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CN109761608A - A method for preparing rod-shaped composite transparent ceramics based on direct writing 3D printing technology - Google Patents

A method for preparing rod-shaped composite transparent ceramics based on direct writing 3D printing technology Download PDF

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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
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printing
ceramic
composite transparent
direct
shaped composite
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唐飞
唐定远
王俊
刘鹏
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Jiangsu Normal University
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Jiangsu Normal University
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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

A method of rodlike composite transparent ceramic is prepared based on direct write molding 3D printing technique
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)

1.一种基于直写成型3D打印技术制备棒状复合透明陶瓷的方法，其特征在于，包括以下步骤：1. a method for preparing rod-shaped composite transparent ceramics based on direct writing molding 3D printing technology, is characterized in that, comprises the following steps: S1、分别制备3D打印用稀土掺杂陶瓷浆料Re:M与稀土未掺杂的陶瓷浆料M；S1, respectively preparing rare earth doped ceramic slurry Re:M for 3D printing and rare earth undoped ceramic slurry M; S2、将Re:M、M两种不同的浆料分别转移至3D打印直写快速成型机的储液器A(1)和储液器B(2)中，并使储液器A(1)和储液器B(2)的一端分别与分压控制器(3)相连接，储液器A(1)和储液器B(2)的另一端分别与直写快速成型机的喷嘴(6)腔体连接，气瓶A(4)通过控压阀A(5)连接分压控制器(3)，气瓶B(7)通过控压阀B(8)连接喷嘴(6)腔体；S2. Transfer the two different slurries of Re:M and M to the liquid storage tank A (1) and liquid storage tank B (2) of the 3D printing direct writing rapid prototyping machine respectively, and make the liquid storage tank A (1). ) and one end of the accumulator B (2) are respectively connected with the partial pressure controller (3), and the other ends of the accumulator A (1) and the accumulator B (2) are respectively connected with the nozzle of the direct writing rapid prototyping machine (6) The cavity is connected, the gas cylinder A (4) is connected to the partial pressure controller (3) through the pressure control valve A (5), and the gas cylinder B (7) is connected to the nozzle (6) cavity through the pressure control valve B (8). body; S3、采用计算机辅助软件设计复合透明陶瓷的三维立体结构，并编写直写打印成型程序，通过控压阀A(5)调整输入两个储液器的总气压P，P范围在10Pa～2×106Pa，依据陶瓷浆料的粘度大小不同而定，然后通过分压控制器(3)调整输入储液器A(1)的气压P1和输入储液器B(2)的气压P2，P1、P2范围控制在0～2×106Pa且满足P＝P1+P2，从而精确控制Re:M、M浆料进入喷嘴(6)腔体的速率，两种浆料的进料速率之和范围在0～1000ml/min，通过控压阀B(8)调整输入喷嘴(6)腔体内的气压P’且P’≤P，精确控制直写快速成型机的打印速率；通过逐层叠加的方式，实现Re:M、M两种浆料的沿径向方向快速打印成型，获得棒状陶瓷胚体；S3. Use computer-aided software to design the three-dimensional structure of the composite transparent ceramic, and write a direct-writing printing molding program, and adjust the total air pressure P input to the two liquid reservoirs through the pressure control valve A (5), and the range of P is 10Pa ~ 2× 10 6 Pa, depending on the viscosity of the ceramic slurry, and then adjust the air pressure P 1 input to the accumulator A (1) and the air pressure P 2 input to the accumulator B (2) through the partial pressure controller (3). , P 1 and P 2 are controlled in the range of 0～2×10 6 Pa and satisfy P=P 1 +P 2 , so as to precisely control the speed of Re:M and M slurries entering the cavity of the nozzle (6), the two slurries The sum of the feed rates ranges from 0 to 1000ml/min. Adjust the air pressure P' in the cavity of the input nozzle (6) through the pressure control valve B (8) and P'≤P to precisely control the printing rate of the direct-writing rapid prototyping machine. ; Through the layer-by-layer superposition, the rapid printing and forming of Re:M and M slurry in the radial direction is realized, and the rod-shaped ceramic embryo body is obtained; S4、将直写打印成型的陶瓷胚体先在一定的压力下进行冷等静压成型，然后将冷等静压成型后的坯体置于氧气气氛下进行低温脱脂处理；S4. The ceramic body formed by direct writing printing is first subjected to cold isostatic pressing under a certain pressure, and then the cold isostatic pressing body is placed in an oxygen atmosphere for low-temperature degreasing treatment; S5、将脱脂后的坯体进行高温真空烧结，获得致密的陶瓷烧结体；S5. Perform high temperature vacuum sintering on the degreasing body to obtain a dense ceramic sintered body; S6、烧结后的陶瓷体依次进行含氧气氛条件下高温退火以及精密抛光处理。S6. The sintered ceramic body is sequentially subjected to high temperature annealing and precision polishing under the condition of oxygen-containing atmosphere. 2.根据权利要求1所述的一种基于直写成型3D打印技术制备棒状复合透明陶瓷的方法，其特征在于，步骤S1中，陶瓷浆料制备过程是：将一定比例的原料粉体、溶剂、分散剂、粘结剂和塑化剂进行球磨混合，制得合适固含量和粘度的陶瓷浆料，其中，所述溶剂为去离子水，固含量为50vol％～55vol％，所述分散剂的加入量为2wt.％，所述粘结剂的加入量为1.5wt.％，所述塑化剂的加入量为2wt.％。2. A method for preparing rod-shaped composite transparent ceramics based on direct writing 3D printing technology according to claim 1, wherein in step S1, the ceramic slurry preparation process is: a certain proportion of raw material powder, solvent , dispersant, binder and plasticizer are ball-milled and mixed to obtain ceramic slurry with suitable solid content and viscosity, wherein the solvent is deionized water, and the solid content is 50vol% to 55vol%. The addition amount of the binder is 2 wt. %, the addition amount of the binder is 1.5 wt. %, and the addition amount of the plasticizer is 2 wt. %. 3.根据权利要求2所述的一种基于直写成型3D打印技术制备棒状复合透明陶瓷的方法，其特征在于，所述分散剂为丙三醇，所述粘结剂为聚乙烯醇，所述塑化剂为聚乙二醇。3. A method for preparing rod-shaped composite transparent ceramics based on direct writing 3D printing technology according to claim 2, wherein the dispersant is glycerol, the binder is polyvinyl alcohol, and the The plasticizer is polyethylene glycol. 4.根据权利要求1至3任一项所述的一种基于直写成型3D打印技术制备棒状复合透明陶瓷的方法，其特征在于，步骤S1中，陶瓷M为氧化钇，氧化镥，氧化钪，Y3Al5O12，Lu3Al5O12中的一种，稀土Re为钕，镱，铒，铥，钬，镝，镨，钐，铬，镧中的一种。4. A method for preparing rod-shaped composite transparent ceramics based on direct-write molding 3D printing technology according to any one of claims 1 to 3, wherein in step S1, the ceramic M is yttrium oxide, lutetium oxide, scandium oxide , Y 3 Al 5 O 12 , one of Lu 3 Al 5 O 12 , the rare earth Re is one of neodymium, ytterbium, erbium, thulium, holmium, dysprosium, praseodymium, samarium, chromium, and lanthanum. 5.根据权利要求1至3任一项所述的一种基于直写成型3D打印技术制备棒状复合透明陶瓷的方法，其特征在于，步骤S3中，打印速率为50～1000ml/min。5 . The method for preparing rod-shaped composite transparent ceramics based on direct writing 3D printing technology according to claim 1 , wherein in step S3 , the printing rate is 50-1000 ml/min. 6 . 6.根据权利要求1至3任一项所述的一种基于直写成型3D打印技术制备棒状复合透明陶瓷的方法，其特征在于，步骤S4中，所述冷等静压的压力范围在100～200MPa，保压时间2～10min；所述脱脂处理温度范围700～800℃，煅烧时间5～20h。6. The method for preparing rod-shaped composite transparent ceramics based on direct-writing 3D printing technology according to any one of claims 1 to 3, wherein in step S4, the pressure range of the cold isostatic pressing is 100 ～200MPa, pressure holding time 2～10min; the temperature range of the degreasing treatment is 700～800℃, and the calcination time is 5～20h. 7.根据权利要求1至3任一项所述的一种基于直写成型3D打印技术制备棒状复合透明陶瓷的方法，其特征在于，步骤S5中，真空度范围<10-3Pa，真空烧结温度范围为1700℃～1800℃，烧结时间为10～50h。7. A method for preparing rod-shaped composite transparent ceramics based on direct-write molding 3D printing technology according to any one of claims 1 to 3, characterized in that, in step S5, the vacuum degree range is less than 10 -3 Pa, and vacuum sintering The temperature range is 1700℃～1800℃, and the sintering time is 10～50h. 8.根据权利要求1至3任一项所述的一种基于直写成型3D打印技术制备棒状复合透明陶瓷的方法，其特征在于，步骤S6中，所述退火温度范围在1400～1500℃，退火时间5～20h。8 . The method for preparing rod-shaped composite transparent ceramics based on direct writing 3D printing technology according to any one of claims 1 to 3, wherein in step S6, the annealing temperature ranges from 1400 to 1500°C, Annealing time 5 ~ 20h. 9.根据权利要求1至3任一项所述的一种基于直写成型3D打印技术制备棒状复合透明陶瓷的方法，其特征在于，步骤S6中，所述抛光处理中分别采用碳化硅和氧化铝作为研磨和抛光料。9 . The method for preparing rod-shaped composite transparent ceramics based on direct writing 3D printing technology according to any one of claims 1 to 3, characterized in that, in step S6, silicon carbide and oxide are respectively used in the polishing treatment. Aluminium as grinding and polishing compound. 10.根据权利要求1至3任一项所述的一种基于直写成型3D打印技术制备棒状复合透明陶瓷的方法，其特征在于，步骤S5中，将真空烧结后的陶瓷进一步采取热等静压烧结处理，热等静压烧结温度1600～1700℃，烧结时间为2～10h。10. The method for preparing rod-shaped composite transparent ceramics based on direct-write molding 3D printing technology according to any one of claims 1 to 3, wherein in step S5, the vacuum sintered ceramics are further subjected to thermal isostatic Press sintering treatment, hot isostatic pressing sintering temperature 1600 ~ 1700 ℃, sintering time 2 ~ 10h.
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