CN109761608A - A method of rodlike composite transparent ceramic is prepared based on direct write molding 3D printing technique - Google Patents
A method of rodlike composite transparent ceramic is prepared based on direct write molding 3D printing technique Download PDFInfo
- Publication number
- CN109761608A CN109761608A CN201910171710.3A CN201910171710A CN109761608A CN 109761608 A CN109761608 A CN 109761608A CN 201910171710 A CN201910171710 A CN 201910171710A CN 109761608 A CN109761608 A CN 109761608A
- Authority
- CN
- China
- Prior art keywords
- direct write
- ceramic
- printing
- ceramics
- liquid storage
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a kind of methods for preparing rodlike composite transparent ceramic based on direct write molding 3D printing technique, and step is: preparing 3D printing rare earth doped ceramics slurry Re:M and the undoped ceramic slurry M of rare earth respectively；The two different slurries of Re:M, M are transferred to respectively in the liquid storage device A and liquid storage device B of 3D printing direct write rapidform machine, design the three-dimensional structure of composite transparent ceramic, and write direct write printing shaping program, accurate control Re:M, M slurry enters the rate of nozzle chamber and the printing rate of direct write rapidform machine, realizes that radially continuous alternation occurs slurry for the relative amount of two kinds of ceramic slurries at different location；Then composite ceramics green body further progress isostatic cool pressing after molding and low-temperature defatted processing carry out long-time sintering under the conditions of high-temperature vacuum and hot isostatic pressing respectively, realize the continuously distributed of crystalline ceramics concentration gradient by the thermal diffusion of Doped ions.This method preparation is simple, and condition is controllable, easily operated popularization.
Description
Technical field
The invention belongs to field of ceramic preparation technology, are related to a kind of preparation of crystalline ceramics, and in particular to one kind is based on straight
The method that write forming 3D printing technique prepares rodlike composite transparent ceramic.
Background technique
Crystalline ceramics as a kind of novel optics polycrystalline material, because its with excellent mechanical performance, thermal property with
And the features such as optical property, was always treated as that monocrystalline can be replaced to become for high power solid state laser at the past 20 years
Actual gain medium.However when large power pumping optical acts on the ceramics, what material internal was generated because absorbing a large amount of pump lights
Fuel factor problem, which becomes, restricts the critical bottleneck that its acquisition is more preferably applied.The heat management regulation method of conventional laser material is mainly sharp
The after-heat in laser medium is removed with heat sink equal cooling mode, this cooling method inevitably results in material surface and inside
Inhomogeneous cooling and space heat consumption be unevenly distributed, final result will cause shown in laser ceramics internal temperature uneven distribution.This
The difference of kind Temperature Distribution causes material internal respectively to differential expansion, to generate serious fuel factor and enable crystal modification, significant to drop
Low pump light is in brilliant intracorporal transfer efficiency.In order to efficiently solve " fuel factor " this problem from material itself, phase at present
Guan researcher generally focuses on the research of layered, transparent ceramics, which is based primarily upon the preparation process of high technology ceramics using more
Prepared by the lamination compact technique of layer green body, it is intended to alleviate material in pumping light action by the controllable design to ceramic structure
Influence of the lower fuel factor to laser activity.
So far, for the research of solid laser material composite construction, there are mainly of two types.First is that with thermal diffusion key
The bonded crystals of conjunction technology preparation are research object.For example, Kracht in 2005 et al. utilizes the rodlike of 5 sections of different levels of doping
Compound Nd:YAG crystal realizes the laser output power of 407W, and its maximum temperature and stress all significantly decrease.
Anhui ray machine institute, Chinese Academy of Sciences Fang in 2017 et al. has studied the GYSGG crystal for the output of 2.79m laser, and discovery passes through design
The influence that fuel factor exports laser can be effectively reduced in the composite construction of laser crystal, significantly improves laser output quality.
Er:Yb:YAl is respectively adopted in Fujian Inst. of Matter Structure, Chinese Academy of Sciences Huang Yidong researchers in 2018 and its Team Member3
(BO3)4/YAl3(BO3)4And sapphire/Er:Yb:YAl3(BO3)4/ sapphire composite crystal as working-laser material, wherein
Using doped portion as gain media, it is used as heat absorption medium undoped with part, result of study shows can using the composite construction
To be effectively improved influence of the fuel factor to laser output quality, facilitate the continuous laser output of high-quality.Another kind of is with essence
The layered, transparent ceramics of fine ceramic technique preparation are research object as laser gain medium.For example, Harbin industry in 2016
University Ma et al. was discussed in detail YAG/Nd:YAG/YAG three-stage composite ceramics and Nd:YAG block ceramic in heat distribution and swashed
It is relatively excellent in terms of thermo parameters method to confirm that concentration gradient laser ceramics has from experimental viewpoint for characteristic in terms of optical property
Gesture.Shanghai University Of Engineering Science Cheng in 2017 et al. carries out analog study using Matlab software, has analysed in depth Tm:YAG
Thermo parameters method characteristic of the gradient type composite ceramics under optical pumping effect, demonstrates from theoretical visual angle along single direction gradient
The laser ceramics of structure has unique modulating properties in heat distribution management aspect.The famous ceramic science man of Japan in 2018
Ikesue et al., which further points out the multistage crystalline ceramics based on the preparation of thermal bonding technology, to be had in the property such as machinery, optics, calorifics
The excellent characteristics of energy aspect can realize that high-efficiency and continuous laser exports as gain media.The above research sufficiently shows solid
Laser material is designed to that composite construction helps to optimize material thermo parameters method internal under optical pumping effect, realizes efficiently high
Quality laser output.
Nevertheless, the research work of associated laser material still faces lot of challenges.First from the preparation angle of material
For, the preparation of the concentration gradient crystalline ceramics with excellent optical quality is mainly still based on thermal diffusion bonding techniques, but
The technology is high for precision polishing technique requirement, and ceramic surface flatness needs to reach Nano grade after polishing, while must also
The technology having in terms of crystalline ceramics seriously must be limited using expensive post-hiped technique, these process conditions
Effect is used.Secondly, the research of crystalline ceramics gradient composite construction is concentrated mainly on the one of Doped ions through-thickness at present
Tie up concentration distribution, for Doped ions concentration gradient multi-dimensional design and cut out and its caused thermo parameters method to laser export
The influencing mechanism of characteristic is rarely reported at present.
Summary of the invention
The object of the present invention is to provide a kind of sides that rodlike composite transparent ceramic is prepared based on direct write molding 3D printing technique
Method, realize Doped ions concentration in ceramic body radially there is two-dimentional concentration gradient distribution.
To achieve the above object, The technical solution adopted by the invention is as follows: a kind of form 3D printing technique system based on direct write
The method of standby rodlike composite transparent ceramic, comprising the following steps:
S1,3D printing rare earth doped ceramics slurry Re:M and the undoped ceramic slurry M of rare earth are prepared respectively；
S2, liquid storage device A and the storage that the two different slurries of Re:M, M are transferred to 3D printing direct write rapidform machine respectively
In liquid device B, and one end of liquid storage device A and liquid storage device B is made to be connected respectively with the adapter of gas pressure regulator, liquid storage device A and storage
The other end of liquid device B is connect with the nozzle chamber of direct write rapidform machine respectively, and gas cylinder A passes through pressure valve A connection pressure control
Device, gas cylinder B pass through pressure valve B connection nozzle chamber；
S3, using the three-dimensional structure of computer-aided software engineering composite transparent ceramic, and write direct write and be printed as
Type program adjusts total gas pressure P, the P range of two liquid storage devices of input in 10Pa~2 × 10 by pressure valve A6Pa, according to ceramics
Depending on the viscosity of slurry is of different sizes, the air pressure P of input liquid storage device A is then adjusted by Partial Pressure Controller1With input liquid storage device B
Air pressure P2, P1、P2Scope control is 0~2 × 106Pa and meet P=P1+P2, so that accurately control Re:M, M slurry enters spray
The rate of mouth cavity, the sum of feed rate of two kinds of slurries range adjust input spray in 0~1000ml/min, by pressure valve B
The intracorporal air pressure P ' of mouth chamber and P '≤P, the accurate printing rate for controlling direct write rapidform machine；By way of being successively superimposed,
The radially printing speed molding for realizing two kinds of slurries of Re:M, M, obtains rod shaped ceramic idiosome；
S4, the ceramic idiosome of direct write printing shaping is first subjected to cold isostatic compaction under pressure, it then will be cold
Green body after isostatic pressing, which is placed under oxygen atmosphere, carries out low-temperature defatted processing；
S5, the green body after degreasing is subjected to high-temperature vacuum sintering, obtains fine and close ceramic sintered bodies；
S6, sintered ceramic body successively carry out high annealing and precise polished processing under the conditions of oxygen-containing atmosphere.
Preferably, in step S1, ceramic slurry preparation process is: by a certain proportion of material powder, solvent, dispersing agent,
Binder and plasticiser carry out ball milling mixing, and the ceramic slurry of suitable solid content and viscosity is made, wherein the solvent be go from
Sub- water, solid content are 50vol%~55vol%, and the additional amount of the dispersing agent is 2wt.%, and the additional amount of the binder is
1.5wt.%, the additional amount of the plasticiser are 2wt.%.
Preferably, the dispersing agent is glycerine, and the binder is polyvinyl alcohol, and the plasticiser is polyethylene glycol.
Preferably, in step S1, ceramic M is yttrium oxide, luteium oxide, scandium oxide, Y3Al5O12, Lu3Al5O12One of,
Rare earth Re is neodymium, ytterbium, erbium, thulium, holmium, dysprosium, praseodymium, samarium, chromium, one of lanthanum.
Preferably, in step S3, the printing rate is 50~1000ml/min.
Preferably, in step S4, the pressure limit of the isostatic cool pressing is in 100~200MPa, 2~10min of dwell time；
700~800 DEG C of the ungrease treatment temperature range, 5~20h of calcination time.
Preferably, in step S5, vacuum ranges < 10-3Pa, vacuum-sintering temperature range are 1600 DEG C~1900 DEG C, are burnt
The knot time is 5~50h.
Preferably, in step S6, the annealing region is at 1300~1600 DEG C, 5~20h of annealing time.
Further, in step S6, silicon carbide and aluminium oxide are respectively adopted in the polishing treatment as grinding and polishing
Material.
Further, in step S5, further HIP sintering is taken to handle on the ceramics after vacuum-sintering, heat etc. is quiet
1600~1700 DEG C of sintering temperature of pressure, sintering time are 2~10h, to improve the consistency of ceramics.
The present invention is based on improved, and 3D printing slurry direct write molding (DIW) technology with twin refuelling system realizes ceramic blank
The radial distribution of internal Doped ions concentration, the height for passing through Doped ions in conjunction with high-temperature vacuum and HIP sintering technique
Warm the continuously distributed crystalline ceramics of flooding mechanism preparation concentration gradient.
Compared to the steady temperature field distribution along single direction concentration gradient laser ceramics with obvious orientation, this hair
It is bright to be had using the crystalline ceramics with two-dimentional concentration gradient distribution characteristics radially as laser gain medium
Effect alleviates heat distribution and is orientated problem, realizes the thermo parameters method of space uniform, facilitates the stabilization of high-efficiency high power continuous laser
Output.
It is expected to alleviate in the case where pumping light action using composite transparent ceramic material prepared by the present invention as laser gain medium
The influence that material internal thermal lensing effect exports material laser.
Preparation method provided by the invention is easy to operate, and condition is controllable, easy to spread.
Detailed description of the invention
Fig. 1 is 3D printing DIW moulding process flow process figure of the invention；
Fig. 2 is the concentration distribution schematic diagram of Doped ions in crystalline ceramics before being sintered after 3D printing DIW is formed；
Fig. 3 is the concentration distribution schematic diagram of Doped ions in crystalline ceramics after being sintered；
Fig. 4 is the relative density variation tendency of ceramic body and sintered body in preparation process；
In figure, 1- liquid storage device A, 2- liquid storage device B, 3- Partial Pressure Controller, 4- gas cylinder A, 5- pressure valve A, 6- nozzle, 7- gas cylinder
B, 8- pressure valve B.
Specific embodiment
Invention is further described in detail in the following with reference to the drawings and specific embodiments.
As shown in Figure 1, the equipment of the invention based on direct write molding 3D printing technique includes 3D printing direct write rapid shaping
Liquid storage device A1, liquid storage device B2, Partial Pressure Controller 3, gas cylinder A4, gas cylinder B7, nozzle 6, pressure valve A5, the pressure valve B8 of machine, liquid storage
One end of device A1 and liquid storage device B2 are connected with Partial Pressure Controller 3 respectively, the other end of liquid storage device A1 and liquid storage device B2 respectively with
6 cavity of nozzle of direct write rapidform machine connects, and for gas cylinder A4 by pressure valve A5 connection Partial Pressure Controller 3, gas cylinder B7 passes through control
6 cavity of pressure valve B8 connection nozzle, 6 diameter dimension < 0.5 millimeter of nozzle.
Total gas pressure P, the P range of two liquid storage devices of input is adjusted in 10Pa~2 × 10 by pressure valve A56Pa, according to pottery
Depending on the viscosity of porcelain slurry is of different sizes, then pass through the air pressure P of the adjustment input of Partial Pressure Controller 3 liquid storage device A11It is stored up with input
The air pressure P of liquid device B22, P1、P2Scope control is 0~2 × 106Pa and meet P=P1+P2, input spray is adjusted by pressure valve B8
The intracorporal air pressure P ' of 6 chamber of mouth and P '≤P.
The raw material that ceramic slurry is prepared in following embodiment is the oxidate powder of purity>99.99%, partial size<5 micron
Body, and it is all based on direct write molding 3D printing equipment as shown in Figure 1.
The rodlike crystalline ceramics of embodiment 1:Yb:YAG concentration gradient
The stoichiometric ratio for being primarily based on YAG and Yb:YAG weighs material powder yttrium oxide, aluminium oxide, oxidation respectively
Ytterbium, then using deionized water as solvent, in 55vol%, addition glycerine is dispersing agent (2wt.%) for the solid content control of slurry,
Polyvinyl alcohol is binder (1.5wt.%), and polyethylene glycol is plasticiser (2wt.%), is prepared by long-time planetary type ball-milling
Obtain the preferable two kinds of ceramic slurries of rheological property.Then Yb:YAG, YAG slurry are respectively placed in liquid storage device A1 and liquid storage device B2
Interior, by accurately controlling feed rate, (constant the sum of Yb:YAG, YAG slurry feed rate is 100ml/min, wherein Yb:YAG
Slurry feed rate is gradually increased to 100ml/min by 0,0) YAG slurry feed rate is gradually decrease to and is beaten by 100ml/min
Print rate (50ml/min) prepares bar shaped ceramic base substrate, however successively improves the intensity of green body and low using isostatic cool pressing processing
Warm ungrease treatment excludes the intracorporal organic component of base, and isostatic cool pressing pressure limit is 100MPa, dwell time 2min, at degreasing
Managing temperature range is 700 DEG C, calcination time 5h.Ceramic body after degreasing, which is first placed in vacuum high temperature furnace, carries out long-time burning
Knot, vacuum ranges < 10-3Pa, 1700 DEG C of vacuum-sintering temperature, sintering time 15h, then again by the sintered body after vacuum-sintering
It is placed in hot isostatic pressing furnace and handles, 1600 DEG C of HIP sintering temperature, sintering time 2h.By sintered body through 1400 DEG C of oxygen
Anneal 5h under atmosphere, finally carries out precise polished processing as grinding and polishing material to get institute is arrived using silicon carbide and aluminium oxide
The concentration gradient crystalline ceramics of the radially continuous distribution needed.
Embodiment 2:Yb:Lu2O3Rodlike crystalline ceramics
It is primarily based on Lu2O3And Yb:Lu2O3Stoichiometric ratio weigh material powder luteium oxide, ytterbium oxide respectively, so
Afterwards using deionized water as solvent, in 50vol%, addition glycerine is dispersing agent (2wt.%), poly- second for the solid content control of slurry
Enol is binder (2wt.%), and polyethylene glycol is plasticiser (2wt.%), and stream is prepared by long-time planetary type ball-milling
Denaturation can preferable two kinds of ceramic slurries.Then by Yb:Lu2O3、Lu2O3Slurry is respectively placed in liquid storage device A1 and liquid storage device B2,
By accurately controlling feed rate (Yb:Lu2O3、Lu2O3Constant the sum of slurry feed rate is 300ml/min, wherein Yb:Lu2O3
Slurry feed rate is gradually increased to 300ml/min, Lu by 02O3Slurry feed rate by 300ml/min be gradually decrease to 0) and
Printing rate (250ml/min) prepare bar shaped ceramic base substrate, however successively use isostatic cool pressing processing raising green body intensity with
And low-temperature defatted processing excludes the intracorporal organic component of base, isostatic cool pressing pressure is 150MPa, dwell time 2min, at degreasing
Managing temperature is 700 DEG C, calcination time 20h.Ceramic body after degreasing, which is first placed in vacuum high temperature furnace, carries out long-time sintering,
Vacuum ranges < 10-3Pa, 1850 DEG C of sintering temperature, then the sintered body after vacuum-sintering is placed in heat etc. by sintering time 5h again
Processing in static pressure furnace, 1600 DEG C of HIP sintering temperature, sintering time 10h.By sintered body through under 1550 DEG C of oxygen atmospheres
Anneal 10h, is finally used as grinding and polishing material to carry out precise polished processing using silicon carbide and aluminium oxide required to get arriving
The concentration gradient crystalline ceramics of radially continuous distribution.
Embodiment 3:Er:Y2O3Rodlike crystalline ceramics
It is primarily based on Y2O3And Er:Y2O3Stoichiometric ratio weigh material powder yttrium oxide, erbium oxide respectively, then
Using deionized water as solvent, in 50vol%, addition glycerine is dispersing agent (2.5wt.%), poly- second for the solid content control of slurry
Enol is binder (2wt.%), and polyethylene glycol is plasticiser (2wt.%), and stream is prepared by long-time planetary type ball-milling
Denaturation can preferable two kinds of ceramic slurries.Then by Er:Y2O3、Y2O3Slurry is respectively placed in liquid storage device A1 and liquid storage device B2, is led to
Cross accurate control feed rate (Er:Y2O3、Y2O3Constant the sum of slurry feed rate is 500ml/min, wherein Er:Y2O3Slurry
Feed rate is gradually increased to 500ml/min, Y by 02O3Slurry feed rate is gradually decrease to 0) by 500ml/min and printing is fast
Rate (400ml/min) prepares bar shaped ceramic base substrate, however the intensity and low temperature of green body are successively improved using isostatic cool pressing processing
Ungrease treatment excludes the intracorporal organic component of base, and isostatic cool pressing pressure is 200MPa, dwell time 2min, ungrease treatment temperature
It is 750 DEG C, calcination time 10h.Ceramic body after degreasing, which is first placed in vacuum high temperature furnace, carries out long-time sintering, vacuum degree
Range < 10-3Pa, 1800 DEG C of sintering temperature, then the sintered body after vacuum-sintering is placed in hot isostatic pressing by sintering time 35h again
Processing in furnace, 1700 DEG C of HIP sintering temperature, sintering time 2h.By sintered body through annealing under 1500 DEG C of oxygen atmospheres
20h is finally used as grinding and polishing material to carry out precise polished processing required along diameter to get arriving using silicon carbide and aluminium oxide
To continuously distributed concentration gradient crystalline ceramics.
The rodlike crystalline ceramics of embodiment 4:Er:LuAG
The stoichiometric ratio for being primarily based on LuAG and Er:LuAG weighs material powder luteium oxide, aluminium oxide, oxidation respectively
Erbium, then using deionized water as solvent, in 50vol%, addition glycerine is dispersing agent (2wt.%) for the solid content control of slurry,
Polyvinyl alcohol is binder (1.5wt.%), and polyethylene glycol is plasticiser (2wt.%), is prepared by long-time planetary type ball-milling
Obtain the preferable two kinds of ceramic slurries of rheological property.Then Er:LuAG, LuAG slurry are respectively placed in liquid storage device A1 and liquid storage device
In B2, by accurately control feed rate (the sum of Er:LuAG, LuAG slurry feed rate is constant for 1000ml/min, wherein
Er:LuAG slurry feed rate is gradually increased to 1000ml/min by 0, and LuAG slurry feed rate is gradually subtracted by 1000ml/min
Bar shaped ceramic base substrate 0) as low as is prepared with printing rate (900ml/min), however green body is successively improved using isostatic cool pressing processing
Intensity and low-temperature defatted processing exclude the intracorporal organic component of base, isostatic cool pressing pressure is 200MPa, and the dwell time is
10min.Ungrease treatment temperature is 800 DEG C, calcination time 20h.Ceramic body after degreasing be first placed in vacuum high temperature furnace into
Row is sintered for a long time, vacuum ranges < 10-3Pa, 1600 DEG C of sintering temperature, sintering time 50h, then by the burning after vacuum-sintering
Knot body is placed in hot isostatic pressing furnace again and handles, and 1700 DEG C of HIP sintering temperature, sintering time 10h.Sintered body is passed through
Anneal 10h under 1350 DEG C of oxygen atmospheres, finally carries out precise polished place as grinding and polishing material using silicon carbide and aluminium oxide
It manages to get the concentration gradient crystalline ceramics of required radially continuous distribution is arrived.
Fig. 2 gives Re:Lu before high temperature sintering2O3Doped ions concentration distribution signal in ceramic body radially
Figure, it can be seen that doping replaces radial distribution with undoped green body, and adjacent doping is 0.2mm with undoped region overall width,
Wherein doped region width gradually broadens from center to edge and then becomes narrow gradually undoped with peak width.It is set with by green body
It is sintered for a long time in carrying out high temperature in vacuum drying oven and hot isostatic pressing furnace, adjacent two sides Doped ions are same under the driving of concentration gradient
When to undoped with region carry out thermal diffusion (diffusion length and concentration gradient and sintering schedule are closely related), to be formed along diameter
To direction Re3+The behavior of the slow gradual change of ion concentration, as shown in Figure 3.
Fig. 4 gives the variation tendency of each stage relative density of ceramic preparation process, it can be seen that composite ceramics
Consistency can achieve 90% or so after high-temperature vacuum is sintered, close further across can achieve after HIP sintering
100%.
Claims (10)
1. a kind of based on the direct write molding 3D printing technique method for preparing rodlike composite transparent ceramic, which is characterized in that including with
Lower step:
S1,3D printing rare earth doped ceramics slurry Re:M and the undoped ceramic slurry M of rare earth are prepared respectively；
S2, the liquid storage device A (1) and liquid storage that the two different slurries of Re:M, M are transferred to 3D printing direct write rapidform machine respectively
In device B (2), and one end of liquid storage device A (1) and liquid storage device B (2) is made to be connected respectively with Partial Pressure Controller (3), liquid storage device A (1)
It is connect respectively with the nozzle of direct write rapidform machine (6) cavity with the other end of liquid storage device B (2), gas cylinder A (4) passes through pressure valve A
(5) Partial Pressure Controller (3) are connected, gas cylinder B (7) connects nozzle (6) cavity by pressure valve B (8)；
S3, using the three-dimensional structure of computer-aided software engineering composite transparent ceramic, and write direct write printing shaping journey
Sequence adjusts total gas pressure P, the P range of two liquid storage devices of input in 10Pa~2 × 10 by pressure valve A (5)6Pa, according to ceramic slurry
Depending on the viscosity of material is of different sizes, then pass through the air pressure P of Partial Pressure Controller (3) adjustment input liquid storage device A (1)1It is stored up with input
The air pressure P of liquid device B (2)2, P1、P2Scope control is 0~2 × 106Pa and meet P=P1+P2, thus accurately control Re:M, M slurry
Material enters the rate of nozzle (6) cavity, and the sum of feed rate of two kinds of slurries range passes through pressure valve B in 0~1000ml/min
(8) the intracorporal air pressure P ' of adjustment input nozzle (6) chamber and P '≤P, the accurate printing rate for controlling direct write rapidform machine；Pass through
The mode being successively superimposed realizes the radially printing speed molding of two kinds of slurries of Re:M, M, obtains rod shaped ceramic idiosome；
S4, the ceramic idiosome of direct write printing shaping is first subjected to cold isostatic compaction under pressure, it then will be cold etc. quiet
Green body after molded, which is placed under oxygen atmosphere, carries out low-temperature defatted processing；
S5, the green body after degreasing is subjected to high-temperature vacuum sintering, obtains fine and close ceramic sintered bodies；
S6, sintered ceramic body successively carry out high annealing and precise polished processing under the conditions of oxygen-containing atmosphere.
2. a kind of side for preparing rodlike composite transparent ceramic based on direct write molding 3D printing technique according to claim 1
Method, which is characterized in that in step S1, ceramic slurry preparation process is: it by a certain proportion of material powder, solvent, dispersing agent, glues
It ties agent and plasticiser carries out ball milling mixing, the ceramic slurry of suitable solid content and viscosity is made, wherein the solvent is deionization
Water, solid content are 50vol%~55vol%, and the additional amount of the dispersing agent is 2wt.%, and the additional amount of the binder is
1.5wt.%, the additional amount of the plasticiser are 2wt.%.
3. a kind of side for preparing rodlike composite transparent ceramic based on direct write molding 3D printing technique according to claim 2
Method, which is characterized in that the dispersing agent is glycerine, and the binder is polyvinyl alcohol, and the plasticiser is polyethylene glycol.
4. a kind of direct write molding 3D printing technique that is based on according to any one of claims 1 to 3 prepares rodlike composite transparent
The method of ceramics, which is characterized in that in step S1, ceramic M is yttrium oxide, luteium oxide, scandium oxide, Y3Al5O12, Lu3Al5O12In
One kind, rare earth Re be neodymium, ytterbium, erbium, thulium, holmium, dysprosium, praseodymium, samarium, chromium, one of lanthanum.
5. a kind of direct write molding 3D printing technique that is based on according to any one of claims 1 to 3 prepares rodlike composite transparent
The method of ceramics, which is characterized in that in step S3, printing rate is 50~1000ml/min.
6. a kind of direct write molding 3D printing technique that is based on according to any one of claims 1 to 3 prepares rodlike composite transparent
The method of ceramics, which is characterized in that in step S4, the pressure limit of the isostatic cool pressing is in 100~200MPa, dwell time 2
~10min；700~800 DEG C of the ungrease treatment temperature range, 5~20h of calcination time.
7. a kind of direct write molding 3D printing technique that is based on according to any one of claims 1 to 3 prepares rodlike composite transparent
The method of ceramics, which is characterized in that in step S5, vacuum ranges < 10-3Pa, vacuum-sintering temperature range be 1700 DEG C~
1800 DEG C, sintering time is 10~50h.
8. a kind of direct write molding 3D printing technique that is based on according to any one of claims 1 to 3 prepares rodlike composite transparent
The method of ceramics, which is characterized in that in step S6, the annealing region is at 1400~1500 DEG C, 5~20h of annealing time.
9. a kind of direct write molding 3D printing technique that is based on according to any one of claims 1 to 3 prepares rodlike composite transparent
The method of ceramics, which is characterized in that in step S6, be respectively adopted in the polishing treatment silicon carbide and aluminium oxide as grinding and
Polishing material.
10. a kind of direct write molding 3D printing technique that is based on according to any one of claims 1 to 3 prepares rodlike composite transparent
The method of ceramics, which is characterized in that in step S5, further HIP sintering is taken to handle on the ceramics after vacuum-sintering,
1600~1700 DEG C of HIP sintering temperature, sintering time is 2~10h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910171710.3A CN109761608A (en) | 2019-03-07 | 2019-03-07 | A method of rodlike composite transparent ceramic is prepared based on direct write molding 3D printing technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910171710.3A CN109761608A (en) | 2019-03-07 | 2019-03-07 | A method of rodlike composite transparent ceramic is prepared based on direct write molding 3D printing technique |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109761608A true CN109761608A (en) | 2019-05-17 |
Family
ID=66457935
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910171710.3A Pending CN109761608A (en) | 2019-03-07 | 2019-03-07 | A method of rodlike composite transparent ceramic is prepared based on direct write molding 3D printing technique |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109761608A (en) |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111689764A (en) * | 2020-07-06 | 2020-09-22 | 南京理工大学 | Low-cost preparation of ceramic powder for selective laser melting and defocusing forming method thereof |
| CN111825453A (en) * | 2020-07-24 | 2020-10-27 | 江苏师范大学 | Preparation method of transparent ceramic optical fiber with core-spun structure |
| CN111848141A (en) * | 2020-07-24 | 2020-10-30 | 江苏师范大学 | Preparation method of ceramic paste for 3D printing by direct-writing forming of slurry |
| CN112500162A (en) * | 2020-12-24 | 2021-03-16 | 中红外激光研究院(江苏)有限公司 | YAG transparent ceramic and densification sintering method thereof |
| KR20210044435A (en) * | 2019-10-15 | 2021-04-23 | 한국세라믹기술원 | 3D printing structure with continuous composition gradient and fabricating method |
| CN113001706A (en) * | 2021-02-08 | 2021-06-22 | 刘宇涵 | Preparation method of multi-element ceramic functionally gradient material based on direct writing forming |
| CN113275590A (en) * | 2021-04-27 | 2021-08-20 | 江苏大学 | Method for preparing component with through cavity by direct-writing printing and pressure sintering |
| IT202000005998A1 (en) * | 2020-03-20 | 2021-09-20 | Consiglio Nazionale Ricerche | PROCESS BASED ON LITHOGRAPHY FOR THE PRODUCTION OF TRANSPARENT CERAMICS AND TRANSPARENT CERAMICS SO OBTAINED |
| CN113426464A (en) * | 2021-07-09 | 2021-09-24 | 浙江大学 | Ink direct-writing type 3D printing device of ceramic-based catalyst carrier and manufacturing method |
| CN113546614A (en) * | 2020-04-16 | 2021-10-26 | 中国石油天然气股份有限公司 | Catalyst alumina carrier material with gradient micro-morphology structure and preparation method thereof |
| CN113603474A (en) * | 2021-08-17 | 2021-11-05 | 南通大学 | Preparation method of transparent ceramic optical fiber with core-spun structure |
| CN113754411A (en) * | 2021-08-17 | 2021-12-07 | 南通大学 | Preparation method of 3D printing red overglaze Ce: YAG fluorescent ceramic |
| CN114853462A (en) * | 2022-05-16 | 2022-08-05 | 新沂市锡沂高新材料产业技术研究院有限公司 | Method for preparing YAG-based transparent ceramic by direct writing forming |
| CN116177995A (en) * | 2022-09-07 | 2023-05-30 | 中国科学院上海硅酸盐研究所 | Preparation method of fluorescent ceramic based on 3D printing composite structure |
| CN116178004A (en) * | 2022-12-13 | 2023-05-30 | 中国科学院上海硅酸盐研究所 | Rare earth gradual change doped transparent ceramic and preparation method thereof |
| CN116396070A (en) * | 2023-03-14 | 2023-07-07 | 中国科学院上海光学精密机械研究所 | Multi-material laser ceramic and preparation method of integrated 3D printing molding thereof |
| CN116425531A (en) * | 2023-03-14 | 2023-07-14 | 中国科学院上海光学精密机械研究所 | Infrared transparent ceramic ink and preparation and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101495294A (en) * | 2006-05-26 | 2009-07-29 | Z公司 | Apparatus and methods for handling materials in a 3-d printer |
| CN102066007A (en) * | 2008-12-11 | 2011-05-18 | 株式会社御牧工程 | Three-dimensional inkjet printer |
| CN104148629A (en) * | 2014-08-15 | 2014-11-19 | 江西悦安超细金属有限公司 | 3D printing rapid forming device and method based on metal carbonyl complex |
| CN106348745A (en) * | 2016-09-07 | 2017-01-25 | 济南大学 | Preparation method for rapidly forming YAG transparent ceramic powder material by 3DP (three-dimensional printing) technology |
| CN107056272A (en) * | 2017-04-24 | 2017-08-18 | 中国电子科技集团公司第十研究所 | The preparation method and slab laser ceramics of a kind of slab laser ceramics |
| CN107696233A (en) * | 2017-07-26 | 2018-02-16 | 航天特种材料及工艺技术研究所 | A kind of ceramic 3D printing equipment |
| CN107738334A (en) * | 2017-11-16 | 2018-02-27 | 同济大学 | One kind pottery mud 3 D-printing equipment |
| CN109016070A (en) * | 2018-09-29 | 2018-12-18 | 武汉理工大学 | Double spray head extruded type ceramics 3D printers and its Method of printing |
-
2019
- 2019-03-07 CN CN201910171710.3A patent/CN109761608A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101495294A (en) * | 2006-05-26 | 2009-07-29 | Z公司 | Apparatus and methods for handling materials in a 3-d printer |
| CN102066007A (en) * | 2008-12-11 | 2011-05-18 | 株式会社御牧工程 | Three-dimensional inkjet printer |
| CN104148629A (en) * | 2014-08-15 | 2014-11-19 | 江西悦安超细金属有限公司 | 3D printing rapid forming device and method based on metal carbonyl complex |
| CN106348745A (en) * | 2016-09-07 | 2017-01-25 | 济南大学 | Preparation method for rapidly forming YAG transparent ceramic powder material by 3DP (three-dimensional printing) technology |
| CN107056272A (en) * | 2017-04-24 | 2017-08-18 | 中国电子科技集团公司第十研究所 | The preparation method and slab laser ceramics of a kind of slab laser ceramics |
| CN107696233A (en) * | 2017-07-26 | 2018-02-16 | 航天特种材料及工艺技术研究所 | A kind of ceramic 3D printing equipment |
| CN107738334A (en) * | 2017-11-16 | 2018-02-27 | 同济大学 | One kind pottery mud 3 D-printing equipment |
| CN109016070A (en) * | 2018-09-29 | 2018-12-18 | 武汉理工大学 | Double spray head extruded type ceramics 3D printers and its Method of printing |
Non-Patent Citations (6)
| Title |
|---|
| 徐军主编: "《激光材料科学与技术前沿》", 30 April 2007, 上海：上海交通大学出版社 * |
| 徐巍主编: "《快速成型技术之熔融沉积成型技术实践教程》", 31 December 2015, 上海：上海交通大学出版社 * |
| 李亚运等: ""陶瓷3D 打印技术的研究与进展"，", 《硅酸盐学报》 * |
| 王晓敏等: "《工程材料学 第4版》", 31 July 2017, 哈尔滨：哈尔滨工业大学出版社 * |
| 纪宏超等: "陶瓷３Ｄ打印技术及材料研究进展"", 《材料工程》 * |
| 谭建荣等: "《中国好设计 制造装备创新设计案例研究》", 30 September 2016, 北京：科学普及出版社 * |
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20210044435A (en) * | 2019-10-15 | 2021-04-23 | 한국세라믹기술원 | 3D printing structure with continuous composition gradient and fabricating method |
| KR102308341B1 (en) | 2019-10-15 | 2021-10-06 | 한국세라믹기술원 | 3D printing structure with continuous composition gradient and fabricating method |
| WO2021186076A1 (en) | 2020-03-20 | 2021-09-23 | Consiglio Nazionale Delle Ricerche | Lithography-based process for the production of transparent ceramic bodies with at least two zones of different composition and transparent ceramic bodies thus obtained |
| IT202000005998A1 (en) * | 2020-03-20 | 2021-09-20 | Consiglio Nazionale Ricerche | PROCESS BASED ON LITHOGRAPHY FOR THE PRODUCTION OF TRANSPARENT CERAMICS AND TRANSPARENT CERAMICS SO OBTAINED |
| CN115335221A (en) * | 2020-03-20 | 2022-11-11 | 意大利国家研究委员会 | Lithography-based method for producing a transparent ceramic body having at least two regions of different composition and transparent ceramic body obtained thereby |
| CN115335221B (en) * | 2020-03-20 | 2024-04-02 | 意大利国家研究委员会 | Method based on lithography for producing transparent ceramic bodies having at least two different composition areas and transparent ceramic bodies obtained thereby |
| CN113546614B (en) * | 2020-04-16 | 2023-10-27 | 中国石油天然气股份有限公司 | Catalyst alumina carrier material with gradient microstructure and preparation method thereof |
| CN113546614A (en) * | 2020-04-16 | 2021-10-26 | 中国石油天然气股份有限公司 | Catalyst alumina carrier material with gradient micro-morphology structure and preparation method thereof |
| CN111689764B (en) * | 2020-07-06 | 2022-05-31 | 南京理工大学 | Low-cost preparation of ceramic powder for selective laser melting and defocusing forming method thereof |
| CN111689764A (en) * | 2020-07-06 | 2020-09-22 | 南京理工大学 | Low-cost preparation of ceramic powder for selective laser melting and defocusing forming method thereof |
| CN111848141A (en) * | 2020-07-24 | 2020-10-30 | 江苏师范大学 | Preparation method of ceramic paste for 3D printing by direct-writing forming of slurry |
| CN111825453A (en) * | 2020-07-24 | 2020-10-27 | 江苏师范大学 | Preparation method of transparent ceramic optical fiber with core-spun structure |
| CN112500162A (en) * | 2020-12-24 | 2021-03-16 | 中红外激光研究院(江苏)有限公司 | YAG transparent ceramic and densification sintering method thereof |
| CN113001706A (en) * | 2021-02-08 | 2021-06-22 | 刘宇涵 | Preparation method of multi-element ceramic functionally gradient material based on direct writing forming |
| CN113275590A (en) * | 2021-04-27 | 2021-08-20 | 江苏大学 | Method for preparing component with through cavity by direct-writing printing and pressure sintering |
| CN113426464A (en) * | 2021-07-09 | 2021-09-24 | 浙江大学 | Ink direct-writing type 3D printing device of ceramic-based catalyst carrier and manufacturing method |
| CN113603474A (en) * | 2021-08-17 | 2021-11-05 | 南通大学 | Preparation method of transparent ceramic optical fiber with core-spun structure |
| CN113754411A (en) * | 2021-08-17 | 2021-12-07 | 南通大学 | Preparation method of 3D printing red overglaze Ce: YAG fluorescent ceramic |
| CN114853462A (en) * | 2022-05-16 | 2022-08-05 | 新沂市锡沂高新材料产业技术研究院有限公司 | Method for preparing YAG-based transparent ceramic by direct writing forming |
| CN116177995A (en) * | 2022-09-07 | 2023-05-30 | 中国科学院上海硅酸盐研究所 | Preparation method of fluorescent ceramic based on 3D printing composite structure |
| CN116177995B (en) * | 2022-09-07 | 2024-03-12 | 中国科学院上海硅酸盐研究所 | Preparation method of fluorescent ceramic based on 3D printing composite structure |
| CN116178004A (en) * | 2022-12-13 | 2023-05-30 | 中国科学院上海硅酸盐研究所 | Rare earth gradual change doped transparent ceramic and preparation method thereof |
| CN116396070A (en) * | 2023-03-14 | 2023-07-07 | 中国科学院上海光学精密机械研究所 | Multi-material laser ceramic and preparation method of integrated 3D printing molding thereof |
| CN116425531A (en) * | 2023-03-14 | 2023-07-14 | 中国科学院上海光学精密机械研究所 | Infrared transparent ceramic ink and preparation and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109761608A (en) | A method of rodlike composite transparent ceramic is prepared based on direct write molding 3D printing technique | |
| CN102060539B (en) | Method for preparing yttrium aluminum garnet based transparent ceramic by slip casting | |
| CN111825453A (en) | Preparation method of transparent ceramic optical fiber with core-spun structure | |
| Guo et al. | Fabrication and laser behaviors of Nd: YAG ceramic microchips | |
| Liu et al. | 2.44 KW laser output of Nd: YAG ceramic slab fabricated by a solid-state reactive sintering | |
| An et al. | Two-step pressure sintering of transparent lutetium oxide by spark plasma sintering | |
| CN106673627A (en) | Method for preparing toughened aluminum oxide ceramic based on stereo lithography appearance namely 3D printing | |
| CN101698601B (en) | Sintering method of yttrium oxide base transparent ceramic | |
| Liu et al. | Effects of ball milling time on microstructure evolution and optical transparency of Nd: YAG ceramics | |
| Liu et al. | Sintering and laser behavior of composite YAG/Nd: YAG/YAG transparent ceramics | |
| Ba et al. | Transparent Y3Al5O12 ceramics produced by an aqueous tape casting method | |
| CN114773048B (en) | Preparation method and application of composite ceramic material | |
| CN110028324A (en) | A kind of preparation method of nitride ceramics | |
| Ge et al. | Nd: YAG transparent ceramics fabricated by direct cold isostatic pressing and vacuum sintering | |
| Zhang et al. | Alumina assisted grain refinement and physical performance enhancement of yttria transparent ceramics by two-step sintering | |
| CN109081700A (en) | A kind of method that nothing presses electro-plasma sintering ceramics | |
| Zhang et al. | Three-dimensional printing of transparent ceramics by lithography-based digital projection | |
| CN113773081A (en) | Transparent ceramic and preparation method thereof | |
| Chen et al. | Fabrication of YAG transparent ceramics by two-step sintering | |
| Chen et al. | Densification, microstructure and optical properties of YAG transparent ceramics prepared by dry-pressing and gelcasting | |
| Guo et al. | Effects of composition and sintering temperature on the structure and compressive property of the lamellar Al 2 O 3–ZrO 2 scaffolds prepared by freeze casting | |
| CN107324805A (en) | A kind of multicomponent garnet-base laser transparent ceramic material and preparation method thereof | |
| Jing et al. | Preparation of a Φ60 mm Nd: YAG transparent ceramic disk | |
| CN114853462A (en) | Method for preparing YAG-based transparent ceramic by direct writing forming | |
| CN106587940A (en) | High-purity compact magnesium oxide target material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |