CN115057702B - Zirconia powder molding material for additive manufacturing and preparation method and construction process thereof - Google Patents
Zirconia powder molding material for additive manufacturing and preparation method and construction process thereof Download PDFInfo
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Abstract
The application belongs to the field of rapid forming materials, and in particular relates to a zirconium dioxide powder forming material for additive manufacturing, a preparation method and a construction process thereof, wherein the forming material comprises the following components in percentage by mass: 8 to 15 percent of sodium silicate solution, 1 to 3 percent of silicone-acrylic emulsion, 0.5 to 2 percent of bis (dioctyl oxy pyrophosphato) ethylene titanate chelate, 1 to 3 percent of thixotropic agent, 1 to 2 percent of filling material, 60 to 75 percent of yttrium-stabilized zirconium dioxide powder and 12 to 18 percent of deionized water. The new composition of the molding material provided by the application can ensure that the molding material has excellent thixotropic property and rheological property, and can be better suitable for additive manufacturing.
Description
Technical Field
The application belongs to the field of rapid forming materials, and particularly relates to a zirconium dioxide powder forming material for additive manufacturing, a preparation method and a construction process thereof.
Background
The zirconium dioxide ceramic filter element has high temperature resistance, chemical corrosion resistance, good mechanical strength and filtering adsorption performance, and is widely applied to the aspects of heat exchange materials, automobile tail gas devices, molten metal filtering purification, industrial sewage treatment and the like.
The indexes such as aperture ratio and aperture diameter depend on experience of operators in the current production process, so that the production rejection rate is high, and the complex fine structure is difficult to realize. And thin and brittle ceramic structures are easily produced during sintering, and the fragile structures can be broken due to the pressure used, so that the quality of a user product is influenced.
Disclosure of Invention
Aiming at the technical problems, the application provides a zirconium dioxide powder molding material which has excellent thixotropic property and rheological property and can be better suitable for additive manufacturing, and the adopted technical scheme is as follows:
the zirconium dioxide powder forming material for additive manufacturing comprises the following components in percentage by mass: 8 to 15 percent of sodium silicate solution, 1 to 3 percent of silicone-acrylic emulsion, 0.5 to 2 percent of bis (dioctyl oxy pyrophosphato) ethylene titanate chelate, 1 to 3 percent of thixotropic agent, 1 to 2 percent of filling material, 60 to 75 percent of yttrium-stabilized zirconium dioxide powder and 12 to 18 percent of deionized water.
In a preferred example, the thixotropic agent is a combination of fumed silica and hydroxypropyl methylcellulose.
In a preferred example, the fumed silica is AEROSIL R972 desilication hydrophobic fumed silica.
In a preferred example, the filler material is one or a combination of two of carbon fiber powder and multi-walled carbon nanotubes.
In a preferred example, the multi-walled carbon nanotubes have a tube diameter of 8 to 10nm, a tube length of 30 to 50um, and/or; the particle size of the carbon fiber powder is 150-200 meshes.
In a preferred example, the sodium silicate solution has a modulus of 2 to 2.5, a solids content of 40%, and/or; the solid content of the silicone-acrylic emulsion is 45%, the pH value of the solution is 7-9, and/or the solid content of the silicone-acrylic emulsion is the same as that of the solution; the grain size of the yttrium-stabilized zirconium dioxide powder is 200-250 meshes.
According to another aspect of the present application, the present application further provides a method for preparing the zirconia powder molding material, wherein the raw materials are cheap and easy to obtain, the preparation process is simple, and the adopted technical scheme is as follows:
based on the preparation method of the zirconium dioxide powder molding material for additive manufacturing, the preparation method comprises the following steps: adding a proper amount of thixotropic agent into the preheated sodium silicate solution, and stirring and mixing to obtain a material A; respectively adding bis (dioctyl-oxy-pyrophosphato) ethylene titanate chelate, a filling material and a silicone-acrylic emulsion into deionized water according to a mass ratio, mixing, performing ultrasonic dispersion, and adding yttrium stabilized zirconium dioxide powder with a proper ratio, and uniformly mixing to obtain a material B; mixing the material A and the material B, and obtaining the molding material after vacuum defoaming.
In a preferred example, the thixotropic agent has a pre-heat temperature of 85 ℃ or higher, and/or; and adopting a ball mill or a dispersing machine to carry out dispersion mixing between the components and the materials.
According to still another aspect of the present application, the present application further provides a construction process of the zirconia powder molding material, which is applied to manufacturing of a ceramic filter element, and the ceramic filter element is manufactured with high molding precision, good product uniformity and rapid molding, and the adopted technical scheme is as follows:
the construction process comprises the following steps:
extrusion molding: injecting a molding material into a charging barrel of additive manufacturing equipment for defoaming treatment, and extruding the material layer by a needle under the control of a computer to obtain a filter element green body;
and (3) sectional sintering: and heating and sintering the dried filter element green embryo in a sectioning way.
In a preferred example, in the extrusion molding step, the obtained green filter element is left to stand for 60-90 min in a temperature environment of not lower than 15 ℃ to finish surface curing, and/or; before the step of sectional sintering, the filter element green body is placed at a ventilated drying position for at least 12 hours, and/or; in the step of sectional sintering, firstly, heating to 700-800 ℃ at the speed of 30-45 ℃/min, and preserving heat for 30-35 minutes; then heating to 1100-1300 ℃ at a speed of 25-30 ℃/min, and preserving heat for 35-45 min; finally, the temperature is raised to 1400-1500 ℃ at the speed of 10-15 ℃/min, the temperature is kept for 90-140 minutes, and the furnace is cooled to the room temperature.
The technical scheme adopted by the application has at least the following beneficial effects:
1. the thixotropic agent is added to ensure that the molding material has better thixotropic property in the stirring, conveying and extruding processes, and is not easy to generate obvious deformation under the condition of bearing the subsequent multilayer covering load;
2. by adding the filling material, the molding material has excellent rheological property, and stress concentration points are not easy to generate in the extrusion molding process, so that cracks can not occur due to bursting;
3. the ceramic filter element is manufactured by adding materials to the molding materials with thixotropic properties and rheological properties, and the ceramic filter element has high product precision, good uniformity and good mechanical strength; in addition, the production cycle can be shortened by adopting the additive manufacturing technology, and the workload can be reduced;
4. after the ceramic filter element is extruded by additive manufacturing equipment, stable production with the minimum layer thickness of 0.01mm can be realized, the maximum stacking thickness of single ceramic filter element is 150mm, the ceramic density is not lower than 98%, and the ceramic filter element is suitable for customized production of ceramic filter elements with complex and fine structures.
Detailed Description
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims. The various reagents commonly used in the examples are all commercially available products.
The application provides a zirconium dioxide powder forming material for additive manufacturing, which comprises the following components in percentage by mass: 8 to 15 percent of sodium silicate solution, 1 to 3 percent of silicone-acrylic emulsion, 0.5 to 2 percent of bis (dioctyl oxy pyrophosphato) ethylene titanate chelate, 1 to 3 percent of thixotropic agent, 1 to 2 percent of filling material, 60 to 75 percent of yttrium-stabilized zirconium dioxide powder and 12 to 18 percent of deionized water. Wherein, the modulus of the sodium silicate solution is 2-2.5, and the solid content is 40%; the solid content of the silicone-acrylic emulsion is 45%, and the pH value of the solution is 7-9; the grain size of the yttrium stable zirconium dioxide powder is 200-250 meshes.
The molding material in the embodiment is thixotropic paste, and has good fluidity when sheared, and rapidly turns into colloid when the shearing is stopped and the consistency is increased, so that the thixotropic property in the processes of stirring, conveying and extruding the material can be provided, and the processing and shape-retaining capability is good.
In a preferred embodiment, the thixotropic agent is a combination of AEROSIL R972 desilication hydrophobic fumed silica and hydroxypropyl methylcellulose; the ceramic loss on ignition can be reduced by adopting the combined thixotropic agent.
In another preferred embodiment, the filler material is one or both of carbon fiber powder and multi-walled carbon nanotubes. Specifically, the pipe diameter of the multi-wall carbon nano-tube is 8-10 nm, and the pipe length is 30-50 um; the particle size of the carbon fiber powder is 150-200 meshes. In the embodiment, the conventional filling material addition of more than 1% can cause cracks to be generated due to uneven stress in the extrusion process of the molding material to influence the quality of a finished product, but the filling material in the scheme can be uniformly dispersed into the molding material at the addition ratio of 1% -2%, so that stress concentration points can not be generated, bursting can not be generated to influence the quality of the product, and the obtained finished product has excellent mechanical strength.
In a specific application example, the preparation method of the zirconium dioxide powder molding material for additive manufacturing comprises the following steps:
firstly, heating 10% sodium silicate solution to more than 85 ℃, stirring and adding 3% thixotropic agent, wherein the mass fraction of fumed silica (AEROSIL R972 Desoxacel) is 1.5% and the mass fraction of hydroxypropyl methylcellulose is 1.5%, and stirring for 5-10 minutes to form a material A for later use;
adding 1% of bis (dioctyl oxygen pyrophosphate) ethylene titanate chelate, 2% of carbon fiber powder and 2% of silicone-acrylic emulsion into 15% of deionized water, uniformly stirring, performing ultrasonic dispersion for 20-30 minutes to obtain uniform suspension, mixing with 67% of yttrium stabilized zirconium dioxide powder, and performing ball milling for 30-40 minutes to uniformly disperse to obtain a material B for later use;
and adding the material A and the material B into a dispersing machine, uniformly dispersing for 20-30 minutes, and performing vacuum defoaming to obtain the molding material.
The construction process of the zirconium dioxide powder molding material for additive manufacturing comprises the following steps:
extrusion molding: injecting the molding material into a charging barrel of additive manufacturing equipment for defoaming treatment, extruding the material layer by a needle under the control of a computer, stacking and molding to obtain a filter element green body, and completing surface solidification in an environment of more than or equal to 15 ℃ for 60-90 minutes; the green body should be placed in a through-air-dried place for at least 12 hours prior to sintering.
And (3) sectional sintering: after the green embryo is dried, sectional heating and sintering are adopted, firstly, the temperature is raised to 700-800 ℃ at the speed of 30-45 ℃/min, the temperature is kept for 30-35 min, then the temperature is raised to 1100-1300 ℃ at the speed of 25-30 ℃ and kept for 35-45 min, finally, the temperature is raised to 1400-1500 ℃ at the speed of 10-15 ℃/min, the temperature is kept for 90-140 min, and the furnace is cooled to the room temperature.
The zirconia molding material for additive manufacturing provided by the preparation method is used for manufacturing a ceramic filter element with the diameter of 100mm and the thickness of 20mm for detection according to the construction process, and the result is as follows:
the ceramic surface of the ceramic filter element is smooth and clean, and no obvious internal crack defect is found when the ceramic filter element is scanned by industrial CT; density 1.67g/cm was determined by Archimedes drainage 3 The method comprises the steps of carrying out a first treatment on the surface of the The bending strength tester measures the bending strength at room temperature to be 2.2MPa by a three-point bending method; the normal temperature compression strength is 3MPa; the high temperature resistance is not lower than 1700 ℃.
In still another specific application example, the preparation method of the zirconium dioxide powder molding material for additive manufacturing is as follows:
firstly, heating 8% sodium silicate solution to above 85 ℃, stirring and adding thixotropic agent with a proportion of 2%, wherein the mass fraction of fumed silica (AEROSIL R972 Desoxacel) is 1%, the mass fraction of hydroxypropyl methylcellulose is 1%, and stirring for 5-10 minutes to form a material A for later use;
adding 1.5% of bis (dioctyl oxygen pyrophosphate) ethylene titanate chelate, 1% of multi-wall carbon nano-tube and 2.5% of silicone-acrylic emulsion into 15% of deionized water, uniformly stirring, performing ultrasonic dispersion for 20-30 minutes to obtain uniform suspension, mixing with 70% of yttrium stabilized zirconium dioxide powder, and performing ball milling for 30-40 minutes to uniformly disperse to obtain a material B for later use;
and adding the material A and the material B into a dispersing machine, uniformly dispersing for 20-30 minutes, and performing vacuum defoaming to obtain the molding material.
The zirconia molding material for additive manufacturing, which is provided by the preparation method, is used for manufacturing a ceramic filter element with the diameter of 100mm and the thickness of 20mm for detection according to the construction process, and the result is as follows:
the ceramic surface of the ceramic filter element is smooth and clean, and no obvious internal crack defect is found when the ceramic filter element is scanned by industrial CT; density 1.65g/cm was determined by Archimedes drainage 3 The method comprises the steps of carrying out a first treatment on the surface of the Flexural Strength tester with three-point bending methodThe bending strength at room temperature is 2.4MPa; the normal temperature compression strength is 2.9MPa; the high temperature resistance is not lower than 1700 ℃.
In order to fully recognize and popularize and apply the technical improvements of the present application, the following comparative examples are provided for illustration.
In a comparative example, the zirconia powder molding material for additive manufacturing was prepared by:
firstly, heating 10% sodium silicate solution to above 85 ℃, stirring and adding thixotropic agent fumed silica (AEROSIL R972 Desolid) 3%, and keeping stirring for 5-10 minutes to form a material A for later use;
adding 1% of bis (dioctyl oxygen pyrophosphate) ethylene titanate chelate, 2% of carbon fiber powder and 2% of silicone-acrylic emulsion into 15% of deionized water, uniformly stirring, performing ultrasonic dispersion for 20-30 minutes to obtain uniform suspension, mixing with 67% of yttrium stabilized zirconium dioxide powder, and performing ball milling for 30-40 minutes to uniformly disperse to obtain a material B for later use;
and adding the material A and the material B into a dispersing machine, uniformly dispersing for 20-30 minutes, and performing vacuum defoaming to obtain the molding material.
In this comparative example, after the combination thixotropic agent in the foregoing example is adjusted to be the fumed silica thixotropic agent used alone, practice proves that when the molding material obtained by the preparation method is used in the additive manufacturing process, the fluidity of the finished material is large during the extrusion process of the needle, and precise shaping is difficult.
In another comparative example, the preparation method of the zirconium dioxide powder molding material for additive manufacturing was:
firstly, heating 8% sodium silicate solution to above 85 ℃, stirring and adding thixotropic agent 2%, wherein fumed silica (AEROSIL R972 Desoxase) 1% and hydroxypropyl methylcellulose 1%, and stirring for 5-10 minutes to form a material A for later use;
adding 1.5% of bis (dioctyl oxygen pyrophosphate) ethylene titanate chelate, 3% of multi-wall carbon nano-tube and 2.5% of silicone-acrylic emulsion into 15% of deionized water, uniformly stirring, performing ultrasonic dispersion for 20-30 minutes to obtain uniform suspension, mixing with 69% of yttrium stabilized zirconium dioxide powder, and performing ball milling for 30-40 minutes to uniformly disperse to obtain a material B for later use;
and adding the material A and the material B into a dispersing machine, uniformly dispersing for 20-30 minutes, and performing vacuum defoaming to obtain the molding material.
Compared with the previous embodiment, the mass content of the multi-wall carbon nano-tube is improved from 1% to 3%, and the practice proves that cracks appear on the surface of the sintered ceramic filter element, and the industrial CT scanning of the ceramic filter element is adopted, so that more cracks exist in the ceramic filter element.
The foregoing examples illustrate only a few embodiments of the application and are described in detail herein without thereby limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. Accordingly, the scope of the application should be assessed as that of the appended claims.
Claims (9)
1. The zirconium dioxide powder forming material for additive manufacturing is characterized by being applied to ceramic filter element manufacturing and comprising the following components in percentage by mass:
8-15% of sodium silicate solution, 1-3% of silicone-acrylic emulsion, 0.5-2% of bis (dioctyl-oxy-pyrophosphoric acid ester) ethylene titanate chelate, 1-3% of thixotropic agent, 1-2% of filling material, 60-75% of yttrium-stabilized zirconium dioxide powder and 12-18% of deionized water;
the thixotropic agent is a combination of fumed silica and hydroxypropyl methylcellulose.
2. The zirconia powder forming material for additive manufacturing of claim 1, wherein the fumed silica is AEROSIL R972 desilication hydrophobic fumed silica.
3. The zirconia powder forming material for additive manufacturing according to claim 1, wherein the filler material is one or a combination of two of carbon fiber powder and multi-walled carbon nanotubes.
4. The zirconia powder molding material for additive manufacturing according to claim 3, wherein the multi-wall carbon nanotubes have a tube diameter of 8-10 nm and a tube length of 30-50 μm,
and/or;
the particle size of the carbon fiber powder is 150-200 meshes.
5. The zirconia powder molding material for additive manufacturing according to claim 1, wherein the sodium silicate solution has a modulus of 2 to 2.5 and a solid content of 40%,
and/or;
the solid content of the silicone-acrylic emulsion is 45%, the pH value of the solution is 7-9,
and/or;
the particle size of the yttrium-stabilized zirconium dioxide powder is 200-250 meshes.
6. A method for preparing a zirconia powder molding material for additive manufacturing according to any one of claims 1 to 5, comprising:
adding a proper amount of thixotropic agent into the preheated sodium silicate solution, and stirring and mixing to obtain a material A;
respectively adding bis (dioctyl-oxy-pyrophosphato) ethylene titanate chelate, a filling material and a silicone-acrylic emulsion into deionized water according to a mass ratio, mixing, performing ultrasonic dispersion, and adding yttrium stabilized zirconium dioxide powder with a proper ratio, and uniformly mixing to obtain a material B;
mixing the material A and the material B, and obtaining the molding material after vacuum defoaming.
7. The method according to claim 6, wherein,
the preheating temperature of the sodium silicate solution is more than 85 ℃,
and/or;
and adopting a ball mill or a dispersing machine to carry out dispersion mixing between the components and the materials.
8. A construction process based on a zirconia powder forming material for additive manufacturing according to any one of claims 1 to 5, characterized by being applied to ceramic filter element manufacturing, comprising:
extrusion molding: injecting a molding material into a charging barrel of additive manufacturing equipment for defoaming treatment, and extruding the material layer by a needle under the control of a computer to obtain a filter element green body;
and (3) sectional sintering: and heating and sintering the dried filter element green embryo in a sectioning way.
9. The construction process according to claim 8, wherein,
in the extrusion molding step, the obtained filter element green embryo stands for 60-90 min in the temperature environment of not lower than 15 ℃ to finish surface solidification,
and/or;
before the step of sectional sintering, the filter element green body is placed in a ventilated drying place for at least 12 hours,
and/or;
in the step of sectional sintering, firstly, heating to 700-800 ℃ at a speed of 30-45 ℃/min, and preserving heat for 30-35 minutes; then heating to 1100-1300 ℃ at a speed of 25-30 ℃/min, and preserving heat for 35-45 min; and finally, heating to 1400-1500 ℃ at a speed of 10-15 ℃/min, preserving heat for 90-140 minutes, and cooling to room temperature in a furnace.
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