CN112374903A - Preparation method for zirconia ceramic 3D printing material - Google Patents
Preparation method for zirconia ceramic 3D printing material Download PDFInfo
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- CN112374903A CN112374903A CN202011513867.9A CN202011513867A CN112374903A CN 112374903 A CN112374903 A CN 112374903A CN 202011513867 A CN202011513867 A CN 202011513867A CN 112374903 A CN112374903 A CN 112374903A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6026—Computer aided shaping, e.g. rapid prototyping
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Abstract
The invention provides a preparation method for a zirconia ceramic 3D printing material, which comprises the steps of preparing an ammonium zirconium carbonate solution, preparing zirconia superfine powder, adding a cross-linking body, a dispersing agent and deionized water into the zirconia superfine powder, mixing and ball-milling to obtain slurry, adding carbon fibers and an adhesive into the slurry to obtain the zirconia ceramic 3D printing material, and the invention obtains the zirconia ceramic 3D printing material by the operation of the steps of preparing the ammonium zirconium carbonate solution, preparing the zirconia superfine powder and the like, finally obtaining the zirconia superfine powder, adding the cross-linking body, the dispersing agent and the deionized water, mixing and ball-milling to obtain the slurry, adding the carbon fibers and the adhesive into the slurry to obtain the zirconia ceramic 3D printing material, can be applied to 3D printing, has less cracks on the surface of the printed zirconia ceramic, and has high strength of the printed product due to the addition of the carbon fibers and the adhesive into the material, meanwhile, the preparation method has the advantages of easily available raw materials, simple operation and low production cost.
Description
Technical Field
The invention relates to the technical field of 3D printing, in particular to a preparation method for a zirconia ceramic 3D printing material.
Background
The zirconia ceramic is a ceramic with stable cubic zirconia as a main crystal phase, has excellent mechanical and thermal properties and the like, is a novel structural ceramic material with a good development prospect, and has been widely applied in various fields. Zirconia toughened ceramics have been widely used due to their excellent properties, and their application fields are continuously expanding.
The existing zirconia ceramic molding is to fully mix zirconia ceramic powder with a large amount of organic binder, plasticizer, dispersant and the like to obtain flowable viscous slurry, add the slurry into a hopper of a casting machine, control the thickness by a scraper, flow out to a conveyor belt through a feed nozzle, and obtain a film blank after drying. The process is suitable for preparing film materials, a large amount of organic matters are added for obtaining better flexibility, the process parameters are required to be strictly controlled, otherwise, the defects of peeling, stripes, low film strength, difficult peeling and the like are easily caused. The production of the zirconia ceramics requires the preparation of powder with high purity, good dispersion performance, superfine particles and narrow particle size distribution, and the characteristic can be well applied to the 3D printing technology, so that the zirconia ceramics can be molded and manufactured by the 3D printing technology to obtain a molding structure meeting the requirements.
Disclosure of Invention
The invention aims to provide a preparation method for a zirconia ceramic 3D printing material.
A preparation method for a zirconia ceramic 3D printing material comprises the following steps:
s1, preparing ammonium zirconium carbonate solution
Preparing a zirconium oxychloride solution with the molar concentration of 6.0-7.5mol/L, preparing an ammonium carbonate aqueous solution with the molar concentration of 5.5-6.5mol/L, mixing the two solutions, and uniformly stirring to prepare an ammonium zirconium carbonate solution;
s2, preparing the zirconia superfine powder
Adding 35% alkaline aqueous solution by mass into the prepared ammonium zirconium carbonate solution until the pH value of the solution is 9.5 to obtain white precipitate, filtering and washing;
adding anhydrous ethanol into the white precipitate, stirring to uniform state, filtering, soaking in anhydrous ethanol, and stirring to obtain emulsion;
placing into a pressure reaction kettle, heating to 160 deg.C, controlling pressure at 2.0MPa, maintaining for a certain time, and evacuating ethanol vapor when pressure is reduced to below 0.4MPa to obtain white powder; calcining the white powder at 1200 ℃ to obtain zirconium oxide superfine powder;
and S3, adding the cross-linked body, the dispersing agent and the deionized water into the zirconia ultrafine powder, mixing and ball-milling to obtain slurry, and adding the carbon fiber and the adhesive into the slurry to obtain the zirconia ceramic 3D printing material.
Further, the mass ratio of the absolute ethyl alcohol to the white precipitate is 3-10.
Further, the weight ratio of the zirconium oxide superfine powder, the cross-linked body, the dispersing agent and the deionized water is 100: 6: 5: 8.
further, in S3, the dispersant is organic base tetramethylammonium hydroxide.
Further, the cross-linked body is poly-triallyl isocyanurate.
Further, in S3, the content of the carbon fibers in the slurry is 25% by volume.
Further, the mass ratio of the binder to the carbon fibers is 4: 1 to 3.
Further, the binder is an epoxy resin.
Further, the alkaline aqueous solution is an aqueous sodium hydroxide solution or an aqueous potassium hydroxide solution.
Advantageous effects
The invention relates to a preparation method for a zirconia ceramic 3D printing material, which comprises the steps of preparing an ammonium zirconium carbonate solution, preparing zirconia superfine powder and the like, finally obtaining the zirconia superfine powder, adding a cross-linking body, a dispersing agent and deionized water, mixing and ball-milling to obtain slurry, adding carbon fibers and an adhesive into the slurry to obtain the zirconia ceramic 3D printing material.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms also include the plural forms unless the context clearly dictates otherwise, and further, it is understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, devices, components, and/or combinations thereof.
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method for a zirconia ceramic 3D printing material comprises the following steps:
s1, preparing ammonium zirconium carbonate solution
Preparing a zirconium oxychloride solution with the molar concentration of 6.0-7.5mol/L, preparing an ammonium carbonate aqueous solution with the molar concentration of 5.5-6.5mol/L, mixing the two solutions, and uniformly stirring to prepare an ammonium zirconium carbonate solution;
s2, preparing the zirconia superfine powder
Adding 35% sodium hydroxide aqueous solution by mass fraction into the prepared ammonium zirconium carbonate solution until the pH value of the solution is 9.5 to obtain white precipitate, filtering and washing;
adding absolute ethyl alcohol into the white precipitate, wherein the mass ratio of the absolute ethyl alcohol to the white precipitate is 3-10, stirring to a uniform state, filtering, soaking with the absolute ethyl alcohol, and stirring to obtain an emulsion;
placing into a pressure reaction kettle, heating to 160 deg.C, controlling pressure at 2.0MPa, maintaining for a certain time, and evacuating ethanol vapor when pressure is reduced to below 0.4MPa to obtain white powder; calcining the white powder at 1200 ℃ to obtain zirconium oxide superfine powder;
s3, adding poly (triallyl isocyanurate), organic alkali tetramethyl ammonium hydroxide and deionized water into the zirconia ultrafine powder, wherein the weight ratio of the zirconia ultrafine powder to the poly (triallyl isocyanurate) to the organic alkali tetramethyl ammonium hydroxide to the deionized water is 100: 6: 5: and 8, mixing and ball-milling to obtain slurry, adding carbon fiber and epoxy resin into the slurry, wherein the volume content of the carbon fiber in the slurry is 25%, and the mass ratio of the epoxy resin to the carbon fiber is 4: and 1, obtaining the zirconia ceramic 3D printing material.
Example 2
A preparation method for a zirconia ceramic 3D printing material comprises the following steps:
s1, preparing ammonium zirconium carbonate solution
Preparing a zirconium oxychloride solution with the molar concentration of 6.0-7.5mol/L, preparing an ammonium carbonate aqueous solution with the molar concentration of 5.5-6.5mol/L, mixing the two solutions, and uniformly stirring to prepare an ammonium zirconium carbonate solution;
s2, preparing the zirconia superfine powder
Adding 35% sodium hydroxide aqueous solution by mass fraction into the prepared ammonium zirconium carbonate solution until the pH value of the solution is 9.5 to obtain white precipitate, filtering and washing;
adding absolute ethyl alcohol into the white precipitate, wherein the mass ratio of the absolute ethyl alcohol to the white precipitate is 3-10, stirring to a uniform state, filtering, soaking with the absolute ethyl alcohol, and stirring to obtain an emulsion;
placing into a pressure reaction kettle, heating to 160 deg.C, controlling pressure at 2.0MPa, maintaining for a certain time, and evacuating ethanol vapor when pressure is reduced to below 0.4MPa to obtain white powder; calcining the white powder at 1200 ℃ to obtain zirconium oxide superfine powder;
s3, adding poly (triallyl isocyanurate), organic alkali tetramethyl ammonium hydroxide and deionized water into the zirconia ultrafine powder, wherein the weight ratio of the zirconia ultrafine powder to the poly (triallyl isocyanurate) to the organic alkali tetramethyl ammonium hydroxide to the deionized water is 100: 6: 5: and 8, mixing and ball-milling to obtain slurry, adding carbon fiber and epoxy resin into the slurry, wherein the volume content of the carbon fiber in the slurry is 25%, and the mass ratio of the epoxy resin to the carbon fiber is 4: and 2, obtaining the zirconia ceramic 3D printing material.
Example 3
A preparation method for a zirconia ceramic 3D printing material comprises the following steps:
s1, preparing ammonium zirconium carbonate solution
Preparing a zirconium oxychloride solution with the molar concentration of 6.0-7.5mol/L, preparing an ammonium carbonate aqueous solution with the molar concentration of 5.5-6.5mol/L, mixing the two solutions, and uniformly stirring to prepare an ammonium zirconium carbonate solution;
s2, preparing the zirconia superfine powder
Adding 35% by mass of potassium hydroxide aqueous solution into the prepared ammonium zirconium carbonate solution until the pH value of the solution is 9.5 to obtain white precipitate, filtering and washing;
adding absolute ethyl alcohol into the white precipitate, wherein the mass ratio of the absolute ethyl alcohol to the white precipitate is 3-10, stirring to a uniform state, filtering, soaking with the absolute ethyl alcohol, and stirring to obtain an emulsion;
placing into a pressure reaction kettle, heating to 160 deg.C, controlling pressure at 2.0MPa, maintaining for a certain time, and evacuating ethanol vapor when pressure is reduced to below 0.4MPa to obtain white powder; calcining the white powder at 1200 ℃ to obtain zirconium oxide superfine powder;
s3, adding poly (triallyl isocyanurate), organic alkali tetramethyl ammonium hydroxide and deionized water into the zirconia ultrafine powder, wherein the weight ratio of the zirconia ultrafine powder to the poly (triallyl isocyanurate) to the organic alkali tetramethyl ammonium hydroxide to the deionized water is 100: 6: 5: and 8, mixing and ball-milling to obtain slurry, adding carbon fiber and epoxy resin into the slurry, wherein the volume content of the carbon fiber in the slurry is 25%, and the mass ratio of the epoxy resin to the carbon fiber is 4: and 3, obtaining the zirconia ceramic 3D printing material.
According to the method, the zirconium oxide superfine powder is finally obtained through the operations of preparing the ammonium zirconium carbonate solution, preparing the zirconium oxide superfine powder and other steps, the cross-linked body, the dispersing agent and the deionized water are added, the mixture is subjected to ball milling to obtain the slurry, and the carbon fibers and the adhesive are added into the slurry to obtain the 3D printing material of the zirconium oxide ceramic.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. A preparation method for a zirconia ceramic 3D printing material is characterized by comprising the following steps:
s1, preparing ammonium zirconium carbonate solution
Preparing a zirconium oxychloride solution with the molar concentration of 6.0-7.5mol/L, preparing an ammonium carbonate aqueous solution with the molar concentration of 5.5-6.5mol/L, mixing the two solutions, and uniformly stirring to prepare an ammonium zirconium carbonate solution;
s2, preparing the zirconia superfine powder
Adding 35% alkaline aqueous solution by mass into the prepared ammonium zirconium carbonate solution until the pH value of the solution is 9.5 to obtain white precipitate, filtering and washing;
adding anhydrous ethanol into the white precipitate, stirring to uniform state, filtering, soaking in anhydrous ethanol, and stirring to obtain emulsion;
placing into a pressure reaction kettle, heating to 160 deg.C, controlling pressure at 2.0MPa, maintaining for a certain time, and evacuating ethanol vapor when pressure is reduced to below 0.4MPa to obtain white powder; calcining the white powder at 1200 ℃ to obtain zirconium oxide superfine powder;
and S3, adding the cross-linked body, the dispersing agent and the deionized water into the zirconia ultrafine powder, mixing and ball-milling to obtain slurry, and adding the carbon fiber and the adhesive into the slurry to obtain the zirconia ceramic 3D printing material.
2. The preparation method of the zirconia ceramic 3D printing material according to claim 1, wherein the mass ratio of the absolute ethyl alcohol to the white precipitate is 3-10.
3. The preparation method of the zirconia ceramic 3D printing material according to claim 1, wherein the weight ratio of the zirconia ultrafine powder, the cross-linked body, the dispersing agent and the deionized water is 100: 6: 5: 8.
4. the method of claim 1, wherein in S3, the dispersant is tetramethylammonium hydroxide, an organic base.
5. The method for preparing a zirconia ceramic 3D printing material according to claim 1, wherein the cross-linked body is poly-triallyl isocyanurate.
6. The method for preparing a zirconia ceramic 3D printing material according to claim 1, wherein the volume content of the carbon fiber in the slurry in S3 is 25%.
7. The preparation method of the zirconia ceramic 3D printing material according to claim 1, wherein the mass ratio of the binder to the carbon fiber is 4: 1 to 3.
8. The method for preparing a zirconia ceramic 3D printing material according to claim 1, wherein the binder is an epoxy resin.
9. The method for preparing a zirconia ceramic 3D printing material according to claim 1, wherein the alkaline aqueous solution is an aqueous sodium hydroxide solution or an aqueous potassium hydroxide solution.
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| CN202011513867.9A CN112374903A (en) | 2020-12-21 | 2020-12-21 | Preparation method for zirconia ceramic 3D printing material |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1559982A (en) * | 2004-02-17 | 2005-01-05 | 哈尔滨工程大学 | Preparation process for superfine powder of zirconium oxide |
| CN104193345A (en) * | 2014-08-20 | 2014-12-10 | 中南大学 | Method for preparing wave-absorbing ceramic component on basis of 3D printing technique |
| CN105198414A (en) * | 2015-09-16 | 2015-12-30 | 东莞深圳清华大学研究院创新中心 | Ceramic material for 3D printing and preparation method thereof |
| CN107553686A (en) * | 2017-08-11 | 2018-01-09 | 武汉理工大学 | A kind of manufacture method of the fiber reinforcement gradient porous ceramics based on 3D printing |
| CN108033802A (en) * | 2017-12-15 | 2018-05-15 | 天津大学 | Fiber reinforced ceramic profiled piece forming method based on gel injection-moulding 3D printing |
| CN108069706A (en) * | 2017-12-15 | 2018-05-25 | 天津大学 | A kind of forming method of the fiber reinforced ceramic thin-wall part based on 3D printing technique |
| CN110372374A (en) * | 2019-07-05 | 2019-10-25 | 北京航空航天大学 | A kind of ceramic member and its structure design and 3D printing method |
| CN111377738A (en) * | 2020-02-11 | 2020-07-07 | 甘肃机电职业技术学院（甘肃省机械工业学校、甘肃省机械高级技工学校） | Preparation method of ceramic material for 3d printing |
-
2020
- 2020-12-21 CN CN202011513867.9A patent/CN112374903A/en not_active Withdrawn
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1559982A (en) * | 2004-02-17 | 2005-01-05 | 哈尔滨工程大学 | Preparation process for superfine powder of zirconium oxide |
| CN104193345A (en) * | 2014-08-20 | 2014-12-10 | 中南大学 | Method for preparing wave-absorbing ceramic component on basis of 3D printing technique |
| CN105198414A (en) * | 2015-09-16 | 2015-12-30 | 东莞深圳清华大学研究院创新中心 | Ceramic material for 3D printing and preparation method thereof |
| CN107553686A (en) * | 2017-08-11 | 2018-01-09 | 武汉理工大学 | A kind of manufacture method of the fiber reinforcement gradient porous ceramics based on 3D printing |
| CN108033802A (en) * | 2017-12-15 | 2018-05-15 | 天津大学 | Fiber reinforced ceramic profiled piece forming method based on gel injection-moulding 3D printing |
| CN108069706A (en) * | 2017-12-15 | 2018-05-25 | 天津大学 | A kind of forming method of the fiber reinforced ceramic thin-wall part based on 3D printing technique |
| CN110372374A (en) * | 2019-07-05 | 2019-10-25 | 北京航空航天大学 | A kind of ceramic member and its structure design and 3D printing method |
| CN111377738A (en) * | 2020-02-11 | 2020-07-07 | 甘肃机电职业技术学院（甘肃省机械工业学校、甘肃省机械高级技工学校） | Preparation method of ceramic material for 3d printing |
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Application publication date: 20210219 |