CN115819110A - Metallized porous ceramic composite material and preparation method thereof - Google Patents
Metallized porous ceramic composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of ceramic materials, in particular to a metallized porous ceramic composite material and a preparation method thereof, wherein the preparation method of the metallized porous ceramic composite material comprises the following steps: (A) Carrying out dry ball milling on high-purity quartz sand or silicon carbide, then sieving to obtain superfine powder, adding ferronickel powder, boron oxide, a sintering aid, glass powder and a pore-forming agent, and carrying out low-speed ball milling and fully mixing to obtain mixed powder; (B) Mixing the mixed powder with a polyvinyl alcohol aqueous solution, and forming by adopting a dry pressing method to obtain a ceramic green body; (C) And drying the ceramic green body in a drying box, then preserving heat in a program temperature-controlled box type furnace, and cooling to room temperature along with the furnace. The dry pressing method adopted by the invention has simple process, the metal alloy powder is added to form a metal phase in the ceramic, the metal phase is combined with the ceramic to improve the strength of the three-dimensional framework of the ceramic, the matrix can form metallurgical bonding with the heating layer, the strength is improved, and the oil guiding speed of the metallized porous ceramic is accelerated.
Description
Technical Field
The invention relates to the field of ceramic materials, in particular to a metallized porous ceramic composite material and a preparation method thereof.
Background
In the existing partial atomizing heating structure, for example, an atomizing core in an aerosol generating device, a porous ceramic material is used as a base, a heating film is disposed on the base, and an atomizing substrate absorbed by the base is heated and atomized by the heating film to generate aerosol. The porous ceramic material is adopted as the matrix, so that the atomized matrix is uniformly distributed on the matrix, and the heating effect is better.
At present, diatomite is mostly used as a base material of the porous ceramic material, and the diatomite has micro pores, so that native partial pores can be reserved after sintering, and the porous ceramic material can be sintered and formed by adding a binder and a pore-forming agent. Due to the micropores of the diatomite, the porosity of the porous ceramic material formed after sintering can reach the standard, but the diatomite needs to be sintered at high temperature, the preparation process is complex, the preparation flow is long, most of silicon dioxide components contained in the diatomite belong to amorphous silicon dioxide, the strength for crystal form transformation and increase in the high-temperature firing process is limited, so that the three-dimensional framework of the porous ceramic material is fragile and poor in toughness, and a matrix made of the porous ceramic material is easy to break when other parts are assembled, so that the powder falling phenomenon is generated, and the service life and the safety of the matrix are influenced; meanwhile, the porous ceramic material substrate has poor binding force with the metal heating film, and the film substrate is easy to separate and layer in the atomization process, so that burnt flavor is easy to generate, and the taste of aerosol is influenced. According to the technical scheme of the existing porous ceramic, diatomite is mainly used as a main substrate material, the diatomite has micropores, the original part of the micropores can be reserved after sintering, and sintering forming is carried out by adding a certain bonding agent and a certain pore-forming agent.
On one hand, due to the micro pores of the diatomite, the porosity after sintering is ensured, but the main SiO2 component in the diatomite belongs to amorphous SiO2, the strength for crystal form transformation and increase in the high-temperature firing process is limited, and the ceramic matrix is easy to break and generate the powder falling phenomenon during assembly.
On the other hand, the bonding force between the ceramic substrate taking the diatomite as the main body and the metal heating film is poor, a stable metallurgical bonding layer cannot be formed between the heating film and the substrate, and the film substrate is easily separated from the layering in the atomization process, so that the burnt smell is generated, and the use experience of the product is influenced.
Chinese patent application document CN114988903A discloses a high-strength low-shrinkage porous ceramic and a preparation method thereof, and the high-strength low-shrinkage porous ceramic comprises 6-12 parts of a framework material A, 48-54 parts of a framework material B, 15-24 parts of a first pore-forming agent, 15-24 parts of a second pore-forming agent and 1-2 parts of a binder. The porous ceramic is prepared by adopting a pore-forming agent adding method, and meanwhile, the two pore-forming agents, namely the first pore-forming agent and the second pore-forming agent, are added, so that the temperature range of gas released by the pore-forming agent during combustion is widened, the shrinkage rate of the porous ceramic is reduced, and the porous ceramic product with higher porosity and bending strength is obtained. However, the preparation process of the porous ceramic applied by the patent of the invention is relatively complex, and the bending strength of the prepared porous ceramic product is still insufficient and is only 14.56-15.96MPa.
The Chinese invention patent application document CN115180932A discloses an in-situ synthesized mullite porous ceramic based on high-sodium industrial alumina and a preparation method thereof, and the technical scheme is as follows: mixing high-sodium industrial alumina fine powder and tertiary alumina fine powder in a mass ratio of 1: 2.3-3.3 in a ball mill to obtain a mixture; adding a polyvinyl alcohol solution with the weight percent of 10-20% of the mixture, and mixing to obtain ceramic powder; pressing the ceramic powder under the condition of 80-150 MPa, and drying at the temperature of 100-110 ℃; then placing the mixture into a muffle furnace, preserving the heat for 2 to 3 hours under the conditions of air atmosphere and 1550 to 1650 ℃, and cooling to obtain the mullite porous ceramic synthesized in situ on the basis of the high-sodium industrial alumina. The porosity of the porous ceramic prepared by the patent application of the invention is 33-40%, the bending strength is 90-110MPa, and the strength and the air permeability are insufficient.
Disclosure of Invention
In order to overcome the defects of long flow and complex process of the preparation process in the prior art; the prepared porous ceramic material has the defects of poor combination of a heating film and a substrate, short service life, insufficient strength, insufficient toughness, powder falling phenomenon and the like.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
the invention provides a preparation method of a metallized porous ceramic composite material, which is applied to an electronic cigarette atomizer and can also be applied to other ceramic atomization related fields. The method comprises the following specific steps:
(A) Pretreatment and powder mixing
Mixing high-purity quartz sand or silicon carbide and zirconia balls according to the mass ratio of 1: performing dry ball milling at the ratio of 0.5-1.5, then sieving with a 200-600 mesh sieve to obtain superfine quartz powder or silicon carbide powder, adding ferronickel alloy powder, boron oxide (B2O 3), a sintering aid, glass powder and a pore-forming agent into the superfine powder, wherein the softening point of the glass powder is 500-800 ℃, and fully and uniformly mixing the glass powder by low-speed ball milling to obtain mixed powder;
(B) Porous ceramic forming
Mixing the mixed powder with a polyvinyl alcohol aqueous solution, stirring and uniformly mixing, and forming by adopting a dry pressing method to obtain a ceramic green body;
(C) Sintering and forming of metallized porous ceramics
Drying the ceramic green body in a drying box, heating the ceramic green body in a program temperature-controlled box furnace at the speed of 2-10 ℃/min to reach 1100-1180 ℃, preserving the heat for 0.5-1h, and cooling the ceramic green body to room temperature along with the furnace to obtain the metallized porous ceramic composite material.
Preferably, the mixed powder comprises, by mass, 40-50% of silicon carbide or quartz powder, 3-5% of boron oxide (B2O 3), 3-6% of a sintering aid, 8-15% of glass powder, 3-8% of nickel-iron alloy powder and 30-40% of a pore-forming agent.
Preferably, the SiO2 content in the adopted quartz sand is more than 99 percent, or the purity of the silicon carbide is more than 99 percent.
Preferably, the nickel-iron alloy powder contains 50-65% of nickel and the balance of iron by mass percent, and the mesh number is 300-400 meshes.
Preferably, the sintering aid is CaCO3; the pore-forming agent is one or all of PMMA (polymethyl methacrylate) and PS (polystyrene), and the particle size is 50-200um.
Preferably, the mass percentage concentration of the polyvinyl alcohol aqueous solution is 0.9-1.0%, and the mass of the polyvinyl alcohol aqueous solution is 5-7% of the mass of the mixed powder.
Preferably, the pressure of the dry pressing molding is 400-600MPa, and the dwell time is 5-10min.
Preferably, the temperature in the drying oven is 70-90 ℃, and the drying time in the drying oven is 4-6h.
Preferably, the boron oxide (B2O 3) is all in the form of particles or powder, and the mesh number is 300-400.
The metallized porous ceramic composite material prepared by the method has the advantages of apparent porosity of 50-60%, pore diameter of 16-40um and bending strength of 130-200MPa.
The dry pressing method adopted by the invention has simple process, the metal alloy powder is added to form a metal phase in the ceramic, the metal phase is combined with the ceramic to improve the three-dimensional framework strength of the ceramic, meanwhile, the matrix can also form metallurgical combination with the heating layer, the service life is prolonged, and the oil guiding speed of the metallized porous ceramic is accelerated. The ceramic is metallized by adding the ferronickel alloy into the ceramic powder, the three-dimensional framework in the matrix is jointly composed of a ceramic phase and a metal phase, compared with a single ceramic phase, the formation of the metal phase changes the original heat conductivity coefficient and thermal expansion coefficient of the ceramic matrix, the performance of the metallized composite material is changed from the typical brittleness and hardness of the ceramic phase to the toughness and toughness of the metal phase, the comprehensive mechanical property is greatly improved, the original mechanical adhesion and combination between the heating film and the matrix is changed into metallurgical combination, the single ceramic phase and the heating film cause the matrix to break during atomization due to the great difference of the thermal expansion coefficients, and the change of the heat conductivity coefficient and the thermal expansion coefficient of the composite material can better match the heating film and the metallurgical combination layer formed by the heating film, so that the service life is obviously prolonged.
The metalized porous ceramic composite material prepared by the invention has obviously improved strength, can meet the manufacturing and assembling requirements under various composite stress conditions, forms metallurgical bonding with the heating layer of the thick film printing and thin film coating, greatly prolongs the service life of the atomizing core, meets the high-power atomizing requirement, and accelerates the oil guiding speed of the metalized porous ceramic composite material.
Detailed Description
In terms of explanation, the terms "ultrafine powder", "ultrafine quartz powder" and "ultrafine silicon carbide powder" as used in the present specification and claims refer to respective powders having a particle size of 2 to 90 μm.
The following describes specific embodiments of the present invention in terms of material composition, mixture ratio, specific preparation steps, test results, and the like.
The porosity, the pore diameter of the through hole and the bending strength value of the metallized porous ceramic composite material prepared in all the examples are measured.
Porosity: the apparent porosity, i.e. porosity, of the porous ceramic was tested according to the national standard GB/T1996-1996. The percentage of the volume of open pores in a porous material to the total volume of the material is called the apparent porosity and the standard specifies their formula for calculation as follows:
q-apparent porosity of sample,%;
m 1-drying quality of the sample;
m 2-mass of saturated sample in air;
m 3-mass of saturated sample in water;
wherein the saturated sample can be prepared by vacuum pumping or boiling.
Through hole diameter: the pore diameter of the porous ceramic material is measured according to a test method of the pore diameter of the porous ceramic according to the national standard GB/T1967-1996, and the specific operation is that a porous ceramic sample is immersed in test liquid (distilled water) and then immersed in the test liquid, gas (air or nitrogen) is slowly introduced into the porous ceramic sample, the pressure is gradually increased on the porous ceramic sample, so that the test gas is forced to pass through the porous ceramic sample in saturated water, the minimum pressure required when first bubbles are formed on the surface of the porous ceramic sample is obtained, and the maximum capillary pore diameter of the porous ceramic sample can be calculated.
Bending strength: the ceramic material was tested for flexural strength according to the national standard GB/T4741-1999. The standard specifies that the room temperature bending strength of ceramic materials is measured by a three-point load method, and a bending strength tester is used for testing the bending strength.
Example 1:
1. composition and proportion of mixed powder
2. The concrete preparation steps
(A) Pretreatment and powder mixing
(a) Mixing quartz sand and zirconia balls according to the mass ratio of 1:1, performing dry ball milling for 2 hours, and sieving with a 300-mesh sieve to obtain superfine quartz powder;
(b) Adding a sintering aid CaCO3, ferronickel powder, boron oxide, glass powder and a pore-forming agent PMMA into the superfine quartz powder, and fully and uniformly mixing the materials through low-speed ball milling to obtain mixed powder;
(B) Porous ceramic forming
(a) Mixing the mixed powder with a polyvinyl alcohol aqueous solution, wherein the mass percentage concentration of the polyvinyl alcohol aqueous solution is 1.0 percent, the mass of the polyvinyl alcohol aqueous solution is 6 percent of the mass of the mixed powder, and stirring and mixing
Mixing uniformly;
(b) Forming by dry pressing method under 400-600MPa for 5-10min to obtain ceramic green body;
(C) Low temperature sintering
(a) Drying the ceramic green body in a drying oven at 85 ℃ for 4 hours;
(b) Then heating up in a program temperature control box type furnace at the speed of 5 ℃/min to achieve 1120 ℃ and preserving heat for 0.5h;
(c) Cooling to room temperature along with the furnace.
3. Test results
The basic properties of the prepared metallized porous ceramic composite material are determined as follows:
example 2:
1. composition and proportion of mixed powder
2. The concrete preparation steps
(A) Pretreatment and powder mixing
(a) Mixing quartz sand and zirconia balls according to the mass ratio of 1:1, performing dry ball milling for 2 hours, and sieving with a 300-mesh sieve to obtain superfine quartz powder;
(b) Adding a sintering aid CaCO3, ferronickel powder, boron oxide, glass powder and a pore-forming agent PMMA into the superfine quartz powder, and fully and uniformly mixing the materials through low-speed ball milling to obtain mixed powder;
(B) Porous ceramic forming
(a) Mixing the mixed powder with a polyvinyl alcohol aqueous solution, wherein the mass percentage concentration of the polyvinyl alcohol aqueous solution is 1.0 percent, and the mass of the polyvinyl alcohol aqueous solution is 6 percent of the mass of the mixed powder, stirring and mixing
Mixing uniformly;
(b) Forming by dry pressing method under 400-600MPa for 5-10min to obtain ceramic green body;
(C) Low temperature sintering
(a) Drying the ceramic green body in a drying oven at 85 ℃ for 4 hours;
(b) Then heating up in a program temperature control box type furnace at the speed of 5 ℃/min to achieve 1120 ℃ and preserving heat for 0.5h;
(c) Cooling to room temperature along with the furnace.
3. Test results
The basic properties of the prepared metallized porous ceramic composite material are determined as follows:
| porosity of the material | Aperture of through hole | Bending strength |
| 53.15％ | 21.26um | 172MPa |
The preparation method adopts a dry pressing process which is simple, the melting temperature of the nickel-iron alloy is obviously reduced by adding boron oxide, the nickel, iron and boron elements and the Si element in the ceramic powder form a NiFeBSi amorphous alloy metal phase in the high-temperature sintering process and are connected with the matrix through non-covalent bonds and covalent bonds, a continuous metal phase is formed in the porous ceramic three-dimensional framework after sintering, the metal phase is combined with the ceramic phase to improve the strength of the ceramic three-dimensional framework, meanwhile, the matrix can also form metallurgical combination with the heating layer to improve the service life, and the oil guiding speed of the metallized porous ceramic is accelerated. The ceramic is metallized by adding the ferronickel alloy into the ceramic powder body, the three-dimensional framework in the matrix is jointly formed by the ceramic phase and the metal phase, compared with a single ceramic phase, the formation of the metal phase changes the original heat conductivity coefficient and thermal expansion coefficient of the ceramic matrix, the performance of the metallized composite material is changed from the typical brittleness and hardness of the ceramic phase to the toughness and toughness of the metal phase, the comprehensive mechanical property is greatly improved, the original mechanical adhesion and combination between the heating film and the matrix is changed into metallurgical combination, the single ceramic phase and the heating film cause the matrix to break during atomization due to the great difference of the thermal expansion coefficients, the change of the heat conductivity coefficient and the thermal expansion coefficient of the composite material can better match the heating film and the metallurgical combination layer formed by the heating film, the service life can be obviously prolonged, and the requirement of high-power atomization on the whole atomization core is also met.
The metalized porous ceramic composite material prepared by the invention has obviously improved strength, can meet the manufacturing and assembling requirements under various composite stress conditions, forms metallurgical bonding with the heating layer of the thick film printing and thin film coating, greatly prolongs the service life of the atomizing core, meets the high-power atomizing requirement, and accelerates the oil guiding speed of the metalized porous ceramic composite material.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and modifications and variations of the present invention are also intended to fall within the scope of the appended claims. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. A preparation method of a metallized porous ceramic composite material comprises the following steps:
(A) Pretreatment and powder mixing
Mixing high-purity quartz sand or silicon carbide and zirconia balls according to the mass ratio of 1: performing dry ball milling at the ratio of 0.5-1.5, then sieving with a 200-600 mesh sieve to obtain superfine quartz powder or silicon carbide powder, adding ferronickel alloy powder, boron oxide, a sintering aid, glass powder and a pore-forming agent into the superfine powder, wherein the softening point of the glass powder is 500-800 ℃, and performing low-speed ball milling and fully mixing to obtain mixed powder;
(B) Porous ceramic forming
Mixing the mixed powder with a polyvinyl alcohol aqueous solution, stirring and mixing uniformly, and forming by adopting a dry pressing method to obtain a ceramic green body;
(C) Sintering and forming of metallized porous ceramics
Drying the ceramic green body in a drying box, then heating in a program temperature-controlled box furnace at the speed of 2-10 ℃/min to reach 1100-1180 ℃, preserving heat for 0.5-1h, and cooling to room temperature along with the furnace.
2. The method for preparing the ceramic composite material according to claim 1, wherein the mixed powder comprises, by mass, 40-50% of silicon carbide or quartz powder, 3-5% of boron oxide, 3-6% of a sintering aid, 8-15% of glass powder, 3-8% of nickel-iron alloy powder and 30-40% of a pore-forming agent.
3. The method for preparing a ceramic composite material according to claim 1 or 2, wherein the quartz sand used has a SiO2 content of more than 99% or a silicon carbide purity of more than 99%.
4. The method for preparing a ceramic composite material according to claim 1 or 2, wherein the nickel-iron alloy powder contains 50 to 65 mass percent of nickel and the balance of iron, and the mesh number is 300 to 400.
5. The method for preparing the ceramic composite material as claimed in claim 1 or 2, wherein the sintering aid is CaCO3, and the pore-forming agent is one or both of polymethyl methacrylate and polystyrene.
6. The preparation method of the ceramic composite material according to claim 1 or 2, wherein the mass percentage concentration of the polyvinyl alcohol aqueous solution is 0.9-1.0%, and the mass of the polyvinyl alcohol aqueous solution is 5-7% of the mass of the mixed powder.
7. The method for preparing a ceramic composite material according to claim 1 or 2, wherein the pressure for the dry-pressing molding is 400 to 600MPa, and the dwell time is 5 to 10min.
8. The method of claim 1 or 2, wherein the temperature in the drying oven is 70-90 ℃ and the drying time in the drying oven is 4-6h.
9. The method of claim 1 or 2, wherein the boron oxide is entirely in the form of particles or powder, and has a mesh size of 300 to 400 mesh.
10. A metallized porous ceramic composite material prepared by the method of any one of claims 1-9, having a porosity of 50-60%, a pore size of 16-40um, and a flexural strength of 130-200MPa.
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