CN113213931B - 一种基于Isobam凝胶与熔融纺丝技术的透明陶瓷光纤制备方法 - Google Patents

一种基于Isobam凝胶与熔融纺丝技术的透明陶瓷光纤制备方法 Download PDF

Info

Publication number
CN113213931B
CN113213931B CN202110498840.5A CN202110498840A CN113213931B CN 113213931 B CN113213931 B CN 113213931B CN 202110498840 A CN202110498840 A CN 202110498840A CN 113213931 B CN113213931 B CN 113213931B
Authority
CN
China
Prior art keywords
optical fiber
transparent ceramic
ceramic optical
slurry
preparation
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.)
Active
Application number
CN202110498840.5A
Other languages
English (en)
Other versions
CN113213931A (zh
Inventor
田俊杰
姚庆
刘红梅
孙洪浩
郭容
王东
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nantong University
Original Assignee
Nantong University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nantong University filed Critical Nantong University
Priority to CN202110498840.5A priority Critical patent/CN113213931B/zh
Publication of CN113213931A publication Critical patent/CN113213931A/zh
Application granted granted Critical
Publication of CN113213931B publication Critical patent/CN113213931B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/08—Apparatus or processes for treating or working the shaped or preshaped articles for reshaping the surface, e.g. smoothing, roughening, corrugating, making screw-threads
    • B28B11/0845—Apparatus or processes for treating or working the shaped or preshaped articles for reshaping the surface, e.g. smoothing, roughening, corrugating, making screw-threads for smoothing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
    • B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B17/00—Details of, or accessories for, apparatus for shaping the material; Auxiliary measures taken in connection with such shaping
    • B28B17/02—Conditioning the material prior to shaping
    • B28B17/026—Conditioning ceramic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
    • B28B3/003—Pressing by means acting upon the material via flexible mould wall parts, e.g. by means of inflatable cores, isostatic presses
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/638—Removal thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/606—Drying
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6565—Cooling rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646—Optical properties
    • C04B2235/9653—Translucent or transparent ceramics other than alumina

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)
  • Lasers (AREA)

Abstract

本发明公开了一种基于Isobam凝胶与熔融纺丝技术的Nd：YAG激光透明陶瓷光纤制备方法，本发明属于激光透明陶瓷技术领域。该制备方法首先利用Isobam凝胶成型技术制备Nd：YAG透明陶瓷光纤浆料，其次加入高分子化合物颗粒加强其韧性，得到透明陶瓷光纤前驱体，然后通过纺丝机得到透明陶瓷光纤素坯，最后通过温等静压和真空烧结实现透明陶瓷光纤的制备。本发明的制备方法不仅具有无模具、可操作性强、易大规模生产等商业特点，而且具有可控制光纤直径，制备过程柔性高等工艺优点，制成的透明陶瓷光纤具有高韧性、高固含量，高强度的特点。

Description

一种基于Isobam凝胶与熔融纺丝技术的透明陶瓷光纤制备 方法
技术领域
本发明属于激光透明陶瓷技术领域，具体涉及一种基于Isobam凝胶与熔融纺丝技术的Nd：YAG激光透明陶瓷光纤制备方法。
背景技术
以光纤材料为增益介质的光纤激光器得益于它易于得到理性的激光光束质量、超高的转换效率以免维护、高稳定性、体积小、便于材料内部热管理等特点，在近年来发展十分迅猛，并且迅速在高功率切割和焊接等市场占据了一席之地。从单根光纤最初输出只有百瓦级到目前达到的千瓦级，国内的光纤激光器的研究取得了长足的进步和发展，与国外距离正在缩短。
传统的光纤激光器大都使用掺杂了稀土离子的玻璃光纤作为增益介质，然而石英玻璃的热导率较低(1.38W/(m·K))、机械性能差、弯曲半径不能过小等缺点，导致传统光纤激光器在长时间工作时易出现热梯度变大、光学畸变、输出功率受限、机械破坏以及热透镜效应造成的光束质量下降等问题。透明陶瓷具有陶瓷优良的机械与力学性能，也同样具有优良的光学性能，其高晶体场有利于稀土离子与过渡金属离子的电子辐射跃迁。自1995年日本Akio Ikesue博士制备世界上首块激光透明陶瓷以来，人们发现陶瓷材料的热导率高达11 W/(m·K)，具有更好的热管理能力可以承受更高的功率，因此相对于玻璃光纤，陶瓷热学性能好非常有利于应用推广。
目前已经报道的YAG基透明陶瓷光纤，如专利CN 110885244 B与CN 111270347 A都是将陶瓷浆料吸入毛细玻璃管中，不仅无法得到细长的陶瓷光纤，而且难以大批量大规模生产；专利CN 104451953 A中公开了一种采用注浆成型制备镥铝石榴石透明陶瓷光纤的方法，将浆料注入自制石膏模具中制备光纤素坯，注浆成型制备的陶瓷素坯强度低，在极细的光纤素坯上将会体现更加明显，容易断裂，同时，由于浆料表面张力的存在，浆料在注入小孔径石膏模具时比较困难，甚至可能在素坯中形成孔洞；专利CN 111620566 A中公开了一种多相透明陶瓷光纤的方法，先制得前驱体玻璃作为纤芯玻璃，再采用现有的玻璃光纤拉制技术制备得到透明陶瓷光纤，但此专利需要两种晶相一起析出才可以得到透明陶瓷光纤，并且对氟化物相的含量要求极高，很容易造成不透明的现象。
发明内容
本发明的目的是提供一种基于Isobam凝胶与熔融纺丝技术的Nd：YAG激光透明陶瓷光纤，通过采用Isobam凝胶成型技术与现代化纺丝技术制备Nd：YAG激光透明陶瓷光纤，工艺简单、高效，并且得到的透明陶瓷光纤具有良好的韧性与光学性能。
为了实现上述发明目的，本发明采用以下技术方案：
一种基于Isobam凝胶与熔融纺丝技术的Nd：YAG透明陶瓷光纤的制备方法，首先利用Isobam凝胶成型技术制备Nd：YAG透明陶瓷光纤浆料，其次加入高分子化合物颗粒加强其韧性，得到透明陶瓷光纤前驱体，然后通过纺丝机得到透明陶瓷光纤素坯，最后通过温等静压和真空烧结实现透明陶瓷光纤的制备。具体包括如下步骤：
Step1、按照Nd: YAG透明陶瓷材料 (Y1-xNdx)3A15O12，0.01≤x≤0.04的化学计量比分别称量原料粉体，进行除杂处理；
Step2、将原料粉体、烧结助剂、Al2O3磨球、无水乙醇混合，球磨24~36 h，得到混合浆料；
Step3、将混合浆料烘干，过筛后置于马弗炉中煅烧，冷却后得到原料粉；
Step4、采用PIBM凝胶注模体系，使用上述原料粉配制陶瓷浆料；
Step5、在上述浆料中加入高分子化合物颗粒，得到透明陶瓷光纤前驱体；
Step6、将上述前驱体加入熔融纺丝机中纺丝成型，得到透明陶瓷光纤素坯；
Step7、将透明陶瓷光纤素坯进行温等静压、干燥、排胶、真空烧结、抛光处理，即可得到透明陶瓷光纤。
进一步地，Step1中，所述原料粉体为氧化钕Nd2O3、氧化铝Al2O3和氧化钇Y2O3；除杂处理采用煅烧方法。
进一步地，Step2中，所述烧结助剂为MgO和SiO2的混合物。
进一步地，Step2中，烧结助剂、Al2O3磨球、无水乙醇和原料粉体的用量比为1：600：240：200。
进一步地，Step3中，烘干采用40～100 ℃恒温烘箱，浆料蒸发时间为24～48 h；煅烧温度为800～1000 ℃，保温8～24 h。
进一步地，Step4中，所述PIBM凝胶注模体系使用Isobam104#作为凝胶剂；陶瓷浆料的固含量为45 vol.%~ 50 vol.%。
进一步地，Step5中，所述高分子化合物颗粒为聚己内酯（PCL）、聚乳酸（PLA）或聚氨酯（TPU）。
进一步地，Step5中，高分子化合物颗粒的用量为浆料的0.1 wt.%~ 0.5 wt.%。
进一步地，Step6中，熔融纺丝机的熔融温度为90~120 ℃，压力为100~120 MPa，纺丝速度为0.1~0.5 m/s。
进一步地，Step7中，所述温等静压的条件为100～200 MPa下5～20 min；所述干燥工艺是在100～120 ℃的烘箱中干燥4～8 h；所述排胶是室温～450 ℃升温速度为0.5～2℃/min，450～800 ℃升温速度为0.5～3 ℃/min，在800 ℃保温2～6 h；所述真空烧结工艺为：室温下先按5～10 ℃/min升温到200 ℃，保温10～30 min，再按10～20 ℃/min升温到1000 ℃并保温10～30 min，然后按1～5 ℃/min升温到1650 ℃并保温6～10 h，最后以5～10 ℃/min降温到室温，烧结过程中真空度保持在1×10-2～1×10-5 Pa。
与现有技术相比，本发明具有如下的有益效果：
1. 本发明提供的一种基于Isobam凝胶与熔融纺丝技术的Nd：YAG透明陶瓷光纤制备方法，采用Isobam凝胶成型的方法，使制成的透明陶瓷光纤具有高韧性、高固含量、高强度的特点。
2. 本发明提供的一种基于Isobam凝胶与熔融纺丝技术的Nd：YAG透明陶瓷光纤制备方法，利用纺丝机的纺丝技术来制备透明陶瓷光纤，不仅具有无模具、可操作性强、易大规模生产等商业特点，而且具有可控制光纤直径，制备过程柔性高等工艺优点。
附图说明
图1为实施例1样品熔融纺丝机制备素坯图，其中(b)为(a)中截取的陶瓷光纤，所截取的光纤长度为30 cm，直径为500 μm。
图2为实施例1样品的制备现场图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清晰，结合具体实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，但不应以此限制本发明的保护范围。
实施例1
一种基于Isobam凝胶与熔融纺丝技术的Nd：YAG激光透明陶瓷光纤制备方法，包括以下步骤：
Step1、按照1% Nd: YAG的化学计量比分别称量高纯纳米Y2O3粉体（纯度>99.99%）33.799 g、高纯纳米Al2O3粉体（纯度>99.99%）25.692 g，高纯Nd2O3粉体（纯度>99.99%）0.509 g，除杂预处理。
Step2、使用烧结助剂SiO2为0.2 g和MgO为0.1 g、高纯Al2O3磨球180 g、无水乙醇72 ml、充分搅拌后放入球磨罐中，混合球磨24 h均匀后得到混合浆料。
Step3、将混合浆料置于40 ℃恒温烘箱烘48 h后过筛，将过筛后的粉体置于马弗炉中煅烧，从室温升温到1000 ℃，保温8 h后自然冷却，作为凝胶注模成型的原料粉。
Step4、采用PIBM凝胶注模体系，在30 g的去离子水中，加入Isobam104# 0.3 g，用四甲基氢氧化铵调节pH到11，采用柠檬酸铵分散剂0.24 g，并加入原料粉60 g后充分球磨，制备固含量为45 vol.%的陶瓷浆料，再用真空除泡机进行除泡处理，得到透明陶瓷光纤浆料。
Step5、将上述透明陶瓷光纤浆料加入0.1wt.%的聚己内酯（PCL）后放入搅拌机内搅拌30 min，得到透明陶瓷光纤前驱体。
Step6、将上述前驱体放入纺丝机内，以100 MPa的压力与0.1 m/s速度进行纺丝，得到透明陶瓷光纤素坯。
Step7、所述透明陶瓷光纤素坯素坯进行温等静压处理在温度40 ℃，200 MPa压力下温等5 min。然后进行干燥处理：放入100 ℃烘箱中保温8 h。干燥后进行排胶处理，从室温开始以2 ℃/min升温速度到450 ℃，再以3 ℃/min升温速度到800 ℃，并保温2 h。最后真空烧结，室温开始以10 ℃/min升温到200 ℃，保温10 min，再次按10 ℃/min升温到1000℃并保温10 min，然后按5 ℃/min升温到1650 ℃并保温6 h，最后以5 ℃/min降温到室温，整个烧结过程中真空度保持在1×10-2 Pa。再经过抛光处理，得到1%Nd: YAG透明陶瓷光纤。
实施例2
一种基于Isobam凝胶与熔融纺丝技术的Nd：YAG激光透明陶瓷光纤制备方法，它包括以下步骤：
Step1、按照4% Nd: YAG的化学计量比分别称量高纯纳米Y2O3粉体（纯度>99.99%）32.503g、高纯纳米Al2O3粉体（纯度>99.99%）25.479 g，高纯Nd2O3粉体（纯度>99.99%）2.018g，除杂预处理。
Step2、使用烧结助剂SiO2为0.25 g和MgO为0.05 g、高纯Al2O3磨球180 g、无水乙醇72 ml、充分搅拌后放入球磨罐中，混合球磨36 h均匀后得到混合浆料。
Step3、将混合浆料置于100 ℃恒温烘箱烘24 h后过筛，将过筛后的粉体置于马弗炉中煅烧，从室温升温到800 ℃，保温24 h后自然冷却，作为凝胶注模成型的原料粉。
Step4、采用PIBM凝胶注模体系，在23 g的去离子水中，加入Isobam104# 0.3 g，用四甲基氢氧化铵调节pH到11，采用柠檬酸铵分散剂0.3 g，并加入原料粉60 g后充分球磨，制备固含量为50 vol.%的陶瓷浆料，再用真空除泡机进行除泡处理，得到透明陶瓷光纤浆料。
Step5、将上述透明陶瓷光纤浆料加入0.5 wt.%聚乳酸（PLA）后放入搅拌机内搅拌60min，得到透明陶瓷光纤前驱体。
Step6、将上述前驱体放入纺丝机内，以100 MPa的压力与0.1 m/s速度进行纺丝，得到透明陶瓷光纤素坯。
Step7、所述透明陶瓷光纤素坯素坯进行温等静压处理在温度80 ℃，100 MPa压力下温等20 min。然后进行干燥处理：放入120 ℃烘箱中保温4 h。干燥后进行排胶处理，从室温开始以0.5 ℃/min升温速度到450 ℃，再以0.5 ℃/min升温速度到800 ℃，并保温6 h。最后真空烧结，室温开始以5 ℃/min升温到200 ℃，保温30 min，再次按20 ℃/min升温到1000 ℃并保温30 min，然后按1 ℃/min升温到1650 ℃并保温10 h，最后以10 ℃/min降温到室温，整个烧结过程中真空度保持在1×10-5 Pa。再经过抛光处理，得到4%Nd: YAG激光透明陶瓷光纤。
实施例3
一种基于Isobam凝胶与熔融纺丝技术的Nd：YAG激光透明陶瓷光纤制备方法，它包括以下步骤：
Step1、按照2% Nd: YAG的化学计量比分别称量高纯纳米Y2O3粉体（纯度>99.99%）33.364g、高纯纳米Al2O3粉体（纯度>99.99%）25.621 g，高纯高纯Nd2O3（纯度>99.99%）1.015g，除杂预处理。
Step2、使用烧结助剂SiO2为0.2 g和MgO为0.1g、高纯Al2O3磨球180 g、无水乙醇72ml、充分搅拌后放入球磨罐中，混合球磨30 h均匀后得到混合浆料。
Step3、将混合浆料置于60 ℃恒温烘箱烘36 h后过筛，将过筛后的粉体置于马弗炉中煅烧，从室温升温到900 ℃，保温12 h后自然冷却，作为凝胶注模成型的原料粉。
Step4、采用PIBM凝胶注模体系，在25 g的去离子水中，加入Isobam104# 0.3 g，用四甲基氢氧化铵调节pH到12，采用柠檬酸铵分散剂0.24 g，并加入原料粉60 g后充分球磨，制备固含量为48 vol.%的陶瓷浆料，再用真空除泡机进行除泡处理，得到透明陶瓷光纤浆料。
Step5、将上述透明陶瓷光纤浆料加入0.25 wt.%聚氨酯（TPU）后放入搅拌机内搅拌45 min，得到透明陶瓷光纤前驱体。
Step6、将上述前驱体放入纺丝机内，以100 MPa的压力与0.1 m/s速度进行纺丝，得到透明陶瓷光纤素坯。
Step7、所述透明陶瓷光纤素坯素坯进行温等静压处理在温度60 ℃，150 MPa压力下温等10 min。然后进行干燥处理：放入110 ℃烘箱中保温6 h。干燥后进行排胶处理，从室温开始以1 ℃/min升温速度到450 ℃，再以1 ℃/min升温速度到800 ℃，并保温4 h。最后真空烧结，室温开始以8 ℃/min升温到 200 ℃，保温20 min，再次按15 ℃/min升温到1000℃并保温20 min，然后按3 ℃/min升温到1650 ℃并保温8 h，最后以7 ℃/min降温到室温，整个烧结过程中真空度保持在1×10-3 Pa。再经过抛光处理，得到2%Nd: YAG激光透明陶瓷光纤。

Claims (7)

1.一种基于Isobam凝胶与熔融纺丝技术的Nd：YAG透明陶瓷光纤的制备方法，其特征在于：包括如下步骤：
Step1、按照Nd: YAG透明陶瓷材料 (Y1-xNdx)3A15O12，0.01≤x≤0.04的化学计量比分别称量原料粉体，进行除杂处理；
Step2、将原料粉体、烧结助剂、Al2O3磨球、无水乙醇混合，球磨24~36 h，得到混合浆料；
Step3、将混合浆料烘干，过筛后置于马弗炉中煅烧，冷却后得到原料粉；
Step4、采用PIBM凝胶注模体系，使用上述原料粉配制陶瓷浆料；
Step5、在上述浆料中加入高分子化合物颗粒，得到透明陶瓷光纤前驱体；
所述高分子化合物颗粒为聚己内酯、聚乳酸或聚氨酯，高分子化合物颗粒的用量为浆料的0.1 wt.%~ 0.5 wt.%；
Step6、将上述前驱体加入熔融纺丝机中纺丝成型，得到透明陶瓷光纤素坯；
熔融纺丝机的熔融温度为90~120 ℃，压力为100~120 MPa，纺丝速度为0.1~0.5 m/s；
Step7、将透明陶瓷光纤素坯进行温等静压、干燥、排胶、真空烧结、抛光处理，即可得到透明陶瓷光纤。
2.根据权利要求1所述的制备方法，其特征在于：Step1中，所述原料粉体为氧化钕Nd2O3、氧化铝Al2O3和氧化钇Y2O3；除杂处理采用煅烧方法。
3.根据权利要求1所述的制备方法，其特征在于：Step2中，所述烧结助剂为MgO和SiO2的混合物。
4.根据权利要求1所述的制备方法，其特征在于：Step2中，烧结助剂、Al2O3磨球、无水乙醇和原料粉体的用量比为1：600：240：200。
5.根据权利要求1所述的制备方法，其特征在于：Step3中，烘干采用40～100 ℃恒温烘箱，浆料蒸发时间为24～48 h；煅烧温度为800～1000 ℃，保温8～24 h。
6.根据权利要求1所述的制备方法，其特征在于：Step4中，所述PIBM凝胶注模体系使用Isobam104#作为凝胶剂、柠檬酸铵作为分散剂；陶瓷浆料的固含量为45 vol.%~ 50 vol.%。
7.根据权利要求1所述的制备方法，其特征在于：Step7中，所述温等静压的条件为100～200 MPa下5～20 min；所述干燥工艺是在100～120 ℃的烘箱中干燥4～8 h；所述排胶是室温～450 ℃升温速度为0.5～2 ℃/min，450～800 ℃升温速度为0.5～3 ℃/min，在800℃保温2～6 h；所述真空烧结工艺为：室温下先按5～10 ℃/min升温到200 ℃，保温10～30min，再按10～20 ℃/min升温到1000 ℃并保温10～30 min，然后按1～5 ℃/min升温到1650 ℃并保温6～10 h，最后以5～10 ℃/min降温到室温，烧结过程中真空度保持在1×10-2～1×10-5 Pa。
CN202110498840.5A 2021-05-08 2021-05-08 一种基于Isobam凝胶与熔融纺丝技术的透明陶瓷光纤制备方法 Active CN113213931B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110498840.5A CN113213931B (zh) 2021-05-08 2021-05-08 一种基于Isobam凝胶与熔融纺丝技术的透明陶瓷光纤制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110498840.5A CN113213931B (zh) 2021-05-08 2021-05-08 一种基于Isobam凝胶与熔融纺丝技术的透明陶瓷光纤制备方法

Publications (2)

Publication Number Publication Date
CN113213931A CN113213931A (zh) 2021-08-06
CN113213931B true CN113213931B (zh) 2022-06-24

Family

ID=77091800

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110498840.5A Active CN113213931B (zh) 2021-05-08 2021-05-08 一种基于Isobam凝胶与熔融纺丝技术的透明陶瓷光纤制备方法

Country Status (1)

Country Link
CN (1) CN113213931B (zh)

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106927808B (zh) * 2017-04-10 2020-05-01 山东大学 一种钇铝石榴石连续纤维的制备方法
CN110042504B (zh) * 2019-03-14 2021-10-01 国装新材料技术(江苏)有限公司 具有凝胶纺丝功能的环糊精复合陶瓷前驱体及制备方法
CN110373738B (zh) * 2019-08-19 2021-12-03 闽江学院 一种暖色光发光纤维的制备方法
CN112341184B (zh) * 2020-11-09 2021-11-23 新沂市锡沂高新材料产业技术研究院有限公司 一种基于Isobam凝胶态浸涂技术的波导结构激光透明陶瓷光纤的制备方法

Also Published As

Publication number Publication date
CN113213931A (zh) 2021-08-06

Similar Documents

Publication Publication Date Title
CN102060539B (zh) 利用注浆成型制备钇铝石榴石基透明陶瓷的方法
CN100360469C (zh) 双掺杂的钇铝石榴石透明陶瓷材料及制备方法
CN112341184B (zh) 一种基于Isobam凝胶态浸涂技术的波导结构激光透明陶瓷光纤的制备方法
CN100564310C (zh) 双掺杂的钇铝石榴石透明陶瓷材料及制备方法
CN110885244B (zh) 一种钇铝石榴石基透明陶瓷光纤的制备方法
CN108516820B (zh) 一种氧化铟锡靶材的短流程烧结工艺
CN111253154A (zh) 一种凝胶注模制备yag基芯壳结构棒状透明陶瓷的方法
CN105218095B (zh) 利用凝胶注模成型反应烧结制备钇铝石榴石透明陶瓷的方法
CN107721424B (zh) 一种凝胶注模成型制备yag透明陶瓷的方法
CN103626487A (zh) 复合结构钇铝石榴石透明陶瓷的制备方法
CN111270347A (zh) 一种凝胶注模成型制备透明陶瓷光纤的方法
CN105601277A (zh) 一种氧化钇基透明陶瓷的制备方法
CN101985398A (zh) 一种透明多晶Re:YAG陶瓷的制备方法
CN104725052A (zh) 一种多层复合结构透明陶瓷的制备方法
CN112209715B (zh) 一种用于激光器的金属包层的Nd:YAG陶瓷光纤及其制备方法
CN104451953B (zh) 三价镱离子掺杂镥铝石榴石透明陶瓷光纤的制备方法
CN109095916A (zh) 一种sps烧结制备yag透明陶瓷的方法
CN112281213B (zh) 稀土掺杂(LuaScbYc)2O3(a+b+c=1）单晶光纤及其制备方法与应用
CN111925202A (zh) 一种无烧结助剂的钇铝石榴石粉体、钇铝石榴石陶瓷、其制备方法与应用
CN104926355B (zh) 基于明胶溶液冷冻干燥技术制备定向多孔氮化硅陶瓷的方法
CN103319093B (zh) 掺镱氟磷酸锶微晶掺镱氟磷酸盐玻璃复合材料及制备方法
CN105565810A (zh) 稀土离子掺杂的氧化钇激光陶瓷光纤的制备方法
CN113213931B (zh) 一种基于Isobam凝胶与熔融纺丝技术的透明陶瓷光纤制备方法
CN107324805A (zh) 一种多组分石榴石基激光透明陶瓷材料及其制备方法
CN104829221A (zh) 凝胶注模成型制备Re:YAG透明陶瓷的方法

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
GR01 Patent grant
GR01 Patent grant