intermediate transition layer 3 with a specific formula are designed to be between the coating 2 and the ceramic substrate 1, and the thermal expansion coefficient of the intermediate transition layer is also between the coating 2 and the ceramic substrate 1, so that a transition of the thermal expansion coefficient can be formed between the coating 2 and the ceramic substrate 1, and the effect of reducing the difference of the thermal expansion coefficients is achieved, thereby reducing the thermal stress of the material of the coating 2 and the material of the ceramic substrate 1 under the high-temperature condition, and enhancing the anti-stripping capability of the coating 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 or chemical etching. 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.
It is understood that, in the process of preparing the composite setter plate, the intermediate transition layer 3 may be formed on, for example, the first surface 11 of the ceramic substrate 1 before the coating layer 2 is formed on the ceramic substrate 1, so as to increase the bonding force between the coating layer 2 and the ceramic substrate 1, and at the same time, the double-layer coating may better block the impurity infiltration contamination in the ceramic substrate 1.
The intermediate transition layer 3 may be formed as 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 between the coating 2 and the ceramic substrate 1, and thus, the thermal expansion coefficient thereof is also between the coating 2 and the ceramic substrate 1, so that a thermal expansion coefficient transition can be formed between the coating 2 and the ceramic substrate 1, which serves to reduce the thermal expansion coefficient difference.
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 the double-layer coating 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.
The thickness of the intermediate transition layer 3 is set to 0.02mm to 0.1mm, for example. 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 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 S301 to S303:
step S301, providing a ceramic substrate 1, as shown in fig. 1;
the ceramic matrix 1 is, for example, 99-Al 2 O 3 A ceramic matrix or a corundum-mullite ceramic matrix.
Step S302, dispersing a first set material in the sol-gel sol, and fully reacting at a set temperature to obtain a composite slurry;
wherein the first setting material comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria;
and S303, carrying out heat treatment on the blank obtained in the step S302, and naturally cooling to obtain the composite setter plate.
Optionally, the ceramic substrate 1 is pre-machined to a predetermined shape.
For example, the ceramic base 1 is previously processed into a shape of a setter, and a composite setter having a predetermined shape can be directly formed without cutting it at a later stage.
Optionally, in the step 302 of preparing the composite slurry, the set temperature is 75 ℃ to 85 ℃.
Optionally, in forming the coating: the drying step comprises natural drying for 2 to 3 hours and drying for 5 to 7 hours at the temperature of between 45 and 65 ℃; the sintering step comprises heat preservation for 3-5 h at 1500-1600 ℃.
Under the above-mentioned drying conditions and sintering conditions, the formed coating 2 can be made to have a greatly reduced tendency to crack during drying and sintering. The composite setter plate formed by the method also has the excellent performances of high bonding strength, low porosity, few micro-defects and high surface density.
Optionally, the preparation method further comprises the following steps: before the step of coating the composite slurry on the surface of the ceramic substrate 1, the method further includes:
firstly forming a rough structure with the roughness Ra of more than or equal to 10 mu m on the surface of the ceramic matrix 1, wherein the rough structure is provided with concave-convex pits; and/or the presence of a gas in the atmosphere,
an intermediate transition layer is formed on the surface of the ceramic substrate 1 by a sol-gel method.
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 or chemical etching treatment 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 A ceramic matrix or a corundum-mullite ceramic matrix, the surface of the ceramic matrix 1 of which is relatively smooth, is not conducive to the formation of coatings. Based on this, before the step 302 is performed, the roughness of the surface of the ceramic substrate 1 may be increased, for example, by sandblasting and grinding, so as to enlarge the specific surface area, so as to facilitate uniform coating of the composite slurry, and improve the bonding force between the formed coating 2 and the ceramic substrate 1.
When the composite slurry is coated, the composite slurry can partially enter the concave pits with the rough structure and the unevenness, 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.
Optionally, the preparation method of the 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 a sol-gel method.
As an optimized preparation method provided by the present application, before the coating 2 is formed, an intermediate transition layer 3 may be formed on the first surface 11 of the ceramic substrate 1, and the main material of the intermediate transition layer 3 is alumina or a composite material of zirconia and alumina. The double-layer coating formed on the ceramic substrate 1 can better prevent the impurity infiltration pollution in the ceramic substrate 1.
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.
The composite setter plate provided by the embodiment of the application comprises 99-Al 2 O 3 The ceramic matrix or corundum-mullite ceramic matrix is coated on any one of the ceramic matrix and the corundum-mullite ceramic matrix in a sol-gel way to form a coating 2 with a specific component, or form a double-layer coating of an intermediate transition layer 3 and the coating 2. Compared with the titanium alloy sintered massive zirconia or yttria setter plates used in the current market, the titanium alloy sintered massive zirconia or yttria setter plate has the advantages of low cost, long service life, good high-temperature stability, no product pollution and the like.
In a specific example of the present application, the step of preparing the composite paste comprises:
dissolving zirconium oxide containing crystal water in alcohol or water, and adding a colloidal particle generating agent to obtain a mixed solution; wherein the colloidal particle generating agent is urea;
y with the mass fraction of the substance of 2.5 to 3.5 percent 2 O 3 Adding into hydrochloric acid solution, heating until hydrochloric acid is evaporated to dryness, dissolving the obtained product in deionized water under ultrasonic condition to obtain Y 2 O 3 By YCl 3 Exists in the form of (1);
subjecting the obtained YCl to 3 Dispersing into the mixed solution, and then adding a dispersing agent to obtain yttrium-containing zirconium dioxide sol as composite slurry; wherein the dispersant is polyethylene glycol.
The preparation methods provided in the examples of the present application are described in detail below by examples 1 to 3.
Example 1
The preparation method of the composite setter plate comprises the following steps:
the ceramic matrix 1 is 99-Al 2 O 3 Ceramic matrix or corundum-mullite ceramic matrix.
wherein the first setting material comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria;
step 3, coating the composite slurry on the ceramic matrix 1 to form a wet blank, drying and sintering the wet blank, and forming a coating 2 on the ceramic matrix 1 to obtain the composite setter plate;
wherein the drying step comprises natural drying for 2 to 3 hours and drying for 5 to 7 hours at the temperature of between 45 and 65 ℃; the sintering step comprises heat preservation for 3-5 h at 1500-1600 ℃.
Example 2
Referring to fig. 1, the preparation method of the composite setter plate includes:
the ceramic matrix 1 is 99-Al 2 O 3 A ceramic matrix or a corundum-mullite ceramic matrix.
step 3, dispersing the first set material in the sol-gel sol, and fully reacting at 75-85 ℃ to obtain composite slurry; wherein the first setting material comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria;
step 4, coating the composite slurry on the first surface 11 of the ceramic matrix 1 to form a wet blank, drying and sintering the wet blank, and forming a coating on the first surface 11 of the ceramic matrix 1 to obtain the composite setter plate;
wherein the drying step comprises natural drying for 2 to 3 hours and drying for 5 to 7 hours at the temperature of between 45 and 65 ℃; the sintering step comprises heat preservation for 3-5 h at 1500-1600 ℃.
Example 3
Referring to fig. 2, the preparation method of the composite setter plate includes:
the ceramic matrix 1 is 99-Al 2 O 3 A ceramic matrix or a corundum-mullite ceramic matrix.
step 3, forming an intermediate transition layer 3 on the first surface 11 in a sol-gel manner after the step 2, wherein the main material of the intermediate transition layer 2 is a second setting material, and the second setting material comprises single crystal alumina or a dual-phase material formed by yttrium-stabilized zirconia and alumina;
step 4, dispersing the first set material in the sol-gel sol, and fully reacting at 75-85 ℃ to obtain composite slurry;
wherein the first setting material comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria;
step 5, coating the composite slurry on a first surface 11 of the ceramic substrate 1 to form a wet blank, drying and sintering the wet blank, and forming a coating on the first surface 11 to obtain the composite setter plate;
wherein the drying step comprises natural drying for 2-3 h and drying for 5-7 h at 45-65 ℃; the sintering step comprises heat preservation for 3-5 h at 1500-1600 ℃.
The difference between the above embodiment 1 and embodiment 2 is that the composite setter plate provided in embodiment 2 is additionally provided with a surface treatment on the surface of the ceramic substrate 1 to increase roughness, so as to improve the bonding force between the ceramic substrate 1 and the coating 2.
The embodiment 3 is added with the intermediate transition layer 3 on the basis of the embodiment 2. The intermediate transition layer 3 is additionally arranged before the coating 2 is formed on the ceramic matrix 1, so that the bonding strength between the coating 2 and the ceramic matrix 1 is improved, and the double-layer coating can better prevent the impurity permeation and pollution in the ceramic matrix 1. 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 example, it should be understood by those skilled in the art that the above examples are for illustration only and are 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 (14)
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 dispersing a first set material in a sol-gel solution to form composite slurry and then drying and sintering the composite slurry;
wherein the first setting material 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 of claim 1, wherein the ceramic matrix (1) has at least one first surface (11), at least a part of the first surface (11) is formed with a coarse structure having a roughness Ra ≧ 10 μm, the coarse structure having rugged pits;
the composite slurry can be embedded into the concave pits with the rough structures and the uneven parts, so that an embedded structure is formed between the coating (2) and the ceramic matrix (1).
4. The composite setter plate of any one of claims 1 to 3, wherein the bonding force between the coating (2) and the ceramic substrate (1) is 15MPa or more.
5. The composite setter plate as set forth in claim 4, further comprising an intermediate transition layer (3), the intermediate transition layer (3) being formed on the surface of the ceramic substrate (1) by a sol-gel method, the intermediate transition layer (3) being interposed between the ceramic substrate (1) and the coating layer (2) such that the coating layer (2) is spaced apart from the ceramic substrate (1).
6. The composite setter plate of claim 5, wherein the intermediate transition layer (3) is formed by: dispersing a second set material in the sol-gel solution, then coating the sol-gel solution on the surface of the ceramic substrate, and drying and sintering the sol-gel solution to obtain the ceramic substrate;
wherein the second setting material is single crystal alumina; alternatively, the first and second electrodes may be,
the second setting material is formed of yttrium-stabilized zirconia and alumina as a dual phase material; wherein the mass fraction of the yttrium-stabilized zirconia is 60-80%, and the mass fraction of the alumina is 20-40%.
7. Composite setter plate according to claim 5, characterized in that the thermal expansion coefficient of the intermediate transition layer (3) is set between that of the ceramic matrix (1) and that of the coating (2).
8. The composite setter plate of claim 1, wherein the ceramic matrix (1) comprises 99-Al 2 O 3 A ceramic matrix or a corundum-mullite ceramic matrix.
9. A method of making a composite setter plate as set forth in any one of claims 1 to 8, characterized in that the method of making comprises:
providing a ceramic substrate;
dispersing a first set material in the sol-gel sol, and fully reacting at a set temperature to obtain a composite slurry; wherein the first setting material comprises at least one of magnesia-stabilized zirconia, yttria-stabilized zirconia, calcia-stabilized zirconia, alumina-stabilized zirconia, and yttria;
and coating the composite slurry on the surface of the ceramic matrix to form a wet blank, and drying and sintering the wet blank to form a coating on the surface of the ceramic matrix to obtain the composite setter plate.
10. The method of making a composite setter plate as set forth in claim 9, comprising, in the step of preparing the composite slurry:
dissolving zirconium oxide containing crystal water in alcohol or water, and adding a colloidal particle generating agent to obtain a mixed solution; wherein the colloidal particle generating agent is urea;
y with the mass fraction of the substance of 2.5 to 3.5 percent 2 O 3 Adding into hydrochloric acid solution, heating until hydrochloric acid is evaporated to dryness, dissolving the obtained product in deionized water under ultrasonic condition to obtain Y 2 O 3 By YCl 3 Exists in the form of (a);
subjecting the obtained YCl to 3 Dispersing into the mixed solution, and then adding a dispersing agent to obtain yttrium-containing zirconium dioxide sol as composite slurry; wherein the dispersant is polyethylene glycol.
11. The method of claim 9, wherein the ceramic substrate is pre-machined to a predetermined shape.
12. The method for producing a composite setter plate as set forth in claim 9, wherein the set temperature is 75 ℃ to 85 ℃ in the step of producing the composite slurry.
13. The method of making a composite setter plate of claim 9, wherein in forming the coating: the drying step comprises natural drying for 2 to 3 hours and drying for 5 to 7 hours at the temperature of between 45 and 65 ℃; the sintering step comprises heat preservation for 3-5 h at 1500-1600 ℃.
14. The method of preparing a composite setter plate as set forth in claim 9, further comprising, before the step of coating the composite slurry on the surface of the ceramic substrate:
firstly forming a rough structure with the roughness Ra of more than or equal to 10 mu m on the surface of the ceramic matrix, wherein the rough structure is provided with rugged pits; and/or the presence of a gas in the atmosphere,
and forming an intermediate transition layer on the surface of the ceramic matrix by a sol-gel method.
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