CN113603467B - Photocuring ceramic slurry for 3D printing and pretreatment method of formed blank - Google Patents
Photocuring ceramic slurry for 3D printing and pretreatment method of formed blank Download PDFInfo
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- CN113603467B CN113603467B CN202110910670.7A CN202110910670A CN113603467B CN 113603467 B CN113603467 B CN 113603467B CN 202110910670 A CN202110910670 A CN 202110910670A CN 113603467 B CN113603467 B CN 113603467B
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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
- C04B35/10—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 aluminium oxide
- C04B35/111—Fine ceramics
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
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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
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
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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
- C04B35/486—Fine ceramics
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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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
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Abstract
The invention discloses a photocuring ceramic slurry for 3D printing, which comprises the following components in parts by weight: 50-85 parts of ceramic powder, 9-40 parts of photosensitive organic matter, 3-30 parts of plasticizer, 1-10 parts of liquid paraffin, 0.075-2 parts of photoinitiator and 0.5-3 parts of dispersant. The photocuring ceramic slurry is prepared by optimizing the formula type and the dosage, so that the stability of 3D printing is improved, and the efficiency of the subsequent degreasing process is improved; in addition, the application also provides a pretreatment method for the formed blank prepared from the ceramic slurry, the prepared photocuring ceramic slurry is printed and formed in a 3D printer, the formed blank is soaked in kerosene, and the soaked blank is placed in a drying box for drying.
Description
Technical Field
The invention relates to the technical field of 3D printing materials and methods, in particular to a photocuring ceramic slurry for 3D printing and a pretreatment method of a formed blank.
Background
The ceramic photocuring forming is a novel forming method which does not depend on a mould and can quickly and efficiently prepare a ceramic device with a fine structure. The forming process of the method is mainly based on photoinitiation for preparation, namely ultraviolet laser irradiates the surface of ceramic slurry with photosensitive characteristic to excite free radical polymerization reaction, so that a solidified layer is formed in a laser scanning area; then the solidified layer descends by a platform height, the uncured slurry is paved above the solidified layer again, laser irradiation and curing are carried out again, then the platform descends again, the paving material … … finally forms a ceramic green body with a certain shape and structure in a layer curing and combining mode, and then the green body is subjected to thermal degreasing, sintering and post-processing to form finished ceramic.
The ceramic green body is obtained by 3D printing of ceramic slurry, and because the ceramic slurry contains more than 20% of organic matters, thermal removal is carried out in a subsequent degreasing link. If the organic content is too high, a polymer network structure is formed by crosslinking in the photocuring process, and stress is generated due to curing shrinkage in the photocuring molding process, which increases the difficulty of degreasing. In order to avoid undesirable phenomena such as cracking, deformation and the like, a common means is to add a plasticizer into the components of the slurry to improve interlayer bonding stress in a printing blank; secondly, the temperature rise of the degreasing is reduced in the degreasing process, even to 10 ℃/h, so that the whole degreasing time can be as long as about 6 days.
Therefore, it is an urgent problem to be solved by those skilled in the art to reduce the viscosity of the slurry as much as possible, reduce the internal stress of the green body, and improve the reliability of the degreasing process.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the photocuring ceramic slurry for 3D printing, the formula type and the dosage of the slurry are optimally proportioned, the stability of 3D printing is favorably improved, and the efficiency of the subsequent degreasing process is improved; in addition, the application also provides a pretreatment method for the formed blank prepared from the ceramic slurry, and the risk of shrinkage cracking and deformation caused by direct thermal degreasing can be reduced by the pretreatment method of kerosene soaking.
In order to achieve the purpose, the invention provides the following technical scheme:
the photocuring ceramic slurry for 3D printing comprises the following components in parts by weight: 50-85 parts of ceramic powder, 9-40 parts of photosensitive organic matter, 3-30 parts of plasticizer, 1-10 parts of liquid paraffin, 0.075-2 parts of photoinitiator and 0.5-3 parts of dispersant.
Further, the ceramic powder is at least one of alumina or zirconia.
The photosensitive organic matter is a combination of at least two or more of epoxy acrylate oligomer, polyester acrylate oligomer, urethane acrylate oligomer, aliphatic urethane acrylate oligomer, (2) ethoxylated bisphenol a diacrylate, (4) ethoxylated bisphenol a diacrylate, 1,6-ethylene glycol diacrylate, (2) propoxylated neopentyl glycol diacrylate, trimethylolpropane acrylate, (3) ethoxylated trimethylolpropane acrylate, (6) ethoxylated trimethylolpropane acrylate, di-trimethylolpropane tetraacrylate, pentaerythritol tetraacrylate, or (4) ethoxylated pentaerythritol tetraacrylate.
Further, the plasticizer is at least one of polyethylene glycol 200, polyethylene glycol 400, linseed oil, oleic acid, tributyl citrate, acetyl tributyl citrate, trioctyl citrate, glycerin, phenyl alkylsulfonate, dioctyl phthalate, dibutyl phthalate, acetyl trioctyl citrate, cyclohexane 1,2-diisononyl phthalate, or epoxidized soybean oil.
Further, the photoinitiator is one or the combination of more than one of 2-dimethylamino-2-benzyl-1- (4-piperidinophenyl) -1-butanone, 1-hydroxycyclohexyl phenyl ketone, 4,4-bis (diethoxy) benzophenone, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide, 2-methyl-2 (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-propanone and 2-isopropyl thioxanthone.
Further, the dispersing agent is at least one of a copolymer with an acid group, a modified polyether with high pigment affinity performance or a polyether polyol modified polyurethane polymer.
The types of these dispersants include, but are not limited to, BYK111, BYK102, BYK180, BYK2205, solsperse 85000, solsperse 32000, solsperse 39000, solsperse 75000, dispers _689, dispers _655, dispers _628, EFKA 4701, EFKA 4732, R1100.
The dispersant, the plasticizer and the photosensitive organic matter jointly form organic resin in the slurry, the plasticizer can improve interlayer bonding stress in the printing blank, and the dispersant can uniformly mix the components of the slurry; in addition, the liquid paraffin added into the system can reduce the viscosity.
Further, the photocuring ceramic slurry comprises the following components in parts by weight: 60 parts of ceramic powder, 20 parts of photosensitive organic matter, 15 parts of plasticizer, 5 parts of liquid paraffin, 1 part of photoinitiator and 1 part of dispersant.
The photocuring ceramic slurry is prepared by the following method: weighing photosensitive organic matters, a dispersing agent, a plasticizer, liquid paraffin and a photoinitiator according to parts by weight, adding the weighed photosensitive organic matters into a ball milling tank, and adding zirconia milling media serving as milling dispersion media into the ball milling tank, wherein the proportion of the milling dispersion media in the ball milling tank is not higher than 1/3 of the volume of the ball milling tank; then ball milling and dispersing for 0.5-4 hours at a lower rotating speed; and then, adding ceramic powder for at least two times, performing ball milling for 10-24 hours again, and discharging to obtain the photocuring ceramic slurry.
The invention also provides a pre-treatment method of the formed blank body, which comprises the steps of printing and forming the prepared photo-cured ceramic slurry in a 3D printer, soaking the formed blank body in kerosene, and drying the soaked blank body in a drying box.
Further, the kerosene is aviation kerosene; the soaking temperature is 20-40 ℃, and the soaking time is 4-48 h; the drying temperature is 20-60 ℃, and the drying time is 2-12 h.
Based on the technical scheme, the invention has the following technical effects:
(1) According to the photocuring ceramic slurry for 3D printing, provided by the invention, ceramic powder is compounded with photosensitive organic matters, a dispersing agent, a plasticizer, liquid paraffin and a photoinitiator, and the formula type and the dosage of the slurry are optimally proportioned, so that the stability of 3D printing is favorably improved, the efficiency of a subsequent degreasing process is improved, and the cracking and deformation risks in the degreasing process are reduced.
(2) According to the method for pretreating the formed blank, the liquid paraffin can be removed in advance by soaking kerosene, so that part of organic matters can be removed by solvent degreasing of the blank, an exhaust micro-channel is formed in the blank, the content of the organic matters in the blank is reduced, and the stability of a subsequent thermal degreasing process is facilitated.
(3) In addition, in the method for preprocessing the formed blank, as the solvent degreasing process is also a process for releasing the printing stress, the internal stress of the blank can be reduced through the solvent degreasing, and the success rate of the thermal degreasing is increased. The solvent degreasing process is easy to control, the cost is low, and the operability is strong.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following examples. The following examples set forth preferred embodiments of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
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 invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
59.07g of (2) propyleneoxyneopentyl glycol diacrylate, 88.64g of tricyclodecane dimethanol diacrylate, 12.44g of ditrimethylolpropane tetraacrylate, 45.34g of cyclohexane 1,2-diisononyl dicarboxylate, 53.34g of liquid paraffin, 13.33g of dispersant R1100, 0.391g2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 0.39g1-hydroxycyclohexylphenylketone were charged into a ball mill pot loaded with a zirconia milling media, and mixed uniformly by ball milling for 1 hour; 630g of alumina powder having a particle shape of spheroidal with a D50 of about 0.4 μm was added, the ball milling was continued for 16 hours, and the photocurable alumina slurry was prepared by discharging.
Printing a sample strip of the photocured alumina slurry in a cerambuilder 100 type ceramic 3D printer, wherein the design size of the sample strip is as follows: 60mm is multiplied by 5mm is multiplied by 4mm, and the printing laser parameters are as follows: the laser scanning speed is 2000mm/s, the laser filling space is 0.1mm, the laser energy is about 150mW, the single-layer curing depth of the slurry is about 200 mu m under the laser parameters, and the molded blank is obtained through 3D printing.
Example 2
Taking 20 molded blank sample strips in the embodiment 1, weighing and measuring the size of the sample strips respectively, taking 10 molded blank sample strips, placing the 10 molded blank sample strips in aviation kerosene, and soaking the sample strips for 24 hours at room temperature, wherein the sample strips can be completely immersed by the amount of the aviation kerosene; the molded green body sample after completion of the soaking was placed in a petri dish, and then dried in a drying oven, and the petri dish was covered with a lid to keep the petri dish in a half-open state in order to control the drying speed. Then dried at 50 ℃ for 4h.
The molded green body specimens were again subjected to dimensional measurement and weighing, and the average of the measured data was calculated.
In addition, 10 molded blank sample bars are directly dried for 4 hours at 50 ℃ without being soaked in kerosene.
The test data of the shaped bodies after kerosene soaking and drying are shown in table 1:
TABLE 1 test data (mean) of the shaped green bodies, specimens before and after drying by immersion
Sample(s) | Long (mm) | Width (mm) | Thickness (mm) | Weight (g) |
Before soaking | 59.14 | 4.91 | 3.68 | 2.66 |
After soaking and drying | 57.57 | 4.78 | 3.58 | 2.52 |
As can be seen from Table 1, the molded green body specimens subjected to kerosene immersion and drying treatment were able to undergo preliminary shrinkage and thermal weight loss, which reduced undesirable phenomena such as shrinkage cracking, deformation, etc. caused by direct thermal degreasing of the printed green bodies.
In order to further study the beneficial effects of solvent degreasing on the formed body, the formed body sample strips (10 strips) soaked in kerosene and dried are compared with the sample strips (10 strips) not soaked in kerosene, and the porosity of the formed body sample strips is tested by a Mac Auto Pore 9520 mercury intrusion instrument.
And performing Tg/DSC test on a METTLER synchronous thermal analyzer, wherein the set temperature interval is 25-800 ℃, and the heating rate is 10K/min, so as to examine the thermal weight loss condition of the sample strip.
Specific air holes and thermal weight loss are shown in table 2.
TABLE 2 test table for the properties of kerosene-soaked and kerosene-untreated specimens
Sample(s) | Average pore size (nm) | Porosity (%) | Thermal weight loss (%) at 25-800 DEG C |
Kerosene soaked and dried bars | 32.53 | 13.1 | 11.1 |
Sample bar without kerosene soaking treatment | 11.66 | 4.4 | 15.6 |
As can be seen from table 2, the pore size and the porosity of the sample printed from the photo-cured ceramic slurry provided in example 1 are significantly increased after kerosene soaking, and the thermal weight loss is significantly reduced. The increase of the size and the porosity of the air hole is beneficial to the removal of waste gas generated in the organic matter decomposition process in the degreasing process, and the reduction of the total thermal weight loss is beneficial to reducing the risks of adverse effects such as cracking, deformation and the like in the degreasing process, so that the stability of the degreasing process is improved.
The foregoing is merely exemplary and illustrative of the structures of the present invention, which are described in some detail and detail, and are not to be construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications are possible without departing from the inventive concept, and such obvious alternatives fall within the scope of the invention.
Claims (6)
1. A pre-treatment method of a formed blank body is characterized in that photo-cured ceramic slurry is printed and formed in a 3D printer, the formed blank body obtained by printing is soaked in kerosene, and the soaked formed blank body is placed in a drying box for drying;
the kerosene is aviation kerosene; the soaking temperature is 20-40 ℃, and the soaking time is 4-48 h; the drying temperature is 20-60 ℃, and the drying time is 2-12 h;
the light-cured ceramic slurry comprises the following components in parts by weight: 50-85 parts of ceramic powder, 9-40 parts of photosensitive organic matter, 3-30 parts of plasticizer, 1-10 parts of liquid paraffin, 0.075-2 parts of photoinitiator and 0.5-3 parts of dispersant;
the ceramic powder is at least one of alumina or zirconia;
the light-cured ceramic slurry is prepared by the following method: weighing photosensitive organic matters, a dispersing agent, a plasticizer, liquid paraffin and a photoinitiator according to parts by weight, adding the weighed photosensitive organic matters into a ball milling tank, and adding zirconia milling media serving as milling dispersion media into the ball milling tank, wherein the proportion of the milling dispersion media in the ball milling tank is not higher than 1/3 of the volume of the ball milling tank; then ball milling and dispersing for 0.5-4 hours at a lower rotating speed; and then, adding ceramic powder for at least two times, performing ball milling for 10-24 hours again, and discharging to obtain the photocuring ceramic slurry.
2. The method for pretreating a molded body according to claim 1, wherein said photosensitive organic compound is at least two or a combination of two or more of epoxy acrylate oligomer, polyester acrylate oligomer, urethane acrylate oligomer, aliphatic urethane acrylate oligomer, (2) ethoxylated bisphenol a diacrylate, (4) ethoxylated bisphenol a diacrylate, 1,6-ethylene glycol diacrylate, (2) propoxylated neopentyl glycol diacrylate, trimethylolpropane acrylate, (3) ethoxylated trimethylolpropane acrylate, (6) ethoxylated trimethylolpropane acrylate, di-trimethylolpropane tetraacrylate, pentaerythritol tetraacrylate, or (4) ethoxylated pentaerythritol tetraacrylate.
3. The method for pretreating a shaped body according to claim 1, wherein the plasticizer is at least one of polyethylene glycol 200, polyethylene glycol 400, linseed oil, oleic acid, tributyl citrate, acetyl tributyl citrate, trioctyl citrate, glycerol, phenyl alkylsulfonate, dioctyl phthalate, dibutyl phthalate, trioctyl acetyl citrate, cyclohexane 1,2-diisononyl phthalate, or epoxidized soybean oil.
4. The method for pretreating a shaped body according to claim 1, wherein the photoinitiator is one or a combination of more than one of 2-dimethylamino-2-benzyl-1- (4-piperidinophenyl) -1-butanone, 1-hydroxycyclohexylphenylketone, 4,4-bis (diethoxy) benzophenone, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, phenylbis (2,4,6-trimethylbenzoyl) phosphine oxide, 2-methyl-2 (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-propanone, 2-isopropylthioxanthone.
5. The method for pretreating a molded body according to claim 1, wherein the dispersant is at least one of a copolymer having an acid group, a modified polyether having a high pigment affinity, or a polyether polyol-modified polyurethane polymer.
6. The method for pretreating a formed body according to claim 1, wherein the photocurable ceramic slurry comprises the following components in parts by weight: 60 parts of ceramic powder, 20 parts of photosensitive organic matter, 15 parts of plasticizer, 5 parts of liquid paraffin, 1 part of photoinitiator and 1 part of dispersant.
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CN106810215A (en) * | 2017-01-18 | 2017-06-09 | 深圳摩方新材科技有限公司 | A kind of preparation of ceramic size and 3D printing Stereolithography method |
CN106673646A (en) * | 2017-01-20 | 2017-05-17 | 广东工业大学 | Method for preparing zirconium oxide ceramic by 3D (Three Dimensional) printing based on photo-curing molding |
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