CN109734450A - A kind of preparation method of the light sensitive ceramics liquid for photocuring increasing material manufacturing - Google Patents
A kind of preparation method of the light sensitive ceramics liquid for photocuring increasing material manufacturing Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of light sensitive ceramics liquid for photocuring increasing material manufacturing.(1) photosensitive modification is carried out to hydroxy silicon oil: is heated 3-4 hours at 60-80 DEG C after the metallic catalyst of the hydroxy silicon oil of 69-79wt%, the silane coupling agent of 17-27wt%, 4-6wt% are mixed；Modified silicone oil is obtained, the sum of described each liquid percentage is 100%；(2) photosensitive diluent of gained liquid 20-50wt%, the coloring agent of 0-0.1wt%, the photoinitiator of 2-4wt%, to get the light sensitive ceramics liquid for photocuring increasing material manufacturing after mixing are added into liquid obtained by (1).Gained light sensitive ceramics liquid can be used for photocuring increasing material manufacturing, have that volatility is low, environmentally protective advantage.The light sensitive ceramics liquid of gained photocuring increasing material manufacturing is suitable for a variety of photocuring increasing material manufacturing equipment, provides solution for complicated, fine structure ceramics quick, batch productions.
Description
Technical field
The invention belongs to ceramic fields, and in particular to a kind of preparation side of the light sensitive ceramics liquid for photocuring increasing material manufacturing
Method.
Background technique
Ceramic material has the excellent characteristics such as high intensity, high rigidity, high temperature resistant, corrosion-resistant, but traditional ceramics preparation process
If sizing material forming method and dry pressing are difficult to form near-net-shape labyrinth, and green body micro-structure can be caused by being machined
It destroys.Increase material and be shaped to manufacturing theory with cumulative, has the advantages that labyrinth rapid shaping, efficiently production, be very suitable to make
For the preparation method of special-shaped ceramics.
The main application method of the increasing material manufacturing of ceramic material is stereo lithography (SLA), digital optical processing technique
(DLP), selective laser sintering technology (SLS), layer separated growth technology (LOM), inkjet printing technology (IJP), fusion sediment
Forming technique (FDM).Wherein, using photocuring technology as the increases material manufacturing technology of principle, such as stereolithography, digital light processing,
The accuracy of manufacture is other up to micron to nano grade, is the excellent means for producing accurate advanced ceramics structural material.
There are mainly two types of photocuring increasing material manufacturing ceramic material useful raw materials: one is photosensitive resin macromolecule and powder are mixed
Slurry is closed, one is light sensitive ceramics liquid precursors.The former is mainly for the manufacture of oxide ceramics, such as zirconium oxide, aluminium oxide, hydroxyl
Apatite, calcium phosphate, silica etc..For the shrinking percentage for reducing green body in sintering process, photosensitive resin need to uniformly be carried as far as possible
More ceramic powders；In addition to this, powder and liquid resin optical parameter such as refractive index need matched well.But prepare presoma
Ceramic common ceramic liquid precursor --- the problem of two-phase matching is then not present in light sensitive ceramics liquid.Also, with light sensitive ceramics
Liquid is raw material, and design of material scale can be as small as molecular level, have can liquid phase molding, can low-temp ceramics, even green body it is good
Etc. a variety of advantages.
Currently, with the related publication of photocuring 3D printing there are mainly two types of.The first is with photosensitive resin macromolecule
The slurry formed after mixing with powder is raw material manufacture ceramics.Such as a kind of Chinese invention patent " system of 3D printing ceramic slurry
Preparation Method " deionized water, ceramic powder and dispersing agent are subjected to ball milling in (108069704 A of CN), add emulsifier, wadding
The auxiliary agents such as solidifying agent are passed through gas high-speed stirred and emulsify obtained porous ceramics.As Chinese invention patent " beat for photocuring 3D by one kind
The ceramic slurry of print " in (108083817 A of CN) using ceramic powder, dispersing agent, acrylate monomer combination, organic additive,
Photoinitiator etc. prepares ceramic slurry.As Chinese invention patent " provides the light-cured resin based composite ceramic material of bright and clean profile
And idiosome degreasing method " (108249930 A of CN), contacting permeation agent, contour smoothing agent is added in the slurry to improve ceramic slurry
Material system transmission depth reduces compact dimensions error.Although in summary data is it can be found that ceramic slurry prepares ceramics has
The low advantage of shrinking percentage.But in order to keep low-viscosity, holding good light-cured performance while more multiple-bearer powder and divide
Resolution, solve powder etc. second relative to light scattering problems, prevent sintering densification process from generating defect and crackle etc., need
Powder is handled using plurality of reagents during the preparation process, and add a variety of auxiliary agents in the slurry, preparation process complex, no
It is environmentally protective.
Second is to print (compound) resin material by primary raw material of silicone resin.As " a kind of 3D is beaten Chinese invention patent
Print the preparation method and application of ultraviolet curing transparent silicone resin composite material " (105331115 A of CN) middle use low viscosity silicon tree
Relatively soft, not warpage, invariance the silicone resin solidfied material that rouge prepolymer adds reinforcing agent to print；As " 3D is beaten Chinese invention patent
The print preparation method and applications of silicon-containing nano gel light-cured resin " in report silicon-containing nano gel photocuring particle molten
Product after solvent can be used as printing raw material, and printing product has the low advantage of shrinking percentage.But silicon applied by above-mentioned document
Although resin can participate in photocuring printing, it is more difficult for being converted into ceramics by high temperature sintering.This is because it is former
Expect that most solvent content is more, silicon content is few, photocuring is difficult to be crosslinked as close network structure after obtaining blank sintering, it is difficult to convert
For ceramics.
Currently, the case and publication of domestic successful progress light sensitive ceramics liquid precursor preparation are less.This is because,
Firstly, silicone oil selection is more difficult.Macromolecular silicone oil is temperature sensitive, and temperature control is improper in photosensitive modifying process can cause it
Polymerization, makes to increased dramatically in the viscosity short time, to be dfficult to apply to photocuring increasing material manufacturing；And small molecule is silicon oil modified obtains
Light sensitive ceramics liquid precursor, during photocuring increasing material manufacturing, it is difficult to form macromolecular substances in the short time, it is difficult to real
The fast transition of existing liquid-solid, therefore be also difficult to come into operation.Secondly, photosensitive modifying process is complex.Temperature, soda acid
The subtle change of the external factor such as degree easily makes side reaction, destroys target product, leads to modified failure.Again, modified pottery
The photosensitive activity of porcelain liquid is poor.Since modified-reaction is mostly reversible reaction, photosensitive modified-reaction degree is lower, obtained effective product
It is limited.
Content described in this patent is a kind of preparation method of light sensitive ceramics liquid for photocuring increasing material manufacturing, uses this method
The light sensitive ceramics liquid being prepared can be formed using photocuring increasing material manufacturing, and green body after molding occurs in high-temperature sintering process
Organic and inorganic transformation generates silicon-oxygen-carbon ceramic.In the process, ceramic surface and Cross Section Morphology are intact, and surface is without local change
Shape, crackle and expansion, compression strength are megapascal rank.The light sensitive ceramics liquid has stronger light sensitivity, and under light illumination, liquid is handed over
Connection is reticular structure, and realization liquid can be used for photocuring increasing material manufacturing to solid transformation.The light sensitive ceramics liquid volatility
It is low, solidified using photocuring technology, it is environmentally protective.In addition, the light sensitive ceramics liquid can be with the water of at most 40% mass or water-soluble
Liquid dissolves each other, and can dissolve a variety of nitrate insoluble in oily substance including aluminum nitrate, zirconium nitrate, nickel nitrate etc., has
Manufacture the potential quality of composite ceramic material.Preparation process is related to reacting lower to temperature and pH value susceptibility, and reaction process is simpler
It is single.Also, to improve the light sensitivity of liquid, patent creatively proposes that this means of photosensitive diluent, the light being added is added
Quick diluent greatly promotes its photosensitive property while not generating destruction to ceramic liquid.This means has versatility, at it
It can also be applied in his ceramic forerunner system.In addition to this, by changing the content of photosensitive diluent, it can be achieved that photocuring increases material
Effective control of manufacturing speed.
Summary of the invention
The present invention proposes one kind for less situation is studied for the ceramic liquid precursor of photocuring increasing material manufacturing at present
The preparation method of light sensitive ceramics liquid for photocuring increasing material manufacturing.The ceramic liquid being prepared by the preparation method is by light
The processes such as curing molding, drying, heat treatment, can be obtained precursor ceramic.
The present invention is to be achieved by following technical solution.
A kind of preparation method of the light sensitive ceramics liquid for photocuring increasing material manufacturing, specifically implements according to the following steps:
(1) photosensitive modification is carried out to hydroxy silicon oil: by the hydroxy silicon oil of 69-79wt%, 17-27wt% it is silane coupled
It is heated 3-4 hours at 60-80 DEG C after agent, the metallic catalyst mixing of 4-6wt%；Obtain modified silicone oil, each liquid
The sum of body percentage is 100%；
(2) photosensitive diluent of gained liquid 20-50wt%, the dyeing of 0-0.1wt% are added into liquid obtained by (1)
Agent, the photoinitiator of 2-4wt%, to get the light sensitive ceramics liquid for photocuring increasing material manufacturing after mixing.
Hydroxy silicon oil described in step (1) is the liquid silicone that hydroxy radical content is not less than 20%.
Silane coupling agent described in step (1) is γ-methacryloxypropyl trimethoxy silane.
Metallic catalyst described in step (1) is dibutyl tin dilaurate.
Photosensitive diluent described in step (2) be trimethylolpropane trimethacrylate, dipropylene glycol diacrylate or
One of two (trimethylolpropane) tetraacrylates.
Coloring agent described in step (2) is lipid coloring agent, preferably oil red, S Ⅳ.
Photoinitiator described in step (2) is free radical photo-initiation, preferably 2,4,6- trimethylbenzoyl phosphonic acids second
Ester (TPO).
Photocuring technology of the present invention is including but not limited to digital light processing or stereolithography.
Gained light sensitive ceramics liquid can be used for photocuring increasing material manufacturing, have that volatility is low, environmentally protective advantage.This is photosensitive
Ceramic liquid can pour into photocuring increasing material manufacturing machine and carry out increasing material manufacturing, be illustrated with Digital Light Processing apparatus.Liquid need to pour into number
In the liquid bath of word light processing increasing material manufacturing equipment, photocuring increasing material manufacturing is carried out according to preset model, model is with porous structure
Most preferably.When increasing material manufacturing single monolayer thick is 50 μm, the single layer increasing material manufacturing time is 10-21s according to formula rate difference.It obtains
Increasing material manufacturing green body precision can be to micron level.Under normal temperature conditions, green body shrinking percentage is less than or equal to 2%.Photocuring increases material system
After making, green body is removed and obtains silicon oxygen carbon or thyrite by different heat treating regimes.Gained ceramics material
Material is 30-55% relative to green body linear shrinkage ratio；Without partial loop variation, without swelling；Ceramic surface flawless, section cause
It is close；Compression strength is megapascal rank.
The light sensitive ceramics liquid of gained photocuring increasing material manufacturing is suitable for a variety of photocuring increasing material manufacturing equipment, for complicated, essence
Quick, the batch production of close structural ceramics provide solution.
Detailed description of the invention
Fig. 1 is preset model photo in Digital Light Processing apparatus used in embodiment.
Fig. 2 is the super depth of field three-dimensional microscope for the ceramic body that gained raw material is obtained through photocuring increasing material manufacturing in embodiment
Photo.
Fig. 3 is that the super depth of field three-dimensional for the silicon-oxygen-carbon ceramic that ceramic body obtains after drying, heat treatment in embodiment is micro-
Mirror photo.
Fig. 4 is the Electronic Speculum of the artificial section for the silicon-oxygen-carbon ceramic that ceramic body obtains after drying, heat treatment in embodiment
Photo.
Fig. 5 is other green body photos that gained raw material is obtained through photocuring increasing material manufacturing in embodiment.
Specific embodiment
Embodiment 1:
A kind of preparation of the light sensitive ceramics liquid for photocuring increasing material manufacturing precursor ceramic, comprising the following steps:
(1) at room temperature, by 77wt% hydroxy silicon oil (hydroxy radical content 30%), 17wt% γ-methacryloxy third
Base trimethoxy silane, 6wt% dibutyl tin dilaurate after mixing, heat 3.5 hours at 70 DEG C, after be cooled to room
Temperature, for solution at faint yellow, which is modified silicone oil；
(2) two (three hydroxyls of the modified silicone oil 20wt% of gained are added into modified silicone oil obtained in step (1)
Methylpropane) tetraacrylate, the oil red or S Ⅳ of 0.05wt%, the TPO of 4wt% is uniformly mixed, obtains light sensitive ceramics
Liquid is oily liquids；
(3) light sensitive ceramics liquid obtained in step (2), which can be put into digital light processing increasing material manufacturing equipment, is shaped to ceramics
Green body.
Embodiment 2:
A kind of preparation of the light sensitive ceramics liquid for photocuring increasing material manufacturing precursor ceramic, comprising the following steps:
(1) at room temperature, by 79wt% hydroxy silicon oil (hydroxy radical content 20%), 17wt% γ-methacryloxy third
Base trimethoxy silane, 4wt% dibutyl tin dilaurate after mixing, heat 3 hours at 80 DEG C, after be cooled to room
Temperature, for solution at faint yellow, which is modified silicone oil；
(2) dipropylene glycol two of the modified silicone oil 50wt% of gained is added into modified silicone oil obtained in (1)
Acrylate, the TPO of 2wt%, does not add dyestuff, is uniformly mixed, obtains light sensitive ceramics liquid；
(3) light sensitive ceramics liquid obtained in step (2), which can be put into digital light processing increasing material manufacturing equipment, is shaped to ceramics
Green body.
Embodiment 3:
A kind of preparation of the light sensitive ceramics liquid for photocuring increasing material manufacturing precursor ceramic, comprising the following steps:
(1) at room temperature, by 76wt% hydroxy silicon oil (hydroxy radical content 25%), 19wt% γ-methacryloxy third
Base trimethoxy silane, 5wt% dibutyl tin dilaurate heat 4 hours at 60 DEG C, after be cooled to room temperature, solution is at yellowish
Color, the solution are modified silicone oil；
(2) trihydroxy methyl third of the modified silicone oil 30wt% of gained is added into modified silicone oil obtained in (1)
Alkane triacrylate, the oil red or S Ⅳ of 0.05wt%, the TPO of 3wt% are uniformly mixed, obtain light sensitive ceramics liquid；
(3) light sensitive ceramics liquid obtained in step (2), which can be put into digital light processing increasing material manufacturing equipment, is shaped to ceramics
Green body.
Embodiment 4:
A kind of preparation of the light sensitive ceramics liquid for photocuring increasing material manufacturing precursor ceramic, comprising the following steps:
(1) at room temperature, by 71wt% hydroxy silicon oil (hydroxy radical content 30%), 23wt% γ-methacryloxy third
Base trimethoxy silane, 6wt% dibutyl tin dilaurate after mixing, heat 4 hours at 60 DEG C, after be cooled to room
Temperature, for solution at faint yellow, which is modified silicone oil；
(2) trihydroxy methyl third of the modified silicone oil 40wt% of gained is added into modified silicone oil obtained in (1)
Alkane triacrylate, the oil red or S Ⅳ of 0.05wt%, the TPO of 4wt% are uniformly mixed, obtain light sensitive ceramics liquid；
(3) light sensitive ceramics liquid obtained in step (2), which can be put into digital light processing increasing material manufacturing equipment, is shaped to ceramics
Green body.
Embodiment 5:
A kind of preparation of the light sensitive ceramics liquid for photocuring increasing material manufacturing precursor ceramic, comprising the following steps:
(1) at room temperature, by 69wt% hydroxy silicon oil (hydroxy radical content 20%), 27wt% γ-methacryloxy third
Base trimethoxy silane, 4wt% dibutyl tin dilaurate after mixing, heat 3 hours at 80 DEG C, after be cooled to room
Temperature, for solution at faint yellow, which is modified silicone oil；
(2) dipropylene glycol two of the modified silicone oil 50wt% of gained is added into modified silicone oil obtained in (1)
Acrylate, the oil red or S Ⅳ of 0.05wt%, the TPO of 3wt% are uniformly mixed, obtain light sensitive ceramics liquid；
(3) light sensitive ceramics liquid obtained in step (2), which can be put into digital light processing increasing material manufacturing equipment, is shaped to ceramics
Green body.
Embodiment 6:
A kind of preparation of the light sensitive ceramics liquid for photocuring increasing material manufacturing precursor ceramic, comprising the following steps:
(1) at room temperature, by 67wt% hydroxy silicon oil (hydroxy radical content 20%), 27wt% γ-methacryloxy third
Base trimethoxy silane, 6wt% dibutyl tin dilaurate after mixing, heat 3 hours at 80 DEG C, after be cooled to room
Temperature, for solution at faint yellow, which is modified silicone oil；
(2) trihydroxy methyl third of the modified silicone oil 30wt% of gained is added into modified silicone oil obtained in (1)
Alkane triacrylate, the oil red or S Ⅳ of 1wt%, the TPO of 3wt% are uniformly mixed, obtain light sensitive ceramics liquid；
(3) light sensitive ceramics liquid obtained in step (2), which can be put into digital light processing increasing material manufacturing equipment, is shaped to ceramics
Green body.
Digital light processing increasing material manufacturing equipment is put into according to preset model using the light sensitive ceramics liquid prepared in embodiment 1-6
It is shaped to ceramic body.Preset model is as shown in Fig. 1, and appearance is the cylindrical body that diameter is 2cm, and inside is engraved structure.
Molding ceramic body is as shown in Fig. 2, a diameter of 2cm ± 0.2cm, consistent with model structure.The ceramic body is through drying
And high temperature argon tube furnace is sintered to obtain silicon-oxygen-carbon ceramic, as shown in Fig. 3, structure is consistent with model, has compared with moulded dimension
It is shunk, the defects of surface topography and quality are good, no local deformation, flawless and stomata.The Cross Section Morphology of blank structure causes
It is close, flawless stomata, as shown in Fig. 4.The light sensitive ceramics liquid that embodiment 1-6 is prepared also can print other labyrinth bases
Body, as shown in Fig. 5.
A kind of preparation method for light sensitive ceramics liquid for photocuring increasing material manufacturing that the present invention is disclosed and proposed, this field
Technical staff can be by using for reference present disclosure, and the appropriate links such as condition route that change are realized, although method and preparation of the invention
Technology is described by preferred embodiment, related technical personnel obviously can not depart from the content of present invention, spirit and
Methods and techniques described herein route is modified or is reconfigured in range, to realize final technology of preparing.Especially
It should be pointed out that all similar replacements and change it is apparent to those skilled in the art, they all by
It is considered as and is included in spirit of that invention, range and content.
Claims (10)
1. a kind of preparation method of the light sensitive ceramics liquid for photocuring increasing material manufacturing, it is characterized in that including the following steps:
(1) photosensitive modification is carried out to hydroxy silicon oil: by the hydroxy silicon oil of 69-79wt%, the silane coupling agent of 17-27wt%, 4-
It is heated 3-4 hours at 60-80 DEG C after the metallic catalyst mixing of 6wt%；Obtain modified silicone oil, each liquid percentage
Than the sum of be 100%；
(2) photosensitive diluent of gained liquid 20-50wt%, the coloring agent of 0-0.1wt%, 2- are added into liquid obtained by (1)
The photoinitiator of 4wt%, to get the light sensitive ceramics liquid for photocuring increasing material manufacturing after mixing.
2. the method as described in claim 1, it is characterized in that the hydroxy silicon oil is that liquid of the hydroxy radical content not less than 20% is poly-
Siloxanes.
3. the method as described in claim 1, it is characterized in that the silane coupling agent is γ-methacryloxypropyl front three
Oxysilane.
4. the method as described in claim 1, it is characterized in that the metallic catalyst is dibutyl tin dilaurate.
5. the method as described in claim 1, it is characterized in that the photosensitive diluent is trimethylolpropane trimethacrylate, two
One of propylene glycol diacrylate or two (trimethylolpropane) tetraacrylates.
6. the method as described in claim 1, it is characterized in that the coloring agent is lipid coloring agent.
7. the method as described in claim 1, it is characterized in that the coloring agent is oil red or S Ⅳ.
8. the method as described in claim 1, it is characterized in that the photoinitiator is free radical photo-initiation.
9. the method as described in claim 1, it is characterized in that the photoinitiator is 2,4,6- trimethylbenzoyl phosphonic acids second
Ester.
10. the method as described in claim 1, it is characterized in that photocuring technology is including but not limited to digital light processing or cubic light
It carves.
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| CN111362702A (en) * | 2020-03-17 | 2020-07-03 | 中国工程物理研究院激光聚变研究中心 | Preparation method of SiOC radar type wave-absorbing material |
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| CN110467468A (en) * | 2019-09-19 | 2019-11-19 | 广东工业大学 | A kind of photocurable polysilazane and preparation method thereof, SiCN ceramics and preparation method thereof |
| CN110903089A (en) * | 2019-11-27 | 2020-03-24 | 辽宁大学 | SiOC ceramic prepared by 3D printing and preparation method thereof |
| CN111362702A (en) * | 2020-03-17 | 2020-07-03 | 中国工程物理研究院激光聚变研究中心 | Preparation method of SiOC radar type wave-absorbing material |
| CN111362702B (en) * | 2020-03-17 | 2022-05-17 | 中国工程物理研究院激光聚变研究中心 | Preparation method of SiOC radar type wave-absorbing material |
| CN114178704A (en) * | 2021-11-03 | 2022-03-15 | 香港城市大学深圳福田研究院 | Method for producing high-temperature structural material and precursor |
| CN115010877A (en) * | 2022-05-27 | 2022-09-06 | 深圳大学 | Carbon-oxygen-silicon ceramic precursor, thick and compact ceramic part and 3D printing preparation method thereof |
| CN115010877B (en) * | 2022-05-27 | 2023-11-24 | 深圳大学 | Carbon-oxygen-silicon ceramic precursor, thick compact ceramic piece and 3D printing preparation method thereof |
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