CN116655358A - Alumina micro-structural member material for DLP and preparation method thereof - Google Patents

Alumina micro-structural member material for DLP and preparation method thereof Download PDF

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CN116655358A
CN116655358A CN202310718950.7A CN202310718950A CN116655358A CN 116655358 A CN116655358 A CN 116655358A CN 202310718950 A CN202310718950 A CN 202310718950A CN 116655358 A CN116655358 A CN 116655358A
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alumina
structural member
micro
dlp
alumina powder
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刘耀
吴杰华
杨华杰
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Jiangxi Jinshi 3d Intelligent Manufacturing Technology Co ltd
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Jiangxi Jinshi 3d Intelligent Manufacturing Technology Co ltd
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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
    • 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
    • B33Y10/00—Processes of additive manufacturing
    • 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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    • 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
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B35/63—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
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
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    • 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
    • C04B35/63—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
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63488—Polyethers, e.g. alkylphenol polyglycolether, polyethylene glycol [PEG], polyethylene oxide [PEO]
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    • 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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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The application is applicable to the technical field of materials, and provides an alumina micro-structural member material for DLP and a preparation method thereof, wherein the alumina micro-structural member material comprises the following components: 70-90 parts of modified alumina powder, 0-25 parts of epoxy acrylate, 5-25 parts of 1, 6-hexanediol diacrylate, 0.05-0.1 part of phenyl bis (2, 4, 6-trimethyl benzoyl) phosphine oxide, 0.05-0.1 part of 1-hydroxycyclohexyl phenyl ketone and 0.1-0.5 part of defoamer; according to the application, the specific activated and modified alumina powder is added into the resin system, so that the solid phase content of the alumina and the resin during mixing is greatly improved, the photo-curing molding effect is not influenced, the hardness and strength of the finished alumina micro-structural member are enhanced, and the finished alumina micro-structural member has excellent mechanical properties.

Description

Alumina micro-structural member material for DLP and preparation method thereof
Technical Field
The application belongs to the technical field of materials, and particularly relates to an alumina micro-structural member material for DLP and a preparation method thereof.
Background
As a common metal oxide, the alumina has the advantages of high hardness, high strength, high temperature resistance and the like, and is widely applied to the fields of refractory materials, structural materials, functional ceramics and the like. With the development of functional ceramic materials, higher requirements are put on the performance and structure of the materials. Meanwhile, the trend of device integration and miniaturization requires the ceramic material to be reduced in size as much as possible. Alumina has great advantages as a low-cost and widely-used functional ceramic material. However, conventional die pressing and numerical control cutting have been difficult to meet for the preparation of small-sized ceramic materials, and new forming methods have been sought.
The DLP technology is a 3D printing technology based on a photo-curing principle, and can rapidly prepare an alumina model with a specific shape according to a computer model, and remove resin components through degreasing and sintering to obtain the alumina micro-structural member. However, compared with the traditional aluminum oxide parts processed by die pressing, the strength of the aluminum oxide prepared by the DLP technology is lower, and further optimization is needed to meet the use requirements.
Disclosure of Invention
The embodiment of the application provides an alumina micro-structural member material for DLP, which aims to solve the problem of lower strength of alumina prepared by a DLP technology.
The embodiment of the application is realized in such a way that the alumina micro-structural member material for DLP comprises the following raw materials in parts by weight:
70-90 parts of modified alumina powder, 0-25 parts of epoxy acrylate, 5-25 parts of 1, 6-hexanediol diacrylate, 0.05-0.1 part of phenyl bis (2, 4, 6-trimethyl benzoyl) phosphine oxide, 0.05-0.1 part of 1-hydroxycyclohexyl phenyl ketone and 0.1-0.5 part of defoamer;
the preparation method of the modified alumina powder comprises the following steps:
performing reduced pressure rotary evaporation on the alumina powder at 80-120 ℃ to complete the activation treatment;
dispersing activated alumina powder in absolute ethyl alcohol, adding 0.01-0.05wt% of composite surfactant, stirring and dispersing to obtain a mixture;
slowly dripping the high polymer hyperdispersant into the mixture through a constant pressure dropping funnel for reflux reaction, drying and sieving to obtain the high polymer hyperdispersant.
The embodiment of the application also provides a preparation method of the alumina micro-structural member material for DLP, which comprises the following steps:
mixing 0-25 parts of epoxy acrylate, 5-25 parts of 1, 6-hexanediol diacrylate, 0.05-0.1 part of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.05-0.1 part of 1-hydroxycyclohexyl phenyl ketone by stirring to obtain photo-curing resin;
adding 70-90 parts of modified alumina powder into the photo-curing resin, adding 0.1-0.5 part of defoaming agent, and performing ball milling and stirring to obtain alumina photo-curing slurry;
curing the alumina slurry by using a DLP photo-curing printer to obtain a micro-structural member model;
and degreasing and sintering the micro-structural member model to obtain the aluminum oxide micro-structural member material.
According to the alumina micro-structural member material for DLP provided by the embodiment of the application, the epoxy acrylate, the 1, 6-hexanediol diacrylate, the phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and the 1-hydroxycyclohexyl phenyl ketone are mixed to form a resin system, and further the alumina powder subjected to specific activation modification treatment is added into the resin system, so that the solid phase content of alumina and resin during mixing is greatly improved, the photo-curing molding effect is not influenced, the hardness and strength of a finished alumina micro-structural member are enhanced, and the finished alumina micro-structural member has excellent mechanical properties.
Detailed Description
The present application will be described in further detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present application more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The embodiment of the application provides an alumina micro-structural member material for DLP, which comprises the following raw materials in parts by mass:
70-90 parts of modified alumina powder, 0-25 parts of epoxy acrylate, 5-25 parts of 1, 6-hexanediol diacrylate, 0.05-0.1 part of phenyl bis (2, 4, 6-trimethyl benzoyl) phosphine oxide, 0.05-0.1 part of 1-hydroxycyclohexyl phenyl ketone and 0.1-0.5 part of defoamer.
The main reason for the lower strength of the alumina prepared by the existing DLP technology is that the high curing content and the curing performance cannot be considered, the proportion of alumina in a system is likely to be increased in order to improve the strength of the alumina, but the curing performance of the resin is affected due to the increase of the content of the alumina, so that more defects are left when the product is photocured and formed, and therefore, how to consider the mechanical property and the curing performance of the product is a problem of important research. According to the application, epoxy acrylate, 1, 6-hexanediol diacrylate, phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 1-hydroxycyclohexyl phenyl ketone are mixed to form a resin system, and then the alumina powder subjected to specific activation modification treatment is added into the resin system, so that the solid phase content of alumina and resin during mixing is greatly improved, the photo-curing molding effect is not influenced, the hardness and strength of a finished alumina micro-structural member are enhanced, and the finished alumina micro-structural member has excellent mechanical properties.
In the present application, the method for preparing the modified alumina powder comprises the steps of:
and step S1, performing reduced pressure rotary evaporation on the alumina powder at the temperature of 80-120 ℃ to complete the activation treatment.
Specifically, the alumina powder was subjected to rotary evaporation under reduced pressure at 80 to 120℃for 3 to 4 hours to complete the activation treatment.
And S2, dispersing the activated alumina powder in absolute ethyl alcohol, adding 0.01-0.05wt% of composite surfactant, and stirring and dispersing to obtain a mixture.
Specifically, dispersing activated alumina powder in absolute ethyl alcohol, adding 0.01-0.05wt% of composite surfactant, and dispersing for 2-3h at the temperature of 80-100 ℃ with the stirring rate of 300-700r/min to obtain a mixture.
Wherein the compound surfactant consists of fatty alcohol polyoxyethylene-3 ether and polyoxyethylene-9 laurate. The mass ratio of the fatty alcohol polyoxyethylene-3 ether to the lauric acid polyoxyethylene-9 ester is 2:1.
Wherein the mass ratio of the alumina to the absolute ethyl alcohol is 1:10.
And S3, slowly dripping the high-molecular hyperdispersant into the mixture through a constant-pressure dropping funnel for reflux reaction, drying and sieving to obtain the high-molecular hyperdispersant.
Specifically, the high molecular hyperdispersant is slowly dripped into the mixture through a constant pressure dropping funnel, the mass ratio of the alumina powder to the high molecular hyperdispersant is controlled to be (70-90) (1-5), the dripping time is controlled to be 20-50min, the reflux temperature is controlled to be 70-110 ℃, the reflux reaction time is controlled to be 3-6h, and the high molecular hyperdispersant is obtained after drying and sieving.
Wherein the macromolecular hyperdispersant is one or more of EFKA 4703, solsperse AC7570 and Solsperse 41000.
The embodiment of the application provides a preparation method of an alumina micro-structural member material for DLP, which comprises the following steps:
mixing 0-25 parts of epoxy acrylate, 5-25 parts of 1, 6-hexanediol diacrylate, 0.05-0.1 part of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.05-0.1 part of 1-hydroxycyclohexyl phenyl ketone by stirring to obtain photo-curing resin;
adding 70-90 parts of modified alumina powder into the photo-curing resin, adding 0.1-0.5 part of defoaming agent, and performing ball milling and stirring to obtain alumina photo-curing slurry;
curing the alumina slurry by using a DLP photo-curing printer to obtain a micro-structural member model;
and degreasing and sintering the micro-structural member model to obtain the aluminum oxide micro-structural member material.
The step of degreasing and sintering the micro-structural member model to obtain the aluminum oxide micro-structural member material comprises the following steps:
and (3) placing the micro-structural member model in a muffle furnace, heating to 500 ℃ at 0.1-2 ℃/min, heating to 1500-1600 ℃ at 5-10 ℃/min, and preserving heat for 3-5 hours to obtain the aluminum oxide micro-structural member material.
Examples of certain embodiments of the application are given below and are not intended to limit the scope of the application.
In addition, it should be noted that the numerical values set forth in the following examples are as precise as possible, but those skilled in the art will understand that each numerical value should be construed as a divisor rather than an absolute precise numerical value due to measurement errors and experimental operation problems that cannot be avoided.
Example 1
Performing reduced pressure rotary evaporation on the alumina powder for 3 hours at the temperature of 100 ℃ to complete the activation treatment; dispersing activated alumina powder in absolute ethyl alcohol, adding 0.03wt% of a composite surfactant (composed of fatty alcohol polyoxyethylene-3 ether and lauric acid polyoxyethylene-9 ester with the mass ratio of 2:1), controlling the stirring rate to be 500r/min, dispersing at 90 ℃ for 2.5h, and controlling the mass ratio of the alumina to the absolute ethyl alcohol to be 1:10, so as to obtain a mixture; slowly dripping EFKA 4703 into the mixture through a constant pressure dropping funnel, controlling the mass ratio of alumina powder to high polymer hyperdispersant to be 80:3, controlling the dripping time to be 30min, controlling the reflux temperature to be 90 ℃, controlling the reflux reaction time to be 4h, and sieving after drying.
Fully and uniformly stirring and mixing 10g of epoxy acrylate, 20g of 1, 6-hexanediol diacrylate, 0.05g of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.05g of 1-hydroxycyclohexyl phenyl ketone to obtain photo-curing resin; 70g of modified alumina powder and 0.5g of BYK1790 defoamer are added, ball milling and stirring are carried out, and the mixture is completely and uniformly mixed to obtain the alumina photo-curing slurry.
And (3) shaping the alumina photo-curing slurry by using a DLP printer to obtain an alumina blank, heating to 500 ℃ at 0.5 ℃/min in a muffle furnace, heating to 1500 ℃ at 10 ℃/min, and preserving heat for 4 hours to obtain the alumina micro-structural part.
Example 2
Performing reduced pressure rotary evaporation on the alumina powder for 3 hours at the temperature of 100 ℃ to complete the activation treatment; dispersing activated alumina powder in absolute ethyl alcohol, adding 0.03wt% of a composite surfactant (composed of fatty alcohol polyoxyethylene-3 ether and lauric acid polyoxyethylene-9 ester with the mass ratio of 2:1), controlling the stirring rate to be 500r/min, dispersing at 90 ℃ for 2.5h, and controlling the mass ratio of the alumina to the absolute ethyl alcohol to be 1:10, so as to obtain a mixture; slowly dripping EFKA 4703 into the mixture through a constant pressure dropping funnel, controlling the mass ratio of alumina powder to EFKA 4703 to be 80:3, controlling the dripping time to be 30min, controlling the reflux temperature to be 90 ℃, controlling the reflux reaction time to be 4h, and sieving after drying.
Fully and uniformly stirring and mixing 15g of epoxy acrylate, 15g of 1, 6-hexanediol diacrylate, 0.05g of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.05g of 1-hydroxycyclohexyl phenyl ketone to obtain photo-curing resin; 70g of modified alumina powder and 0.5g of BYK1790 defoamer are added, ball milling and stirring are carried out, and the mixture is completely and uniformly mixed to obtain the alumina photo-curing slurry.
And (3) shaping the alumina photo-curing slurry by using a DLP printer to obtain an alumina blank, heating to 500 ℃ at 0.5 ℃/min in a muffle furnace, heating to 1500 ℃ at 10 ℃/min, and preserving heat for 4 hours to obtain the alumina micro-structural part.
Example 3
Performing reduced pressure rotary evaporation on the alumina powder for 3 hours at the temperature of 100 ℃ to complete the activation treatment; dispersing activated alumina powder in absolute ethyl alcohol, adding 0.03wt% of a composite surfactant (composed of fatty alcohol polyoxyethylene-3 ether and lauric acid polyoxyethylene-9 ester with the mass ratio of 2:1), controlling the stirring rate to be 500r/min, dispersing at 90 ℃ for 2.5h, and controlling the mass ratio of the alumina to the absolute ethyl alcohol to be 1:10, so as to obtain a mixture; slowly dripping EFKA 4703 into the mixture through a constant pressure dropping funnel, controlling the mass ratio of alumina powder to EFKA 4703 to be 80:3, controlling the dripping time to be 30min, controlling the reflux temperature to be 90 ℃, controlling the reflux reaction time to be 4h, and sieving after drying.
Fully and uniformly stirring and mixing 20g of epoxy acrylate, 10g of 1, 6-hexanediol diacrylate, 0.05g of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.05g of 1-hydroxycyclohexyl phenyl ketone to obtain photo-curing resin; 70g of modified alumina powder and 0.5g of BYK1790 defoamer are added, ball milling and stirring are carried out, and the mixture is completely and uniformly mixed to obtain the alumina photo-curing slurry.
And (3) shaping the alumina photo-curing slurry by using a DLP printer to obtain an alumina blank, heating to 500 ℃ at 0.5 ℃/min in a muffle furnace, heating to 1500 ℃ at 10 ℃/min, and preserving heat for 4 hours to obtain the alumina micro-structural part.
Example 4
Performing reduced pressure rotary evaporation on the alumina powder for 3 hours at the temperature of 100 ℃ to complete the activation treatment; dispersing activated alumina powder in absolute ethyl alcohol, adding 0.03wt% of a composite surfactant (composed of fatty alcohol polyoxyethylene-3 ether and lauric acid polyoxyethylene-9 ester with the mass ratio of 2:1), controlling the stirring rate to be 500r/min, dispersing at 90 ℃ for 2.5h, and controlling the mass ratio of the alumina to the absolute ethyl alcohol to be 1:10, so as to obtain a mixture; slowly dripping EFKA 4703 into the mixture through a constant pressure dropping funnel, controlling the mass ratio of alumina powder to EFKA 4703 to be 80:3, controlling the dripping time to be 30min, controlling the reflux temperature to be 90 ℃, controlling the reflux reaction time to be 4h, and sieving after drying.
Fully and uniformly stirring and mixing 7g of epoxy acrylate, 13g of 1, 6-hexanediol diacrylate, 0.05g of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.05g of 1-hydroxycyclohexyl phenyl ketone to obtain a photo-curing resin; 80g of modified alumina powder and 0.5g of BYK1790 defoamer are added, ball milling and stirring are carried out, so that the mixture is completely and uniformly mixed to obtain the alumina photo-curing slurry.
And (3) shaping the alumina photo-curing slurry by using a DLP printer to obtain an alumina blank, heating to 500 ℃ at 0.5 ℃/min in a muffle furnace, heating to 1500 ℃ at 10 ℃/min, and preserving heat for 4 hours to obtain the alumina micro-structural part.
Example 5
Performing reduced pressure rotary evaporation on the alumina powder for 3 hours at the temperature of 100 ℃ to complete the activation treatment; dispersing activated alumina powder in absolute ethyl alcohol, adding 0.03wt% of a composite surfactant (composed of fatty alcohol polyoxyethylene-3 ether and lauric acid polyoxyethylene-9 ester with the mass ratio of 2:1), controlling the stirring rate to be 500r/min, dispersing at 90 ℃ for 2.5h, and controlling the mass ratio of the alumina to the absolute ethyl alcohol to be 1:10, so as to obtain a mixture; slowly dripping EFKA 4703 into the mixture through a constant pressure dropping funnel, controlling the mass ratio of alumina powder to EFKA 4703 to be 80:3, controlling the dripping time to be 30min, controlling the reflux temperature to be 90 ℃, controlling the reflux reaction time to be 4h, and sieving after drying.
Fully and uniformly stirring and mixing 3g of epoxy acrylate, 7g of 1, 6-hexanediol diacrylate, 0.05g of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.05g of 1-hydroxycyclohexyl phenyl ketone to obtain photo-curing resin; 90g of modified alumina powder and 0.5g of BYK1790 defoamer are added, ball milling and stirring are carried out, so that the mixture is completely and uniformly mixed to obtain the alumina photo-curing slurry.
And (3) shaping the alumina photo-curing slurry by using a DLP printer to obtain an alumina blank, heating to 500 ℃ at 0.5 ℃/min in a muffle furnace, heating to 1500 ℃ at 10 ℃/min, and preserving heat for 4 hours to obtain the alumina micro-structural part.
Example 6
Performing reduced pressure rotary evaporation on the alumina powder for 3 hours at the temperature of 100 ℃ to complete the activation treatment; dispersing activated alumina powder in absolute ethyl alcohol, adding 0.03wt% of a composite surfactant (composed of fatty alcohol polyoxyethylene-3 ether and lauric acid polyoxyethylene-9 ester with the mass ratio of 2:1), controlling the stirring rate to be 500r/min, dispersing at 90 ℃ for 2.5h, and controlling the mass ratio of the alumina to the absolute ethyl alcohol to be 1:10, so as to obtain a mixture; slowly dripping EFKA 4703 into the mixture through a constant pressure dropping funnel, controlling the mass ratio of alumina powder to EFKA 4703 to be 80:3, controlling the dripping time to be 30min, controlling the reflux temperature to be 90 ℃, controlling the reflux reaction time to be 4h, and sieving after drying.
Fully stirring and uniformly mixing 7g of epoxy acrylate, 13g of 1, 6-hexanediol diacrylate, 0.1g of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.1g of 1-hydroxycyclohexyl phenyl ketone to obtain a photo-curing resin; 80g of modified alumina powder and 0.5g of BYK1790 defoamer are added, ball milling and stirring are carried out, so that the mixture is completely and uniformly mixed to obtain the alumina photo-curing slurry.
And (3) shaping the alumina photo-curing slurry by using a DLP printer to obtain an alumina blank, heating to 500 ℃ at 0.5 ℃/min in a muffle furnace, heating to 1500 ℃ at 10 ℃/min, and preserving heat for 4 hours to obtain the alumina micro-structural part.
The hardness and the bending strength of the aluminum oxide micro-structural parts prepared in examples 1 to 6 are tested according to national standards, and the test results are shown in table 1.
TABLE 1
Microhardness HV Flexural Strength/MPa
Example 1 1315 637
Example 2 1324 644
Example 3 1329 630
Example 4 1396 733
Example 5 1292 587
Example 6 1412 745
In summary, as can be seen from table 1, the aluminum oxide micro-structural materials for DLP provided in examples 1 to 6 of the present application all have higher hardness and strength. Among them, it was found from the comparison of examples 1 to 3 that the ratio of epoxy acrylate and 1, 6-hexanediol diacrylate had less effect on the sample strength, and the change ratio had a major effect on the exposure parameters during the photo-curing. As is evident from the comparison of examples 1, 4-6, the increase of the solid phase content significantly improves the mechanical properties of the product, but when the mass ratio of the sum of the modified alumina powder and the epoxy acrylate-1, 6-hexanediol diacrylate reaches 9: the sample strength showed a significant decrease in the trend at 1.
The following is a related experimental study of the application with respect to the effect of modification process parameters of alumina powder on sample strength:
(1) Varying the effect of the activation treatment parameters on the sample strength
Under other conditions, only the alumina powder activation treatment temperature was changed. According to the method in the present specification, alumina powder is subjected to rotary evaporation under reduced pressure at 80 ℃ to complete the activation treatment; dispersing activated alumina powder in absolute ethyl alcohol, adding 0.03wt% of a composite surfactant (composed of fatty alcohol polyoxyethylene-3 ether and lauric acid polyoxyethylene-9 ester with the mass ratio of 2:1), controlling the stirring rate to be 500r/min, dispersing at 90 ℃ for 2.5h, and controlling the mass ratio of the alumina to the absolute ethyl alcohol to be 1:10, so as to obtain a mixture; slowly dripping EFKA 4703 into the mixture through a constant pressure dropping funnel, controlling the mass ratio of alumina powder to EFKA 4703 to be 80:3, controlling the dripping time to be 30min, controlling the reflux temperature to be 90 ℃, controlling the reflux reaction time to be 4h, drying and sieving to obtain the modified alumina, and marking as experiment 1. The above experiment was repeated at a temperature of 90℃and 100℃and 110℃and 120℃with the activation treatment temperature being changed, and the result was designated as experiment 2-5.
80g of the modified alumina powder prepared in experiments 1-5 is respectively added into a resin system (7 g of epoxy acrylate, 13g of 1, 6-hexanediol diacrylate, 0.05g of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.05g of 1-hydroxycyclohexyl phenyl ketone), then 0.5g of BYK1790 defoamer is added, and ball milling and stirring are carried out to completely and uniformly mix the components to obtain the alumina photo-curing slurry. And (3) shaping the alumina photo-curing slurry by using a DLP printer to obtain an alumina blank, heating to 500 ℃ at 0.5 ℃/min in a muffle furnace, heating to 1500 ℃ at 10 ℃/min, and preserving heat for 4 hours to obtain the alumina micro-structural part. Comparative experiment 1 was prepared in the same manner, wherein the alumina powder in comparative experiment 1 was not subjected to the activation treatment. The results of the intensity test are shown in Table 2.
TABLE 2 influence of varying the activation treatment parameters on sample strength
(2) Changing the influence of EFKA 4703 dripping time on the sample strength
In the case where other conditions are not changed, only the dropping time of EFKA 4703 is changed. According to the method in the present specification, alumina powder is subjected to rotary evaporation under reduced pressure at 100 ℃ to complete the activation treatment; dispersing activated alumina powder in absolute ethyl alcohol, adding 0.03wt% of a composite surfactant (composed of fatty alcohol polyoxyethylene-3 ether and lauric acid polyoxyethylene-9 ester with the mass ratio of 2:1), controlling the stirring rate to be 500r/min, dispersing at 90 ℃ for 2.5h, and controlling the mass ratio of the alumina to the absolute ethyl alcohol to be 1:10, so as to obtain a mixture; slowly dripping EFKA 4703 into the mixture through a constant pressure dropping funnel, controlling the mass ratio of alumina powder to EFKA 4703 to be 80:3, controlling the dripping time to be 20min, controlling the reflux temperature to be 90 ℃, controlling the reflux reaction time to be 4h, drying and sieving to obtain the modified alumina, and recording as experiment 6. The above experiment was repeated with the dropping time changed to 30min, 40min, and 50min, respectively, and recorded as experiment 7-9.
80g of the modified alumina powder prepared in experiment 6-9 is respectively added into a resin system (7 g of epoxy acrylate, 13g of 1, 6-hexanediol diacrylate, 0.05g of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.05g of 1-hydroxycyclohexyl phenyl ketone), then 0.5g of BYK1790 defoamer is added, and ball milling and stirring are carried out to completely and uniformly mix the components, so as to obtain the alumina photo-curing slurry. And (3) shaping the alumina photo-curing slurry by using a DLP printer to obtain an alumina blank, heating to 500 ℃ at 0.5 ℃/min in a muffle furnace, heating to 1500 ℃ at 10 ℃/min, and preserving heat for 4 hours to obtain the alumina micro-structural part. The results of the intensity test are shown in Table 3.
TABLE 3 influence of varying EFKA 4703 addition time on sample strength
(3) Varying the influence of reflux reaction temperature/reaction time on sample strength
Under otherwise unchanged conditions, only the reflux reaction temperature/reaction time was changed. According to the method in the present specification, alumina powder is subjected to rotary evaporation under reduced pressure at 100 ℃ to complete the activation treatment; dispersing activated alumina powder in absolute ethyl alcohol, adding 0.03wt% of a composite surfactant (composed of fatty alcohol polyoxyethylene-3 ether and lauric acid polyoxyethylene-9 ester with the mass ratio of 2:1), controlling the stirring rate to be 500r/min, dispersing at 90 ℃ for 2.5h, and controlling the mass ratio of the alumina to the absolute ethyl alcohol to be 1:10, so as to obtain a mixture; slowly dripping EFKA 4703 into the mixture through a constant pressure dropping funnel, controlling the mass ratio of alumina powder to EFKA 4703 to be 80:3, controlling the dripping time to be 30min, controlling the reflux temperature to be 80 ℃, controlling the reflux reaction time to be 4h, drying and sieving to obtain the modified alumina, and recording as experiment 10. The reflux temperature is changed to 90 ℃, 100 ℃ and 110 ℃ respectively; the reflux reaction time was changed to 3h, 5h, and 6h, respectively, and the above experiment was repeated and recorded as experiments 11 to 16.
80g of the modified alumina powder prepared in experiments 10-16 was added to a resin system (7 g of epoxy acrylate, 13g of 1, 6-hexanediol diacrylate, 0.05g of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, 0.05g of 1-hydroxycyclohexyl phenyl ketone), and then 0.5g of BYK1790 defoamer was added thereto, followed by ball milling and stirring to completely and uniformly mix them, thereby obtaining an alumina photo-curing slurry. And (3) shaping the alumina photo-curing slurry by using a DLP printer to obtain an alumina blank, heating to 500 ℃ at 0.5 ℃/min in a muffle furnace, heating to 1500 ℃ at 10 ℃/min, and preserving heat for 4 hours to obtain the alumina micro-structural part. The results of the intensity test are shown in Table 4.
TABLE 4 influence of varying reflux reaction temperature/reaction time on sample strength
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.

Claims (10)

1. The alumina micro-structural member material for the DLP is characterized by comprising the following raw materials in parts by weight:
70-90 parts of modified alumina powder, 0-25 parts of epoxy acrylate, 5-25 parts of 1, 6-hexanediol diacrylate, 0.05-0.1 part of phenyl bis (2, 4, 6-trimethyl benzoyl) phosphine oxide, 0.05-0.1 part of 1-hydroxycyclohexyl phenyl ketone and 0.1-0.5 part of defoamer;
the preparation method of the modified alumina powder comprises the following steps:
performing reduced pressure rotary evaporation on the alumina powder at 80-120 ℃ to complete the activation treatment;
dispersing activated alumina powder in absolute ethyl alcohol, adding 0.01-0.05wt% of composite surfactant, stirring and dispersing to obtain a mixture;
slowly dripping the high polymer hyperdispersant into the mixture through a constant pressure dropping funnel for reflux reaction, drying and sieving to obtain the high polymer hyperdispersant.
2. The aluminum oxide micro-structural member material for DLP according to claim 1, wherein the composite surfactant is composed of fatty alcohol polyoxyethylene-3 ether and polyoxyethylene-9 laurate.
3. The aluminum oxide micro-structural member material for DLP according to claim 1, wherein the mass ratio of the fatty alcohol polyoxyethylene-3 ether to the lauric acid polyoxyethylene-9 ester is 2:1.
4. The alumina micro-structural material for DLP according to claim 1, wherein the high molecular hyperdispersant is one or more of EFKA 4703, solsperse AC7570, solsperse 41000.
5. The aluminum oxide micro-structural member material for DLP according to claim 1, wherein the step of subjecting the aluminum oxide powder to reduced pressure rotary evaporation at 80 to 120 ℃ to complete the activation treatment comprises:
the alumina powder was subjected to rotary evaporation under reduced pressure at 80-120℃for 3-4 hours to complete the activation treatment.
6. The alumina micro-structural member material for DLP according to claim 1, wherein the activated alumina powder is dispersed in absolute ethanol while adding 0.01-0.05wt% of a complex surfactant, and stirring and dispersing to obtain a mixture, comprising:
dispersing activated alumina powder in absolute ethyl alcohol, adding 0.01-0.05wt% of composite surfactant, controlling stirring speed to 300-700r/min, and dispersing at 80-100deg.C for 2-3h to obtain a mixture.
7. The alumina micro-structural member material for DLP according to claim 1, wherein the step of slowly dropping the polymeric hyperdispersant into the mixture through a constant pressure dropping funnel to perform reflux reaction, drying and sieving comprises the steps of:
slowly dripping the high-molecular hyperdispersant into the mixture through a constant-pressure dropping funnel, controlling the mass ratio of the alumina powder to the high-molecular hyperdispersant to be (70-90) (1-5), controlling the dripping time to be 20-50min, controlling the reflux temperature to be 70-110 ℃, controlling the reflux reaction time to be 3-6h, and sieving after drying.
8. The aluminum oxide micro-structural member material for DLP according to claim 1, wherein the mass ratio of the aluminum oxide to the absolute ethanol is 1:10.
9. The preparation method of the alumina micro-structural member material for the DLP is characterized by comprising the following steps of:
mixing 0-25 parts of epoxy acrylate, 5-25 parts of 1, 6-hexanediol diacrylate, 0.05-0.1 part of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and 0.05-0.1 part of 1-hydroxycyclohexyl phenyl ketone by stirring to obtain photo-curing resin;
adding 70-90 parts of modified alumina powder into the photo-curing resin, adding 0.1-0.5 part of defoaming agent, and performing ball milling and stirring to obtain alumina photo-curing slurry;
curing the alumina slurry by using a DLP photo-curing printer to obtain a micro-structural member model;
and degreasing and sintering the micro-structural member model to obtain the aluminum oxide micro-structural member material.
10. The method for preparing an alumina micro-structural member material for DLP according to claim 9, wherein the step of degreasing and sintering the micro-structural member model to obtain the alumina micro-structural member material comprises the steps of:
and (3) placing the micro-structural member model in a muffle furnace, heating to 500 ℃ at 0.1-2 ℃/min, heating to 1500-1600 ℃ at 5-10 ℃/min, and preserving heat for 3-5 hours to obtain the aluminum oxide micro-structural member material.
CN202310718950.7A 2023-06-16 2023-06-16 Alumina micro-structural member material for DLP and preparation method thereof Pending CN116655358A (en)

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CN106966709A (en) * 2017-04-01 2017-07-21 广东工业大学 A kind of preparation method of transparent alumina ceramics
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CN110480792A (en) * 2019-08-01 2019-11-22 苏州铼赛智能科技有限公司 Manufacturing method, system, 3D printing equipment and image processing method
CN113929500A (en) * 2021-10-08 2022-01-14 西安交通大学 Method for preparing aluminum oxide ceramic surface composite coating for vacuum arc-extinguishing chamber through 3D printing
CN115386051A (en) * 2022-10-09 2022-11-25 江西金石三维智能制造科技有限公司 Light-cured resin for DLP (digital light processing) and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004315340A (en) * 2003-02-26 2004-11-11 Kyocera Corp Method for manufacturing three-dimensional structure and sintered ceramic compact using the same
CN104971693A (en) * 2014-04-09 2015-10-14 中国石油化工股份有限公司 Aluminum moulded material containing nonionic surfactant, preparation and application thereof
CN106966709A (en) * 2017-04-01 2017-07-21 广东工业大学 A kind of preparation method of transparent alumina ceramics
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