CN110511042A - A kind of preparation method of photocuring 3D printing low shrinking ceramic slurry - Google Patents
A kind of preparation method of photocuring 3D printing low shrinking ceramic slurry Download PDFInfo
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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
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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
- C04B35/01—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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- 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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- 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
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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
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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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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Abstract
The invention discloses a kind of preparation methods of photocuring 3D printing low shrinking ceramic slurry, comprising the following steps: 1) is stirred cationic monomer, cationic oligomer, free radical type monomer, free radical type oligomer, cationic initiators, free radical type initiator, dispersing agent to obtain photosensitive resin;2) ceramic powder, dehydrated alcohol, dispersing agent, radical initiator are obtained into surface modified zirconia powder through ball milling mixing, drying;3) photosensitive resin and surface modified zirconia powder ball milling mixing are obtained into ceramic slurry.Photosensitive resin of the present invention is made of cationic system and free radical system, and the shrinkage of photosensitive resin obviously becomes smaller, and slurry volume shrinking percentage prepared by the present invention reaches 2%~5%.
Description
Technical field
The present invention relates to ceramic slurry technical fields, and in particular to be a kind of photocuring 3D printing low shrinking ceramic slurry
Preparation method.
Background technique
Zirconium oxide porcelain material is inorganic non-metallic material.It has high-melting-point, high rigidity, high-wearing feature, resistance to oxidation etc. excellent
Point can be used as structural material, cutter material etc.;Occupy very important status in current Material Field.But it is hard for ceramic material
The advantages of spending high abrasion is but also ceramic material is difficult to form or process device with complex shape, traditional forming method
The easy ceramic part of shape can only be prepared, is unable to satisfy the requirement of today's society, therefore increases material manufacturing technology already
It comes into being.
Photocuring technology have can straight forming go out the advantages of complicated shape ceramics, current photocuring technology is developed existing
Shape, mainly photocuring slurry, the slurry system for influencing ceramic member comprehensive performance are made of photosensitive resin and ceramic powder, and
The main reason for bright quick tree can shrink in solidification, this is influence 3D printing precision, while ceramic powder and resin are mixed
After conjunction be easy sedimentation, slurry system it is unstable, equally will affect printing effect.
Therefore, how reducing the shrinking percentage of 3D printing ceramics and improving the stability of ceramic slurry is one urgently to be solved
Problem.
Summary of the invention
In view of the above shortcomings, the purpose of the present invention is to provide a kind of photocuring 3D printing low shrinking ceramic slurries
Preparation method, the advantage with lower shrinkage.
Technical solution of the present invention is summarized as follows:
A kind of preparation method of photocuring 3D printing low shrinking ceramic slurry, wherein the following steps are included:
1) by cationic monomer, cationic oligomer, free radical type monomer, free radical type oligomer, cationic
Initiator, free radical type initiator, dispersing agent are stirred to obtain photosensitive resin;
2) ceramic powder, dehydrated alcohol, dispersing agent, radical initiator surface is obtained through ball milling mixing, drying to be modified
Zirconium powder;
3) photosensitive resin and surface modified zirconia powder ball milling mixing are obtained into ceramic slurry.
Preferably, the preparation method of the photocuring 3D printing low shrinking ceramic slurry, wherein the step 1) sun
Ionic comonomer is selected from least one of triethylene glycol divinyl ether, dodecyl vinyl;The cationic is oligomeric
Object is selected from least one of aliphatic epoxy resin, cycloaliphatic epoxy resin, modified epoxy.
Preferably, the preparation method of the photocuring 3D printing low shrinking ceramic slurry, wherein the step 1) is certainly
By fundamental mode monomer in dipropylene glycol diacrylate, tripropylene glycol diacrylate, two hexanediyl esters extremely
Few one kind;The free radical type oligomer is selected from epoxy acrylic resin, aliphatic polyurethane acrylic resin, fragrant adoption ammonia
At least one of ester acrylic resin.
Preferably, the preparation method of the photocuring 3D printing low shrinking ceramic slurry, wherein the cationic
Initiator is selected from one of aryl diazonium salts, diaryl iodonium salt, triaryl sulfonium salts, iron arene complexes.
Preferably, the preparation method of the photocuring 3D printing low shrinking ceramic slurry, wherein the free radical type
Initiator is selected from one of acetophenone derivs, acylphosphine oxide, anthraquinone derivative.
Preferably, the preparation method of the photocuring 3D printing low shrinking ceramic slurry, wherein the step 1) and
Dispersing agent is selected from least one of BYK-163, BYK-2008, PM1590, oleic acid in step 2).
Preferably, the preparation method of the photocuring 3D printing low shrinking ceramic slurry, wherein the ceramic powder
For nano zirconium oxide powder, partial size is 0.9~2 μm.
Preferably, the preparation method of the photocuring 3D printing low shrinking ceramic slurry, wherein the cationic
Monomer: cationic oligomer: cationic initiators: the weight percent of dispersing agent is 80:20:0.5%~5%:
0.05%~0.2%;The free radical type monomer: free radical type oligomer: free radical type initiator: the weight percent of dispersing agent
Than for 90%:10%:0.5%~5%:0.05 %~0.2%.
Preferably, the preparation method of the photocuring 3D printing low shrinking ceramic slurry, wherein the step 1) is stirred
Mixing speed is 1500r/min~2000r/min, time 1h.
Preferably, the preparation method of the photocuring 3D printing low shrinking ceramic slurry, wherein the step 2) pottery
Porcelain powder: dehydrated alcohol: radical initiator: the weight percent of dispersing agent is 100%:100%:0.5%~0.2%:
0.05%~0.2%;Step 2) the ball milling mixing specifically: 1h is dispersed with 2000r/min~2500r/min, then
1000r/min~1500r/min disperses 12h;Step 3) the ball milling mixing specifically: 350r/min~650r/min dispersion
20h.Since nano zircite particle surface has great amount of hydroxy group (- OH), lead to the poor compatibility with photosensitive resin, it is heavy to be easy
Drop, so to be modified processing to nano zircite.The slurry of processed nano zirconium oxide powder is added, 20 can be stored
It, does not occur delamination.
The beneficial effects of the present invention are:
(1) photosensitive resin of the present invention is made of cationic system and free radical system, the common photosensitive tree of free radical system
Rouge advantage is that curing reaction speed is fast, the disadvantage is that shrinking greatly, is influenced obviously by oxygen inhibition, cationic system photosensitive resin advantage is
It shrinks small, is not influenced vulnerable to oxygen inhibition, the disadvantage is that curing reaction speed is slow, after two kinds of systems combine, the shrinkage of photosensitive resin
Obviously become smaller, slurry volume shrinking percentage prepared by the present invention reaches 2%~5%.
(2) nano zircite is mixed with free radical type initiator, dispersing agent, dehydrated alcohol, by nano oxidized modified zirconia,
The stability of slurry can be not only greatly improved, but also the ability that curing reaction occurs under ultraviolet light can be improved,
Compensate for the slow defect of cationic system photosensitive resin curing rate.
(3) processed nano zircite is added by carrying out surface modification treatment to nano zircite particle in the present invention
The slurry of powder is stored >=20 days, delamination does not occur.
Detailed description of the invention
Fig. 1 is the schematic diagram of the preparation method of photocuring 3D printing low shrinking ceramic slurry in the present invention.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification
Text can be implemented accordingly.
Embodiment 1:
1) 20g cationic system monomer triethylene glycol divinyl ether, 5g cationic system oligomeric aliphatic epoxy are weighed
Resin, 0.125g cation light initiator triaryl sulfonium salts and 0.0125g dispersant B YK-2008, weigh 22.5g dipropyl two
Alcohol diacrylate, 2.5g epoxy acrylic resin, 0.125g free radical photo-initiation acylphosphine oxide and 0.0125g points
Powder BYK-2008, is added in the beaker of 500ml, and disperses 40min in high speed disperser with 1500r/min, prepares
Photosensitive resin;
2) it weighs 300g nano zirconium oxide powder to be added in the polyurethane ball-milling pot of 1L, pours into the anhydrous second of about 300g
In addition alcohol adds the radical initiator acylphosphine oxide of 1.5g and the dispersing agent PM1590 of 0.15g, then starts to be expert at
In star ball-grinding machine, 1h is dispersed with 2000r/min, 8h is being dispersed with 1000r/min, is being subsequently placed in 60 DEG C of baking ovens 24 hours,
Obtain the modified nano zircite in surface.
3) nano zircite for taking the surface of 292.5g modified is mixed with the above-mentioned photosensitive resin of 50g, in planetary ball mill equipment
In with 400r/min dispersion for 24 hours.The white slurry of solid content 50% is obtained by filtration, white slurry is poured into hopper and is used for light and consolidates
The SLA equipment for changing principle carries out 3D printing molding, cubical contraction 3.6%, appearance N/D.
Embodiment 2:
1) 20g cationic system monomer dodecyl vinyl, 5g cationic system oligomer alicyclic epoxy are weighed
Resin, 0.25g cation light initiator triaryl sulfonium salts and 0.025g dispersant B YK-2008, weigh the free matrix of 22.5g
It is monomer tripropylene glycol diacrylate, 2.5g free radical system oligomeric aliphatic polyurethane acrylic resin, 0.25g freedom
Base photoinitiator acylphosphine oxide and 0.025g dispersant B YK-2008, are added in the beaker of 500ml, and in high speed point
It dissipates in machine and 40min is dispersed with 1600r/min, prepare photosensitive resin;
2) it weighs 300g nano zirconium oxide powder to be added in the polyurethane ball-milling pot of 1L, pours into the anhydrous second of about 300g
In addition alcohol adds the radical initiator acylphosphine oxide of 3.0g and the dispersing agent oleic acid of 0.3g, in planetary ball mill equipment
In, 1h is dispersed with 2100r/min, 8h is being dispersed with 1100r/min, is being subsequently placed in 60 DEG C of baking ovens 24 hours, is obtained to surface and change
Property nano zircite.
3) the surface-modified nano zirconium oxide of 292.5g is taken to mix with 50g photosensitive resin, in planetary ball mill equipment with
500r/min disperses for 24 hours, the white slurry of solid content 50% to be obtained by filtration, and white slurry is poured into hopper and is used for photocuring original
The SLA equipment of reason carries out 3D printing molding, cubical contraction 2.8%, appearance N/D.
Embodiment 3:
1) 20g cationic system monomer dodecyl vinyl, 5g cationic system oligomer modified epoxy tree are weighed
Rouge, 0.5g cation light initiator triaryl sulfonium salts and 0.05g dispersant B YK-163, weigh 22.5g free radical system monomer
Two hexanediyl esters, 2.5g free radical system oligomer aromatic urethane acrylic resin, 0.5g free radical light draw
Send out agent acylphosphine oxide and 0.05g dispersant B YK-163, be added in the beaker of 500ml, and in high speed disperser with
1700r/min disperses 40min, prepares photosensitive resin.
2) it weighs 300g nano zirconium oxide powder to be added in the polyurethane ball-milling pot of 1L, pours into the anhydrous second of about 300g
In addition alcohol adds the radical initiator acylphosphine oxide of 4.5g and the dispersing agent oleic acid of 0.45g, in planetary ball mill equipment
In, 1h is dispersed with 2200r/min, 8h is being dispersed with 1200r/min, is being subsequently placed in 60 DEG C of baking ovens 24 hours, is obtained to surface and change
The nano zircite of property.
3) nano zircite for taking the surface of 292.5g modified is mixed with the above-mentioned photosensitive resin of 50g, in planetary ball mill equipment
In with 450r/min dispersion for 24 hours, the white slurry of solid content 50% is obtained by filtration, white slurry is poured into hopper and is used for light and consolidates
The SLA equipment for changing principle carries out 3D printing molding, cubical contraction 4.1%, appearance N/D.
The test result of Examples 1 to 3 is listed below:
It can be seen from the data in Table 1 that photocuring 3D printing low shrinking ceramic slurry of the invention carries out 3D printing, produce
Product shrinking percentage≤4.1%, shrinking percentage is low, and product stability is high.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details.
Claims (10)
1. a kind of preparation method of photocuring 3D printing low shrinking ceramic slurry, which comprises the following steps:
1) cationic monomer, cationic oligomer, free radical type monomer, free radical type oligomer, cationic are caused
Agent, free radical type initiator, dispersing agent are stirred to obtain photosensitive resin;
2) by ceramic powder, dehydrated alcohol, dispersing agent, radical initiator through ball milling mixing, to obtain surface modified oxidized for drying
Zirconium powder body;
3) photosensitive resin and surface modified zirconia powder ball milling mixing are obtained into ceramic slurry.
2. the preparation method of photocuring 3D printing low shrinking ceramic slurry according to claim 1, which is characterized in that described
Step 1) cationic monomer is selected from least one of triethylene glycol divinyl ether, dodecyl vinyl;It is described sun from
Subtype oligomer is selected from least one of aliphatic epoxy resin, cycloaliphatic epoxy resin, modified epoxy.
3. the preparation method of photocuring 3D printing low shrinking ceramic slurry according to claim 1, which is characterized in that described
Step 1) free radical type monomer is selected from dipropylene glycol diacrylate, tripropylene glycol diacrylate, two hexanediyls
At least one of ester;The free radical type oligomer is selected from epoxy acrylic resin, aliphatic polyurethane acrylic resin, virtue
At least one of fragrant adoption urethane acrylate resin.
4. the preparation method of photocuring 3D printing low shrinking ceramic slurry according to claim 1, which is characterized in that described
Cationic initiators are selected from one of aryl diazonium salts, diaryl iodonium salt, triaryl sulfonium salts, iron arene complexes.
5. the preparation method of photocuring 3D printing low shrinking ceramic slurry according to claim 1, which is characterized in that described
Free radical type initiator is selected from one of acetophenone derivs, acylphosphine oxide, anthraquinone derivative.
6. the preparation method of photocuring 3D printing low shrinking ceramic slurry according to claim 1, which is characterized in that described
Dispersing agent is selected from least one of BYK-163, BYK-2008, PM1590, oleic acid in step 1) and step 2).
7. the preparation method of photocuring 3D printing low shrinking ceramic slurry according to claim 1, which is characterized in that described
Ceramic powder is nano zirconium oxide powder, and partial size is 0.9~2 μm.
8. the preparation method of photocuring 3D printing low shrinking ceramic slurry according to claim 1, which is characterized in that described
Cationic monomer: cationic oligomer: cationic initiators: the weight percent of dispersing agent be 80:20:0.5%~
5%:0.05%~0.2%;The free radical type monomer: free radical type oligomer: free radical type initiator: the weight of dispersing agent
Percentage is 90%:10%:0.5%~5%:0.05%~0.2%.
9. the preparation method of photocuring 3D printing low shrinking ceramic slurry according to claim 1, which is characterized in that described
Step 1) mixing speed is 1500r/min~2000r/min, time 1h.
10. the preparation method of photocuring 3D printing low shrinking ceramic slurry according to claim 1, which is characterized in that institute
State step 2) ceramic powder: dehydrated alcohol: radical initiator: the weight percent of dispersing agent is 100%:100%:0.5%
~0.2%:0.05%~0.2%;Step 2) the ball milling mixing specifically: 1h is dispersed with 2000r/min~2500r/min,
Then 1000r/min~1500r/min disperses 12h;Step 3) the ball milling mixing specifically: 350r/min~650r/min points
Dissipate 20h.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114921115A (en) * | 2022-03-25 | 2022-08-19 | 深圳职业技术学院 | Yttrium-stabilized zirconia ceramic slurry and preparation method and application thereof |
CN116283241A (en) * | 2023-04-03 | 2023-06-23 | 广州瑞鑫通科技有限公司 | Preparation method of photo-curing 3D printing alumina ceramic paste slurry |
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CN109809824A (en) * | 2017-11-21 | 2019-05-28 | 辽宁省轻工科学研究院 | A kind of photocuring ceramic slurry and quick molding method |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114921115A (en) * | 2022-03-25 | 2022-08-19 | 深圳职业技术学院 | Yttrium-stabilized zirconia ceramic slurry and preparation method and application thereof |
CN114921115B (en) * | 2022-03-25 | 2023-05-09 | 深圳职业技术学院 | Yttrium stabilized zirconia ceramic slurry and its preparation method and application |
CN116283241A (en) * | 2023-04-03 | 2023-06-23 | 广州瑞鑫通科技有限公司 | Preparation method of photo-curing 3D printing alumina ceramic paste slurry |
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