CN111269007A - Ceramic photocuring slurry and preparation method thereof - Google Patents
Ceramic photocuring slurry and preparation method thereof Download PDFInfo
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- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
The invention is applicable to the technical field of materials, and provides a ceramic photocuring slurry and a preparation method thereof, wherein the ceramic photocuring slurry comprises the following raw materials in percentage by weight: 50-80% of ceramic powder, 0.05-0.4% of first dispersing agent, 18.2-49.55% of resin and 0.4-2.4% of second dispersing agent; the surface of the ceramic powder contains hydroxyl, and the ceramic photocuring slurry is prepared by the following steps: modifying the surface of the ceramic powder by using a first dispersing agent to obtain modified ceramic powder; and mixing the modified ceramic powder, the resin and the second dispersing agent to obtain the ceramic powder. According to the invention, the surface of the ceramic powder is modified by the first dispersing agent, so that the ceramic powder and the resin are better in affinity, and further the ceramic light-cured slurry is obtained by matching with the resin and the second dispersing agent.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to ceramic photocuring slurry and a preparation method thereof.
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, and the principle of the method is that ultraviolet laser is irradiated on the surface of ceramic slurry with photosensitive characteristic to excite free radical polymerization reaction, so that a laser scanning area forms a cured layer; then the solidified layer descends by a platform height, the uncured slurry is paved on 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 through the layer-layer curing combination mode, and then the green body is degreased, sintered and post-processed to form finished ceramic.
The existing ceramic photocuring slurry mainly comprises the following components: ceramic powder, oligomer, monomer diluent, dispersant, photoinitiator, plasticizer and the like, and in order to achieve the mechanical properties required by structural ceramics, the mass ratio of the ceramic powder in the formula is required to be as high as possible. For example, in order to improve the mechanical properties of an alumina/zirconia photocurable slurry system, it is generally required that the weight ratio of the ceramic powder is 75% or more. While the slurry required by printing equipment adopting SLA (photo-curing molding) as a principle has to ensure good fluidity, the viscosity is less than 5Pa.s, and under general conditions, a proper single dispersant can achieve a good viscosity reduction effect, however, certain contradiction often exists between viscosity reduction and storage stability, namely, although the fluidity of the slurry with lower viscosity is good, the phenomenon of hard agglomeration at the bottom of the slurry can occur after the slurry is stored for a period of time, so that the stability of the slurry and the printing stability are seriously influenced; while the higher viscosity slurry can increase the storage stability, it can affect the slurry transportation and the slurry scraping and leveling during the printing process.
Therefore, the existing ceramic photocuring slurry has the problems that the balance between the viscosity and the storage stability cannot be achieved, and the stability of the slurry and the printing stability are seriously influenced.
Disclosure of Invention
The embodiment of the invention provides a ceramic photocuring slurry, and aims to solve the problems that the existing ceramic photocuring slurry cannot achieve balance between viscosity and storage stability, and the slurry stability and printing stability are seriously affected.
The embodiment of the invention is realized in such a way that the ceramic photocuring slurry comprises the following raw materials in percentage by weight:
50 to 80 percent of ceramic powder, 0.05 to 0.4 percent of first dispersant, 18.2 to 49.55 percent of resin and 0.4 to 2.4 percent of second dispersant;
the surface of the ceramic powder contains hydroxyl, and the ceramic photocuring slurry is prepared by the following steps:
modifying the surface of the ceramic powder by using a first dispersing agent to obtain modified ceramic powder;
and mixing the modified ceramic powder, resin and a second dispersing agent to obtain the ceramic powder.
The embodiment of the invention also provides a preparation method of the ceramic photocuring slurry, which comprises the following steps:
weighing the following raw materials in percentage by weight: 50 to 80 percent of ceramic powder, 0.05 to 0.4 percent of first dispersant, 18.2 to 49.55 percent of resin and 0.4 to 2.4 percent of second dispersant;
modifying the surface of the ceramic powder by using a first dispersing agent to obtain modified ceramic powder;
and mixing the modified ceramic powder, resin and a second dispersing agent to obtain the ceramic powder.
In the embodiment of the invention, the surface of the ceramic powder is modified by the first dispersing agent, so that the ceramic powder has better affinity with resin, and is further matched with the resin and the second dispersing agent to obtain the ceramic photocuring slurry.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The storage stability of the slurry is generally solved by adding some commercial thickeners, such as modified hydrogenated castor oil, fumed silica, bentonite, polyethylene wax, polyamide wax, etc., and the principle of the thickener is that the substances added into the photocurable slurry form a space network structure, so that the slurry generates thixotropy, and the stability of the slurry is enhanced. However, in the printing process of the liquid photo-curing paste, the thixotropy can cause instability in the paste conveying link and the printing link, because the good fluidity of the paste is required in both the pumping link and the printing link.
The embodiment of the invention provides ceramic photocuring slurry for ceramic 3D printing, wherein the surface of ceramic powder is modified by a first dispersing agent, so that the better affinity of the ceramic powder and resin is facilitated, and the ceramic photocuring slurry is obtained by matching with the resin and a second dispersing agent.
In the embodiment of the invention, the ceramic photocuring slurry comprises the following raw materials in percentage by weight:
50 to 80 percent of ceramic powder, 0.05 to 0.4 percent of first dispersant, 18.2 to 49.55 percent of resin and 0.4 to 2.4 percent of second dispersant;
the ceramic photocuring slurry is prepared by the following steps:
modifying the surface of the ceramic powder by using a first dispersing agent to obtain modified ceramic powder;
and mixing the modified ceramic powder, resin and a second dispersing agent to obtain the ceramic powder.
In the embodiment of the present invention, the ceramic powder is an oxide ceramic powder, and may be an alumina ceramic powder, or a silica ceramic powder, or a zirconia ceramic powder, and the surface of the ceramic powder contains hydroxyl groups, and the ceramic powder is obtained by purchasing the ceramic powder from alumina manufacturers such as Alteo corporation, products of sumitomo corporation, zirconia manufacturers such as oriental zirconia industry, sai china corporation, etc., and silica manufacturers such as himei powder technology ltd, etc., and has an average particle size: 0.2-10 μm, and it is noted that the ceramic powder used in the present invention is not limited by the manufacturer.
In the embodiment of the invention, the first dispersant is one or more of capric acid, lauric acid, myristic acid, palmitic acid, pearlescent aliphatic acid, stearic acid, arachidic acid, methacryloyloxyethyl maleic acid monoester, alkyl acrylate phosphate, decylamine, laurylamine, palmitylamine, myristylamine and stearylamine.
In an embodiment of the invention, the second dispersant consists of a low molecular weight dispersant with a molecular weight <10000 and a high molecular weight dispersant with a molecular weight > 20000. The two dispersants can be added separately or simultaneously in the preparation process, and the system effect is not influenced, for example, a low molecular weight dispersant is added before the modified ceramic powder is added, and a high molecular weight dispersant is added after the modified ceramic powder is added.
Wherein the low molecular weight dispersant mainly plays a role in viscosity reduction, is a polymer containing good anchoring groups for the powder, is preferably a dispersant containing phosphate ester, and has the molecular weight of less than 10000; the high molecular weight dispersant provides better stability, has molecular weight more than 20000, belongs to a super dispersant, and has excellent anchoring groups for powder; wherein, the low molecular weight dispersant comprises but is not limited to one or more of BYK111, BYK102, Solsperse 41000, Solsperse 85000, Digao DISPER655, EFKA 4701, EFKA 4732 and the like of Bisco chemical company, and the high molecular weight dispersant is one or more of Solsperse 32000, Solsperse 39000 and Solsperse75000 of Bisco chemical company.
Wherein the mass ratio of the low molecular weight dispersant with the molecular weight of less than 10000 to the high molecular weight dispersant with the molecular weight of more than 20000 is 1-5: 1.
In the embodiment of the invention, the resin is a light-cured resin capable of free radical polymerization, and the light-cured resin is epoxy acrylate oligomer, polyester acrylate oligomer, polyurethane acrylate oligomer, aliphatic polyurethane acrylate oligomer, (2) ethoxylated bisphenol A diacrylate, (4) ethoxylated bisphenol A diacrylate, 1, 6-ethylene glycol diacrylate, tripropylene glycol diacrylate, dipropylene glycol diacrylate, polyethylene glycol (200) diacrylate, polyethylene glycol (400) diacrylate, polyethylene glycol (600) diacrylate, (2) propoxylated neopentyl glycol diacrylate, tricyclodecane dimethanol diacrylate, trimethylolpropane acrylate, isobornyl acrylate, cyclotrimethylolpropane formal acrylate, ethoxylated trimethylolpropane acrylate, ethylene oxide, propylene oxide, or the like, (6) Ethoxylated trimethylolpropane acrylate, di-trimethylolpropane tetraacrylate, pentaerythritol tetraacrylate, (4) ethoxylated pentaerythritol tetraacrylate, and the like.
The embodiment of the invention also provides a preparation method of the ceramic photocuring slurry, which comprises the following steps:
weighing the following raw materials in percentage by weight: 50 to 80 percent of ceramic powder, 0.05 to 0.4 percent of first dispersant, 18.2 to 49.55 percent of resin and 0.4 to 2.4 percent of second dispersant;
modifying the surface of the ceramic powder by using the first dispersant to obtain modified ceramic powder;
and mixing the modified ceramic powder, resin and a second dispersing agent to obtain the ceramic powder.
In a preferred embodiment of the present invention, the step of modifying the surface of the ceramic powder with the first dispersant to obtain a modified ceramic powder specifically includes:
and adding the first dispersing agent into an organic solvent, fully mixing, adding the ceramic powder, and performing ball milling and drying pretreatment to obtain the modified ceramic powder.
In the examples of the present invention, the specific kind of the organic solvent is not limited, and absolute ethyl alcohol is used in the following specific examples.
In a preferred embodiment of the present invention, the step of adding the first dispersant into an organic solvent, mixing thoroughly, adding the ceramic powder, and performing ball milling and drying pretreatment to obtain a modified ceramic powder specifically includes:
adding the first dispersing agent into an organic solvent, adding the ceramic powder after ultrasonic dissolution is complete, ball-milling for 2-5 hours at a rotating speed of 160-320 rpm, and placing at 60-140 ℃ for drying pretreatment to obtain modified ceramic powder.
In a preferred embodiment of the present invention, the step of mixing the modified ceramic powder, the resin, and the second dispersant specifically includes:
and (3) placing the resin and the second dispersing agent in a ball milling tank for full ball milling, adding the pretreated ceramic powder, and continuing to perform full ball milling to obtain the ceramic photocuring slurry.
In a preferred embodiment of the present invention, the step of placing the resin and the second dispersant in a ball mill tank for sufficient ball milling, adding the pretreated ceramic powder, and continuing to perform sufficient ball milling to obtain the ceramic photocuring slurry specifically includes:
and placing the resin and the second dispersing agent into a ball milling tank, performing ball milling dispersion for 0.5-4 hours at a rotating speed of 120-300 revolutions per minute, adding the pretreated ceramic powder, performing ball milling for 10-24 hours, and discharging to obtain the ceramic photocuring slurry.
The technical effects of the ceramic photocurable slurry and the preparation method thereof according to the present invention will be further described with reference to the following specific examples, but the specific implementation methods mentioned in these examples are only illustrative and explanatory of the technical solution of the present invention, and do not limit the implementation scope of the present invention, and all modifications and substitutions based on the above principles should be within the protection scope of the present invention.
Example 1
Taking 160g of absolute ethyl alcohol in a beaker, adding 0.2g of stearic acid, dissolving by ultrasonic waves, pouring into a ball milling tank, adding a zirconium oxide milling medium, adding 200g of alumina ceramic powder, ball milling for 3 hours in a ball mill at 240rpm, discharging, and drying at 100 ℃ to obtain modified ceramic powder;
weighing 30g of propoxylated neopentyl glycol diacrylate in a ball milling tank, weighing 2.5g of BYK111 dispersant, adding zirconia milling media, uniformly mixing, adding 150g of modified ceramic powder, placing in a planetary ball mill, performing ball milling for 19h at the rotating speed of 180rpm, adding 2g of high molecular weight dispersant Solsperse 39000, performing ball milling for 3.5h at the rotating speed of 240rpm, and discharging to obtain the modified neopentyl glycol diacrylate powder.
Example 2
Taking 160g of absolute ethyl alcohol in a beaker, adding 1g of lauric acid, dissolving by ultrasonic waves, pouring into a ball milling tank, adding a zirconia milling medium, adding 200g of alumina ceramic powder, ball milling for 3 hours in a ball mill at 240rpm, discharging, and drying at 100 ℃ to obtain modified ceramic powder;
weighing 30g of cyclotrimethylolpropane methylal acrylate in a ball milling tank, then weighing 4.6g of disper655 dispersant, adding zirconia milling media, uniformly mixing, then adding 150g of modified ceramic powder, placing in a planetary ball mill, carrying out ball milling for 19h at the rotating speed of 180rpm, then adding 1.1g of high molecular weight dispersant Solsperse 39000, carrying out ball milling for 3.5h at the rotating speed of 240rpm, and discharging to obtain the high-molecular-weight modified ceramic powder.
Comparative example 1
On the basis of the modified ceramic powder prepared in example 2, 30g of cyclotrimethylolpropane methylal acrylate was weighed in a ball mill pot, 5.7g of disper655 dispersant was weighed, zirconia milling media was added, the mixture was mixed uniformly, 150g of the modified ceramic powder was added, the mixture was placed in a planetary ball mill, and ball milling was carried out at 180rpm for 24 hours to obtain the final product.
Comparative example 2
On the basis of the modified ceramic powder prepared in example 1, 30g of propoxylated neopentyl glycol diacrylate was weighed in a ball mill pot, 4.5g of high molecular weight dispersant Solsperse 39000 was then weighed, zirconia milling media was added, the mixture was mixed uniformly, 150g of the modified ceramic powder was then added, the mixture was placed in a planetary ball mill and ball-milled for 24 hours at a rotational speed of 180rpm, and the product was obtained.
Respectively testing the viscosity of the ceramic photocuring slurry prepared in the examples 1-2 and the comparative examples 1-2 when the slurry is cooled to room temperature, wherein the viscosity is tested on an SNB-2 type rotational viscometer, and a 4# rotor is adopted to test the viscosity value at the rotating speed of 60 rpm; and the slurry was placed in a 50ml small beaker and allowed to stand at normal temperature and pressure to examine the settling property of the slurry, and the results are shown in table 1.
TABLE 1
In summary, as can be seen from table 1, the ceramic photocuring pastes prepared in examples 1-2 of the present invention all have good storage stability and anti-settling property, and the viscosity is maintained to be less than 5 pa.s; according to the test results of the example 1 and the comparative example 2, although the viscosity can be obviously reduced by adopting a single dispersant in the comparative example 2, the settling property is far inferior to that of the example 1, and the practical situation of ceramic 3D printing is integrated, the slurry has high enough anti-settling property to avoid the bad phenomena of uneven printing property and the like caused by the settling of the slurry in the printing process; according to the test results of the example 2 and the comparative example 1, the example 2 is obviously stronger in slurry viscosity and settling property than the comparative example 1 which only adopts one dispersant; the embodiment of the invention can ensure that the storage stability of the slurry is better by matching the high molecular weight dispersant and the low molecular weight dispersant of the second dispersant, can ensure that the slurry has high enough anti-settling property, and avoids the bad phenomena of uneven printing performance and the like caused by the settling of the slurry in the printing process.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The ceramic photocuring slurry is characterized by comprising the following raw materials in percentage by weight:
50-80% of ceramic powder, 0.05-0.4% of first dispersing agent, 18.2-49.55% of resin and 0.4-2.4% of second dispersing agent;
the surface of the ceramic powder contains hydroxyl, and the ceramic photocuring slurry is prepared by the following steps:
modifying the surface of the ceramic powder by using a first dispersing agent to obtain modified ceramic powder;
and mixing the modified ceramic powder, resin and a second dispersing agent to obtain the ceramic powder.
2. The ceramic photocuring paste of claim 1, wherein the first dispersant is one or more of capric acid, lauric acid, myristic acid, palmitic acid, pearlescent acid, stearic acid, arachidic acid, methacryloyloxyethyl maleate monoester, alkyl acrylate phosphate, decylamine, laurylamine, palmitylamine, myristylamine, and stearylamine.
3. The ceramic photocuring paste of claim 1, wherein the second dispersant consists of a low molecular weight dispersant having a molecular weight of <10000 and a high molecular weight dispersant having a molecular weight of > 20000.
4. The ceramic photocurable slurry according to claim 3, wherein said low molecular weight dispersant having a molecular weight <10000 is a phosphate-containing dispersant.
5. The ceramic photocuring paste of claim 3, wherein the high molecular weight dispersant having a molecular weight of >20000 is a hyperdispersant.
6. The ceramic photocuring paste according to claim 3, wherein the mass ratio of the low-molecular-weight dispersant having a molecular weight of <10000 to the high-molecular-weight dispersant having a molecular weight of >20000 is 1-5: 1.
7. The ceramic photocurable paste according to claim 1, wherein said resin is a photocurable resin capable of undergoing radical polymerization.
8. A method for preparing a ceramic photocuring paste according to any one of claims 1 to 7, comprising:
weighing the following raw materials in percentage by weight: 50-80% of ceramic powder, 0.05-0.4% of first dispersing agent, 18.2-49.55% of resin and 0.4-2.4% of second dispersing agent;
modifying the surface of the ceramic powder by using the first dispersant to obtain modified ceramic powder;
and mixing the modified ceramic powder, resin and a second dispersing agent to obtain the ceramic powder.
9. The method for preparing ceramic photocuring slurry according to claim 8, wherein the step of modifying the surface of the ceramic powder with the first dispersant to obtain modified ceramic powder specifically comprises:
and adding the first dispersing agent into an organic solvent, fully mixing, adding the ceramic powder, and performing ball milling and drying pretreatment to obtain the modified ceramic powder.
10. The method for preparing ceramic photocuring slurry according to claim 8, wherein the step of mixing the modified ceramic powder, resin and second dispersant comprises:
and (3) placing the resin and the second dispersing agent in a ball milling tank for full ball milling, adding the pretreated ceramic powder, and continuing to perform full ball milling to obtain the ceramic photocuring slurry.
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