CN114850472B - Method for coating ceramic particles and preparation method of composite material - Google Patents
Method for coating ceramic particles and preparation method of composite material Download PDFInfo
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- CN114850472B CN114850472B CN202210305408.4A CN202210305408A CN114850472B CN 114850472 B CN114850472 B CN 114850472B CN 202210305408 A CN202210305408 A CN 202210305408A CN 114850472 B CN114850472 B CN 114850472B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/101—Pretreatment of the non-metallic additives by coating
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- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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- C22C14/00—Alloys based on titanium
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
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- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
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Abstract
The invention provides a method for coating ceramic particles and a preparation method of a composite material. The coating method comprises the following steps: mixing ceramic particles with an adhesive, adding coating powder, and stirring to obtain ceramic particles coated by the coating powder; mixing the ceramic particles coated by the coating powder with polyvinyl alcohol, and drying to obtain ceramic particles with the surfaces attached with the coating powder and the polyvinyl alcohol; activating ceramic particles with coating powder and polyvinyl alcohol attached to the surfaces, and performing chemical plating by using plating solution after activation to obtain the ceramic particles coated by the coating powder-metal coating. The preparation method of the composite material comprises the following steps: preparing ceramic particles coated by a coating powder-metal coating; and carrying out pressureless infiltration treatment on the ceramic particles coated by the coating powder-metal coating and the metal matrix to obtain the composite material. According to the method, the protective layer formed by the polyvinyl alcohol can better coat the coating powder on the surface of the ceramic particles, so that a reaction interface can be better formed in the compounding process of the ceramic particles and the metal matrix, and the bonding performance is better.
Description
Technical Field
The invention relates to the technical field of ceramic composite materials, in particular to a method for coating ceramic particles and a preparation method of a composite material.
Background
The ceramic particles have the advantages of low density, high strength, wear resistance and corrosion resistance, the metal material has good plasticity and toughness, the combination of the ceramic particles and the metal material can generate the advantages of existing metal and the characteristics of ceramic, and the ceramic/metal matrix composite material has higher toughness, high hardness and high oxidation resistance.
However, the preparation of ceramic/metal matrix composites becomes quite difficult due to the poor wettability of the ceramic particles with the metal matrix. Attempts have been made to surface-treat ceramic particles before they are combined with a metal matrix to enhance their wettability. The chemical plating technology has the advantages of simple process, uniform plating layer, good bonding force with a substrate and the like, can plate on metal, can directly plate after pretreatment on the surface of a non-conductor such as ceramic, plastic, glass and the like, and is a widely applied ceramic particle surface treatment technology at present, wherein the plating of Ni, cu or Fe and alloys thereof is the main part. However, the plating element diffuses into the molten metal at high temperature and eventually disappears from the ceramic surface. Thus, some ceramic powders, carbide powders, and coated powders such as metallic powders (e.g., metallic titanium) that react with high temperature molten metal to form interfaces have been seen as new developments in core-shell materials.
At present, two preparation methods mainly exist for the core-shell structure, wherein the first method is to mix metal with low melting point such as Ni powder and the like with ceramic particles after ball milling, and then perform vacuum sintering, so that a stable core-shell structure can be obtained by the method, but the method has the defects of long preparation time in the ball milling and vacuum sintering processes; in addition, the method is limited by experimental conditions of high temperature and vacuum, and has the defects of high preparation temperature, high energy consumption and low yield. The second method is to directly bond the coating powder to the surface of the ceramic particles using a binder. The method can obtain the core-shell material in large batch, but in the preparation process of the ceramic/metal matrix composite material, the coating powder which is simply and mechanically combined is directly contacted with flowing high-temperature metal, so that the coating powder on the surface layer can be washed away; in addition, the adhesive of the inner layer can volatilize rapidly under the condition of long-time high temperature, and even the adhesive is entirely dropped into the molten metal from the surface of the ceramic particles, so that the integrity and uniformity of the coating layer formed by the coating powder can be affected to different degrees.
Disclosure of Invention
Aiming at the defects in the prior art, one of the purposes of the invention is to provide a method for obtaining ceramic particles coated by a coating powder-metal coating in a large scale at a low temperature in a short time, and the obtained ceramic particles coated by the coating powder-metal coating are cast with a metal matrix, so that a composite material with complete and uniform interface can be obtained.
In one aspect of the invention, a method of coating ceramic particles is provided, which may include the steps of: mixing ceramic particles with an adhesive, adding coating powder, and stirring to obtain ceramic particles coated by the coating powder; mixing the ceramic particles coated by the coating powder with polyvinyl alcohol, and drying to obtain ceramic particles with the surfaces attached with the coating powder and the polyvinyl alcohol; activating the ceramic particles with the coating powder and the polyvinyl alcohol attached to the surfaces, and plating by using plating solution, such as chemical plating, after activation to obtain the ceramic particles coated by the coating powder-metal coating.
In another aspect of the present invention, a method for preparing a composite material is provided, which may include the steps of: the ceramic particles coated by the coating powder-metal coating are prepared by the method for coating the ceramic particles; and casting the ceramic particles coated by the coating powder-metal coating and the metal matrix to obtain the composite material.
Compared with the prior art, the invention has the beneficial effects that at least one of the following is included:
(1) According to the method, the protective layer formed by the polyvinyl alcohol can enable the coating powder to be better coated on the surfaces of the ceramic particles, so that the coating powder is prevented from being separated from the ceramic particles and being dispersed into the activating solution.
(2) The method of the invention utilizes the metal layer formed after chemical plating to protect the coating powder, can avoid the ceramic particles coated by the coating powder from directly contacting with the metal-based liquid at high temperature to influence the integrity and uniformity of the coating layer, can better form a reactive interface in the compounding process of the ceramic particles and the metal-based, has better bonding performance, and can improve the bonding strength of the interface of the ceramic particles and the metal-based.
(3) The method can obtain ceramic particles coated by the coating powder-metal coating in a short time and in a large scale at a low temperature.
Drawings
The foregoing and other objects and features of the invention will become more apparent from the following description taken in conjunction with the accompanying drawings in which:
FIG. 1 shows ZTA p Ti/PVA before and after activation and ZTA p -appearance topography contrast map before and after Ti activation.
FIG. 2 shows ZTA p -Ti and ZTA p -microscopic morphology contrast before and after Ti/PVA activation.
FIG. 3 shows ZTA p -a surface profile of Ti/pva@cuni cross-section element.
FIG. 4 shows ZTA p -elemental surface profile at Ti/pva@cuni/HCCI interface.
Detailed Description
Hereinafter, a method of coating ceramic particles and a composite material manufacturing method according to the present invention will be described in detail with reference to the accompanying drawings and exemplary embodiments.
In one aspect, the invention provides a method of coating ceramic particles. In one exemplary embodiment of the method of coating ceramic particles of the present invention, the method may include the steps of:
and S01, mixing the ceramic particles with an adhesive, adding the coating powder, and stirring to obtain the ceramic particles coated by the coating powder.
S02, mixing the ceramic particles coated by the coating powder with the polyvinyl alcohol, and drying to obtain the ceramic particles coated by the coating powder and the polyvinyl alcohol.
S03, activating the ceramic particles coated by the coating powder and the polyvinyl alcohol, and performing chemical plating by using a plating solution after activation to obtain the ceramic particles coated by the coating powder-metal coating.
Further, the ceramic particles may be metal oxide ceramic particles, carbide ceramic particles, or boride ceramic particles. For example, ZTA ceramic particles (ZTA p ）、Al 2 O 3 Ceramic particles, tiC particles, siC particles, zrO 2 Ceramic particles, tiB 2 Particles or SiO 2 Ceramic particles. Of course, the kind of the ceramic particles of the present invention is not limited thereto, and may be WC particles or the like.
Further, the adhesive may be a water glass adhesive, a polyvinyl alcohol (PVA) adhesive, or the like. The binder is used for adhering the coating powder to the surface of the ceramic particles.
Further, the coating powder may be one or a combination of several of metal powder, ceramic powder, carbide powder and boride powder. For example, the metal powder may be Ti powder, ni powder, cu powder, or a mixture thereof, or the like. For example, when the ceramic particles are ZTA p When the coating powder is Ti powder, the ceramic particles coated by the obtained coating powder are ZTA p -Ti. The coating method can coat non-conductive ceramic powder, carbide powder and the like on the surfaces of the ceramic particles under the conditions of low temperature and simple process flow.
Further, the radial dimension of the coating powder may be 0.1 μm to 10 μm. The size of the coating powder is smaller than 0.1 mu m, and a coating layer formed on the surface of the ceramic particles is too compact, so that high-temperature molten metal cannot be cast and infiltrated when the composite material is prepared, and the composite effect is affected; the coating powder is too large in size, and the uniformity of coating is affected. For example, the radial dimension of the coating powder may be 0.3 μm to 8 μm or 1 μm to 7 μm.
Further, the purpose of adding polyvinyl alcohol (PVA) is to form a layer of protective film on the surface of the ceramic particles after the coating powder is coated, so that the coating powder can be prevented from being separated from the surface of the ceramic particles in the activation process and being dispersed in the activation liquid, and the coating powder can be better attached to the surface of the ceramic particles to form a layer of coating layer. Preferably, the mass concentration of PVA may be 1.5% -8.5%. If the mass concentration of PVA is lower than 1.5%, the formed protective film is too thin, and the coating powder can be separated from the surface of the ceramic particles and enter the activating solution during activation, so that the effect of preventing the coating powder from separating from the surface of the ceramic particles is not achieved, and the coating layer formed by the coating powder is affected; if the mass concentration of PVA is higher than 8.5%, the formed protective film is too thick, the protective film cannot be completely dissolved during activation, the final plating effect is affected, the activation effect is achieved by the fact that the protective film is too thick, the activation effect cannot be achieved on the coated powder, and the subsequent chemical plating is affected. And forming a proper protective film thickness, wherein a part of the protective film can be dissolved in the activation process, and the other part of the undissolved protective film plays a role in protecting, so that the activated and residual film is mixed on the surface of the coating powder, and the coating powder can be complete and active. Preferentially, the mass concentration of PVA can be 2.5% -3.5% (2.5 g/L-3.5 g/L), and in the mass concentration range, the formed protective film has moderate thickness, so that the activation effect of the coating powder can not be influenced while the coating powder is well prevented from separating from ceramic particles. Here, the mass concentration of PVA refers to the PVA mass/deionized water mass (for example, the mass concentration of PVA is 3%, and when the deionized water mass is 100g, 3g of PVA is added). PVA may be prepared by stirring at 500rpm for 6 hours at 85℃to give a viscous clear solution. Of course, the preparation of PVA of the present invention is not limited thereto, and PVA may be added to deionized water and stirred uniformly.
Further, after the ceramic particles coated by the coating powder are mixed with polyvinyl alcohol, the drying temperature can be 50-70 ℃. Drying in the above temperature range can form a protective film of polyvinyl alcohol on the surface of the ceramic particles, and can avoid the adhesion of the ceramic particles together due to the existence of the polyvinyl alcohol, so that the adhesion surfaces between the ceramic particles cannot be plated effectively. The drying time can be 1 to 2 minutes.
Further, activating the coated powder and the polyvinyl alcohol coated ceramic particles may include activating with an activating solution at a temperature of 150 ℃ to 200 ℃, for example, may be performed at 170 ℃. The purpose of the activation is to provide the particle surface with metal active sites to better plate the metal contained in the plating solution onto the ceramic particle surface. The activating solution may be Ni (Ac) 2 An activating solution of Ni (Ac) 2 The activating solution may be composed of Ni (Ac) 2 、NaH 2 PO 2 、C 2 H 6 O and H 2 O composition, wherein Ni (Ac) 2 、NaH 2 PO 2 、C 2 H 6 O and H 2 The mass concentration ratio of O can be 1 (0.5-1.5): (10-20): (1-3). For example, it may be 1:1:15:2. The activation time is required to activate all the ceramic particles coated by the coating powder, and can be adjusted according to the yield and the activation completeness, for example, the activation time can be 20-30 min, for example, 25min. Specifically, for ceramic particles ZTA with surface-adhered titanium powder and polyvinyl alcohol p Activation of Ti/PVA, possibly with Ni (Ac) 2 :NaH 2 PO 2 :C 2 H 6 O:H 2 The components with the mass concentration ratio of O=1:1:15:2 are the activating solution, and the activating solution is activated for 25min at 170 ℃ to obtain Ni activated ZTA p -Ti/PVA/Ni 2+ . Of course, the activating solution can also be PbCl 2 Activating solution or AgNO 3 Activating liquid.
Further, the plating solution may be a plating solution containing Ni element and/or Cu element. For example, the plating solution may contain nickel sulfate, or copper sulfate, or a mixture of nickel sulfate and copper sulfate.
For example, for a plating layer made of a CuNi alloy, the plating solution may contain nickel sulfate (NiSO 4 ·6H 2 O), copper sulfate (CuSO) 4 ·5H 2 O), sodium citrate (C) 6 H 5 Na 3 O 7 •2H 2 O), sodium hypophosphite (NaH) 2 PO 2 •H 2 O) boric acid (H) 3 BO 3 ) And choline chloride-ethylene glycol (ChCl-EG), wherein the concentration of nickel sulfate in the plating solution can be 25 g/L-35 g/L, copper sulfate (CuSO) 4 ·5H 2 The concentration of O) can be 25 g/L-35 g/L, and sodium citrate (C) 6 H 5 Na 3 O 7 •2H 2 The concentration of O) can be 28g/L to 33g/L, and the concentration of sodium hypophosphite (NaH) 2 PO 2 •H 2 The concentration of O) can be 27g/L to 38g/L, and boric acid (H) 3 BO 3 ) The concentration of (C) may be 13g/L to 17g/L, and the concentration of choline chloride-ethylene glycol (ChCl-EG) may be 0g/L to 40g/L. Mixing the coating powder, the ceramic particles coated by the polyvinyl alcohol and the plating solution, adjusting the pH to 9-10, and chemically plating for 30-70 min at the temperature of 50-80 ℃ under the conditions that the rotating speed is 80-120 rpm. For example, the concentration of nickel sulfate in the plating solutionCan be 30g/L, copper sulfate (CuSO) 4 ·5H 2 The concentration of O) may be 30g/L, sodium citrate (C) 6 H 5 Na 3 O 7 •2H 2 The concentration of O) may be 30g/L, sodium hypophosphite (NaH) 2 PO 2 •H 2 The concentration of O) may be 32g/L, boric acid (H) 3 BO 3 ) The concentration of (C) may be 15g/L and the concentration of choline chloride-ethylene glycol (ChCl-EG) may be 25g/L. Mixing the coating powder, ceramic particles coated by polyvinyl alcohol and the plating solution, adjusting the pH to 9.2, and carrying out chemical plating for 50min at the temperature of 65 ℃ under the condition that the rotating speed is 100 rpm. For example, ZTA for Ni activation p -Ti/PVA/Ni 2+ The ZTA coated by Ti-CuNi can be obtained after plating by the plating solution, namely ZTA p -Ti/PVA@CuNi。
In another aspect of the invention, a method of preparing a composite material is provided. In one exemplary embodiment of the composite preparation method of the present invention, the method may include the steps of:
and S100, mixing the ceramic particles with an adhesive, adding the coating powder, and stirring to obtain the ceramic particles coated by the coating powder.
S101, mixing the ceramic particles coated by the coating powder with polyvinyl alcohol, and drying to obtain the ceramic particles coated by the coating powder and the polyvinyl alcohol.
S102, activating the ceramic particles coated by the coating powder and the polyvinyl alcohol, and carrying out chemical plating by using a metal-containing plating solution to obtain the ceramic particles coated by the coating powder-metal coating.
And S103, casting the ceramic particles coated by the coating powder-metal coating and the metal matrix to obtain the composite material.
The steps S100 to S102 are the same as the steps S01 to S03, and the description thereof will not be repeated here. At present, in the process of preparing a ceramic/metal matrix composite material in the prior art, coating powder is directly adhered to the surface of ceramic particles by using an adhesive and then is directly cast with a metal matrix, and the method has the following problems: on the one hand, the coating powder which is simply and mechanically combined is directly contacted with flowing high-temperature metal, so that the coating powder on the surface layer can be washed away; on the other hand, the adhesive can volatilize rapidly under the condition of long-time high temperature, and even the adhesive falls off from the surface of the ceramic particles to the high-temperature molten metal, so that the integrity and uniformity of the coating layer can be affected to different degrees. The ceramic particles coated by the coating powder-metal coating prepared in the steps S100-S102 can ensure that the coating powder is completely and uniformly coated on the surfaces of the ceramic particles. Through can form one deck metal coating on the coating surface after the electroless plating, avoided cladding powder and the high temperature metal direct contact of flow, avoid cladding powder to be washed away by the molten metal, cladding powder and the metal layer that forms after the electroless plating can make ceramic particle and metal base form reaction type interface better in the compounding process, and the binding performance is better.
Further, the metal base may be titanium base, copper base, iron base or steel base, for example, the metal base may be HCCI high chromium cast iron. Of course, the metal base of the present invention is not limited thereto, and may be, for example, vanadium base, aluminum base, or the like.
Further, the casting treatment may be a treatment in a pressureless impregnation manner.
For a better understanding of the present invention, the content of the present invention is further elucidated below in connection with the specific examples, but the content of the present invention is not limited to the examples below.
Example 1
Step 2, ZTA p Mixing Ti with PVA with mass concentration of 3%, and drying at 60deg.C for 1min to obtain coated powder Ti and PVA coated ZTA p ZTA, i.e p -Ti/PVA。
Step 3, ZTA is carried out p Ti/PVA and Ni (Ac) 2 Mixing the activating solutions, and activating at 170deg.C for 25min to obtain activated ceramic granule ZTA p -Ti/PVA/Ni 2+ Wherein Ni (Ac) 2 The activating solution is Ni (Ac) 2 、NaH 2 PO 2 、C 2 H 6 O and H 2 And the mass concentration ratio of O is 1:1:15:2.
And 4, preparing a CuNi plating solution. Nickel sulfate (NiSO) in CuNi plating solution 4 ·6H 2 O) at a concentration of 30g/L, copper sulfate (CuSO) 4 ·5H 2 The concentration of O) may be 30g/L, sodium citrate (C) 6 H 5 Na 3 O 7 •2H 2 The concentration of O) may be 30g/L, sodium hypophosphite (NaH) 2 PO 2 •H 2 The concentration of O) may be 32g/L, boric acid (H) 3 BO 3 ) The concentration of (C) may be 15g/L and the concentration of choline chloride-ethylene glycol (ChCl-EG) may be 10g/L.
Step 5, the activated ceramic particles ZTA p -Ti/PVA/Ni 2+ Mixing with CuNi plating solution, adjusting pH to 9.5, and chemically plating at 65deg.C at rotation speed of 100rpm for 50min to obtain CuNi coated ZTA p Ti/PVA, ZTA p -Ti/PVA@CuNi。
Step 6, ZTA p Carrying out pressureless infiltration treatment on Ti/PVA@CuNi and high-chromium cast iron to obtain a composite material ZTA p -Ti/PVA@CuNi/HCCI。
Comparative example 1
Step 100, ZTA particles (ZTA p ) Mixing with water glass adhesive, adding Ti powder with particle size of 4 μm, mechanically stirring to obtain coated powder Ti coated ZTA particles, namely ZTA p -Ti。
Step 200, ZTA p Ti and Ni (Ac) 2 Mixing the activating solutions, and activating at 170deg.C for 25min to obtain activated ceramic granule ZTA p -Ti/Ni 2+ Wherein Ni (Ac) 2 The activating solution is Ni (Ac) 2 、NaH 2 PO 2 、C 2 H 6 O and H 2 And the mass concentration ratio of O is 1:1:15:2.
Step 300, preparing a CuNi plating solution. The concentration of nickel sulfate in the CuNi plating solution is 30g/L, and the concentration of copper sulfate (CuSO 4 ·5H 2 The concentration of O) may be 30g/L, sodium citrate (C) 6 H 5 Na 3 O 7 •2H 2 The concentration of O) may be 30g/L, sodium hypophosphite (NaH) 2 PO 2 •H 2 The concentration of O) may be 32g/L, boric acid (H) 3 BO 3 ) The concentration of (C) may be 15g/L and the concentration of choline chloride-ethylene glycol (ChCl-EG) may be 10g/L.
Step 400, activating the ceramic particles ZTA p -Ti/Ni 2+ Mixing with CuNi plating solution, adjusting pH to 9.5, and chemically plating at 65deg.C at rotation speed of 100rpm for 50min to obtain Ti-CuNi coated ZTA, namely ZTA p -Ti@CuNi。
Step 500, ZTA p Performing pressureless infiltration treatment on Ti@CuNi and high-chromium cast iron to obtain a composite material ZTA p -Ti@CuNi/HCCI。
Comparative example 1 differs from example 1 in that comparative example 1 was not subjected to step 2 of example 1, i.e. ZTA was not taken p Ti is mixed with PVA, the other steps being the same.
As shown in fig. 1, fig. 1 shows ZTA of example 1 p ZTA of Ti/PVA before and after activation and comparative example 1 p -appearance topography contrast map before and after Ti activation. White is a small crucible, figure (a 1 And c 1 ) The green liquid is an activating liquid. Fig. (a) shows the original ceramic particles as off-white. After step 1 (or step 100), the ZTA particles are coated with Ti powder and then are gray black, as shown in fig. (b). And after step 2, at ZTA p After coating the Ti particles with a layer of PVA, the ceramic remains grey-black, but the surface presents a distinct gloss, as shown in figure (c). When PVA is not coated, ti powder is separated from the surfaces of ZTA ceramic particles, and the activating solution becomes black as shown in a graph (b 1). While ZTA coated with PVA p Ti, the color of which is still light green, as shown in figure (c 1), is consistent with the color of (a 1) when the titanium is not coated, which proves that the PVA film well protects the Ti powder coated by ZTA particles. After sintering at high temperature for 30min, the color of the sintered ZTA ceramic particles was observed, and the graph (a 2 ) The original ZTA particles of the catalyst are gray, and Ni (Ac) in the activated liquid is used 2 After being reduced by sodium hypophosphite, ni is activated. And graph (b) 2 ) In which no PVA protection is caused by mixing Ti powder into the activating solution, resulting in ZTA after sintering p Black in color. Graph (c) 2 ) In ZTA p The color of the activated Ti-coated PVA is equal to (a) 2 ) No difference, thus indicating that PVA can be used for ZTA at high temperature p Ti plays a protective role and does not affect its activation for the next electroless plating process.
FIG. 2 shows ZTA of example 1 p ZTA of Ti/PVA before and after activation and comparative example 1 p -a microscopic morphology contrast map before and after Ti activation. ZTA particles (figure a) coated with Ti powder p The Ti powder on the surface of the Ti particles is loose (FIG. b), at ZTA p After coating a layer of PVA on the basis of Ti particles, ti powder is coated inside, and the surface only presents a smooth layer of PVA film. ZTA without PVA coating p Spherical particles of CuNi alloy are observed on the surface of the Ti@CuNi particles, and the bare ZTA surface (as shown in figure b 1 ) The method comprises the steps of carrying out a first treatment on the surface of the And ZTA obtained by plating after PVA coating p The surface of the Ti@CuNi particles is uniformly coated by CuNi alloy spherical particles (as shown in figure c 1 ). From the cross section, it can also be seen that ZTA obtained by coating with PVA and then plating p Ti@CuNi particles, wherein Ti powder is completely and uniformly coated on the surfaces of ZTA particles (as shown in figure c 2 ) But ZTA obtained by plating without PVA coating p Ti@CuNi particles, ti powder loss in large amounts (as in Panel b 2 ）。
FIG. 3 shows ZTA prepared in example 1 p -a surface profile of Ti/pva@cuni cross-section element. FIG. (a) is ZTA prepared by step 5 p Appearance of Ti/PVA@CuNi particles, and ZTA coated with copper and nickel p The Ti particles were smooth in surface and had a red metallic luster. The surface distribution of the element in the graph b shows that the mixture of Ti powder and water glass is uniformly coated on the surface of ZTA particles by the CuNi coating.
FIG. 4 shows ZTA prepared in example 1 p -ti@cuni/HCCI interface element profile. FIG. (a) is ZTA prepared in step 6 p -appearance of ti@cuni/HCCI composite material, composite material void free defects. From the graph (b) and the surface distribution of the elements thereof, under the casting infiltration effect of the high-temperature molten iron, the CuNi coating is melted and reacts with Ti powder, and forms a uniform and stable reactive interface with the elements in the high-chromium cast iron.
Although the present invention has been described above by way of the combination of the exemplary embodiments, it should be apparent to those skilled in the art that various modifications and changes can be made to the exemplary embodiments of the present invention without departing from the spirit and scope defined in the appended claims.
Claims (10)
1. A method of coating ceramic particles comprising the steps of:
mixing ceramic particles with an adhesive, adding coating powder, and stirring to obtain ceramic particles coated by the coating powder;
mixing the ceramic particles coated by the coating powder with polyvinyl alcohol, and drying to obtain ceramic particles with the surfaces attached with the coating powder and the polyvinyl alcohol;
activating ceramic particles with coating powder and polyvinyl alcohol attached to the surfaces, and plating by using plating solution after activation to obtain the ceramic particles coated by the coating powder-metal coating.
2. The method of coating ceramic particles according to claim 1, wherein the drying temperature is 50 ℃ to 70 ℃.
3. The method of coating ceramic particles according to claim 1 or 2, wherein the coating powder is one or more of a metal powder, a ceramic powder, a carbide powder and a boride powder.
4. The method of coating ceramic particles according to claim 1 or 2, wherein the radial dimension of the coating powder is 0.1 μm to 10 μm.
5. The method of coating ceramic particles according to claim 1 or 2, wherein the mass concentration of polyvinyl alcohol is 1.5% -8.5%.
6. The method of coating ceramic particles according to claim 1 or 2, wherein the plating solution is one or a mixture of two of a nickel-containing plating solution and a copper-containing plating solution.
7. The method of coating ceramic particles according to claim 1 or 2, wherein activating the ceramic particles with the surface-coating powder and the polyvinyl alcohol comprises mixing the ceramic particles with the surface-coating powder and the polyvinyl alcohol with an activating liquid and then activating at a temperature of 150 ℃ to 200 ℃.
8. The method of coating ceramic particles according to claim 7, wherein the activating solution is Ni (Ac) 2 Activating solution, pbCl 2 Activating solution or AgNO 3 Activating liquid.
9. A method of preparing a composite material, comprising the steps of:
preparing coated powder-metal coated ceramic particles by the method of coating ceramic particles according to any one of claims 1 to 8;
and casting the ceramic particles coated by the coating powder-metal coating and the metal matrix to obtain the composite material.
10. The method of claim 9, wherein the metal base is titanium base, copper base, iron base, or steel base.
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