CN106592018A - 一种氧化铝纤维元素的溶胶凝胶制备方法 - Google Patents

一种氧化铝纤维元素的溶胶凝胶制备方法 Download PDF

Info

Publication number
CN106592018A
CN106592018A CN201611152356.2A CN201611152356A CN106592018A CN 106592018 A CN106592018 A CN 106592018A CN 201611152356 A CN201611152356 A CN 201611152356A CN 106592018 A CN106592018 A CN 106592018A
Authority
CN
China
Prior art keywords
preparation
sol
heat treatment
fibre
alumina
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
Application number
CN201611152356.2A
Other languages
English (en)
Inventor
曾曜龙
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.)
Jiangxi Jinsikang Pharmaceutical Co Ltd
Original Assignee
Jiangxi Jinsikang Pharmaceutical Co Ltd
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 Jiangxi Jinsikang Pharmaceutical Co Ltd filed Critical Jiangxi Jinsikang Pharmaceutical Co Ltd
Priority to CN201611152356.2A priority Critical patent/CN106592018A/zh
Publication of CN106592018A publication Critical patent/CN106592018A/zh
Pending legal-status Critical Current

Links

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
    • C04B35/01—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
    • C04B35/10—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 aluminium oxide
    • 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
    • C04B35/62236—Fibres based on aluminium oxide
    • 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
    • C04B35/624—Sol-gel processing
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • 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
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • 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
    • C04B2235/6567—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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/95—Products characterised by their size, e.g. microceramics
    • 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

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Fibers (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

本发明公开了属于无机纤维领域的一种氧化铝纤维元素的溶胶凝胶制备方法。以结晶氧化铝、去离子水以及铝粉为主要原料，以成丝助剂为辅料，得到可纺溶胶，可纺溶胶经成纤、干燥及热处理过程，最后得到氧化铝纤维。该制备方法原料易得、工艺简单、操作方便、能耗低，可得到连续纤维。所得到的凝胶纤维无色透明有光泽，表面光滑无明显缺陷；一定温度下热处理后得到的氧化铝纤维晶型完整、发育好，纤维表面致密均匀力学性能好。

Description

一种氧化铝纤维元素的溶胶凝胶制备方法
技术领域
本发明属于无机非金属材料制备技术领域，特别涉及一种氧化铝纤维的制备方法。
背景技术
氧化铝纤维是近几年来发展起来的一种新型高性能无机氧化物纤维，它是一种主要成分为氧化铝的多晶质无机纤维。氧化铝纤维具有化学稳定性、结构稳定性以及优异的高温力学性，广泛应用于对材料要求较高的领域。其原料易得，生产路径简单，对生产设备要求不高，无机化过程无需用惰性气体保护，可以直接在空气中进行。相对于碳纤维Nicalon 等商品无机纤维，氧化铝纤维的生产成本要低许多。在经济飞速发展的今天，氧化铝有着超群的性价比、军工上重要的战略意义和巨大的商业价值。作为重要的战略物资，氧化铝纤维的进口一直受到国外的限制，而国内对氧化铝的研究主要局限于短纤维，在连续氧化铝纤维方面，国内研究水平相对落后，得到的纤维连续性和力学性能达不到相关部门应用的要求，因此探索氧化铝纤维新的制备工艺，进一步提高氧化铝纤维的性能指标是目前我国氧化铝纤维研究中的重点。在这种国内生产的短纤维又无法满足需要的情况下，我国研究和开发具有自主知识产权的氧化铝连续纤维很有必要。
发明内容
本发明的目的是提供一种氧化铝纤维元素的溶胶凝胶制备方法。
一种氧化铝纤维元素的溶胶凝胶制备方法，其特征在于，该方法包括下列步骤：
(1) 取一定量的结晶氧化铝，加入去离子水，混合均匀，得到氯化铝溶液；
(2) 将铝粉按n(AlCl3·6H2O)/n(Al) ＝ 1 ∶ 2 ～ 1 ∶ 4 的比例加入所述氯化铝溶液中，在机械搅拌的同时于80 ～ 100℃的恒温水浴中加热回流6 ～ 16h，得到胶体母液；
(3) 将所述胶体母液中加入成纤助剂，搅拌均匀并40 ～ 100℃恒温浓缩一定时间，得到淡黄色透明胶体形态的勃姆石可纺溶胶；
(4) 将所述勃姆石可纺溶胶室温下成纤并干燥，得到凝胶纤维；
(5) 将所述凝胶纤维在1200℃～ 1400℃热处理温度下热处理，即得到氧化铝纤维。
所述胶体母液需进行抽滤处理。
所述成纤助剂为乳酸时，浓度为质量百分比5 ～ 20％。
所述成纤助剂为醋酸时，浓度为质量百分比5 ～ 40％。
所述母液浓缩为勃姆石可纺溶胶所需时间为10 ～ 12h。
所述成纤用勃姆石溶胶粘度为100 ～ 350Pa·s。
所述干燥为室温晾干12 ～ 36h。
所述热处理过程为室温～ 277℃之间的升温速率为0.5 ～ 2℃ /min，保温1 ～3h ；277℃～ 630℃之间的升温速率为0.5 ～ 2℃ /min，保温1 ～ 3h ；630℃以后的升温速率为2 ～ 5℃ /min，保温1 ～ 3h。
本发明的有益效果为：由于勃姆石溶胶采用溶胶凝胶法制备，该方法制备温度低，所用时间短，所得溶胶均匀性好，纯度高，性能稳定，而且该工艺简单易操作，工艺条件要求低，适于工业化推广应用。
附图说明
图1 是实施例1 制备的氧化铝纤维放大3000 倍的扫描电子显微镜(SEM) 图片。
图2 是实施例2 制备的氧化铝纤维放大3000 倍的扫描电子显微镜(SEM) 图片。
具体实施方式
采用溶胶凝胶法，以氯化铝、铝粉、水为原料制得胶体母液。将成纤助剂乳酸加入胶体母液中浓缩，得到可纺溶胶。可纺溶胶成纤得到凝胶纤维，干燥并一定温度下热处理后，最终得到氧化铝纤维。
下面结合附图和实施例对本发明作进一步说明：
实施例1
取一定量的结晶氧化铝，加入去离子水，混合均匀，得到氯化铝溶液。将铝粉按
n(AlCl3·6H2O)/n(Al) ＝ 1 ∶ 2 的比例加入所述氯化铝溶液中，在机械搅拌的同时于80℃的恒温水浴中加热回流12h，得到胶体母液，然后转移至抽滤装置中进行抽滤处理。在胶体母液中加入质量百分比为5％的乳酸成纤助剂，搅拌均匀并于60℃恒温浓缩12h，得到淡黄色透明胶体形态的粘度为100Pa·s 勃姆石可纺溶胶。将勃姆石可纺溶胶室温下成纤并干燥18h，得到凝胶纤维。凝胶纤维在1400℃热处理温度下热处理，室温～ 277℃之间的升温速率为1℃ /min，保温1h ；277℃～ 630℃之间的升温速率为1℃ /min，保温1h ；630℃～1400℃之间的升温速率为2℃ /min，保温1.5h，即得到氧化铝纤维。
图1 是实施例1 制备的氧化铝纤维放大3000 倍的扫描电子显微镜(SEM) 图片，可以看出纤维表面均匀致密、无表面缺陷。所得氧化铝纤维直径约为7μm，拉伸强5.8cN/dtex，断裂伸长率为12.07％。
实施例2
取一定量的结晶氧化铝，加入去离子水，混合均匀，得到氯化铝溶液。将铝粉按
n(AlCl3·6H2O)/n(Al) ＝ 1 ∶ 3 的比例加入所述氯化铝溶液中，在机械搅拌的同时于90℃的恒温水浴中加热回流10h，得到胶体母液，然后转移至抽滤装置中进行抽滤处理。在胶体母液中加入质量百分比为30％的醋酸成纤助剂，搅拌均匀并70℃恒温浓缩10h，得到淡黄色透明胶体形态的粘度为200Pa·s 勃姆石可纺溶胶，室温下成纤并在室温空气干燥24h，得到凝胶纤维。凝胶纤维在1200℃热处理温度下热处理，控制室温～ 277℃之间的升温速率为2℃ /min，保温3h ；控制277℃～ 630℃之间的升温速率为2℃ /min，保温3h ；控制630℃～1200℃之间的升温速率为5℃ /min，保温2h，即得到氧化铝纤维。
图2 是实施例2 制备的氧化铝纤维放大3000 倍的扫描电子显微镜(SEM) 图片，从图中可以看出氧化铝纤维表面均匀，有少许孔洞。所得氧化铝纤维直径约为6μm，拉伸强度
为3.8cN/dtex，断裂伸长率为9.07％。

Claims (8)

1.一种氧化铝纤维元素的溶胶凝胶制备方法，其特征在于，该方法包括下列步骤：
(1) 取一定量的结晶氧化铝，加入去离子水，混合均匀，得到氯化铝溶液；
(2) 将铝粉按n(AlCl3·6H2O)/n(Al) ＝ 1 ∶ 2 ～ 1 ∶ 4 的比例加入所述氯化铝溶液中，在机械搅拌的同时于80 ～ 100℃的恒温水浴中加热回流6 ～ 16h，得到胶体母液；
(3) 将所述胶体母液中加入成纤助剂，搅拌均匀并40 ～ 100℃恒温浓缩一定时间，得到淡黄色透明胶体形态的勃姆石可纺溶胶；
(4) 将所述勃姆石可纺溶胶室温下成纤并干燥，得到凝胶纤维；
(5) 将所述凝胶纤维在1200℃～ 1400℃热处理温度下热处理，即得到氧化铝纤维。
2.根据权利要求1 所述的制备方法，其特征在于：步骤(2) 中，所述胶体母液需进行抽滤处理。
3.根据权利要求1 所述的制备方法，其特征在于：步骤(3) 中，所述成纤助剂为乳酸时，浓度为质量百分比5 ～ 20％。
4.根据权利要求3 所述的制备方法，其特征在于：步骤(3) 中，所述成纤助剂为醋酸时，浓度为质量百分比5 ～ 40％。
5.根据权利要求1 所述的制备方法，其特征在于：步骤(3) 中，所述母液浓缩为勃姆石可纺溶胶所需时间为10 ～ 12h。
6.根据权利要求1 所述的制备方法，其特征在于：步骤(3) 中，所述成纤用勃姆石溶胶粘度为100 ～ 350Pa·s。
7.根据权利要求1 所述的制备方法，其特征在于：步骤(4) 中，所述干燥为室温晾干12～ 36h。
8.根据权利要求1 所述的制备方法，其特征在于：步骤(5) 中，所述热处理过程为室温～ 277℃之间的升温速率为0.5 ～ 2℃ /min，保温1 ～ 3h ；277℃～ 630℃之间的升温速率为0.5 ～ 2℃ /min，保温1 ～ 3h ；630℃以后的升温速率为2 ～ 5℃ /min，保温1～ 3h。
CN201611152356.2A 2016-12-14 2016-12-14 一种氧化铝纤维元素的溶胶凝胶制备方法 Pending CN106592018A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611152356.2A CN106592018A (zh) 2016-12-14 2016-12-14 一种氧化铝纤维元素的溶胶凝胶制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611152356.2A CN106592018A (zh) 2016-12-14 2016-12-14 一种氧化铝纤维元素的溶胶凝胶制备方法

Publications (1)

Publication Number Publication Date
CN106592018A true CN106592018A (zh) 2017-04-26

Family

ID=58801226

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611152356.2A Pending CN106592018A (zh) 2016-12-14 2016-12-14 一种氧化铝纤维元素的溶胶凝胶制备方法

Country Status (1)

Country Link
CN (1) CN106592018A (zh)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108486932A (zh) * 2018-03-28 2018-09-04 方建波 一种高稳定型环保固色剂的制备方法
CN111153685A (zh) * 2020-01-06 2020-05-15 佛山科学技术学院 连续氮化铝纤维及其制备方法
CN114591091A (zh) * 2022-04-08 2022-06-07 南通恩普热能技术有限公司 一种耐高温多晶绝热纤维生产装置及工艺

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108486932A (zh) * 2018-03-28 2018-09-04 方建波 一种高稳定型环保固色剂的制备方法
CN111153685A (zh) * 2020-01-06 2020-05-15 佛山科学技术学院 连续氮化铝纤维及其制备方法
CN111153685B (zh) * 2020-01-06 2022-03-22 佛山科学技术学院 连续氮化铝纤维及其制备方法
CN114591091A (zh) * 2022-04-08 2022-06-07 南通恩普热能技术有限公司 一种耐高温多晶绝热纤维生产装置及工艺

Similar Documents

Publication Publication Date Title
CN102965764B (zh) 一种氧化铝陶瓷连续纤维的制备方法
CN101239828B (zh) 氧化锆耐火纤维的制备方法
CN102167567B (zh) 一种柔性氧化铝陶瓷纤维及其制备方法
CN104141181B (zh) 一种含有SiO2掺杂的ZrO2纤维的制备方法
CN101498063B (zh) 全稳定立方相氧化锆晶体纤维的制备方法
CN106592018A (zh) 一种氧化铝纤维元素的溶胶凝胶制备方法
CN106757525A (zh) 一种晶体纤维的生产方法
CN108570725A (zh) 一种氧化铝连续纤维的熔融纺丝原料、其制备方法及制得的氧化铝连续纤维
CN109851336A (zh) 一种高模量致密连续莫来石纳米陶瓷纤维及其制备方法
CN106637510B (zh) 一种氧化锆纤维的制备方法
WO2024041439A1 (zh) 一种连续SiO2气凝胶复合纤维及其制备方法与应用
CN103114352A (zh) 一种氧化铝纤维的溶胶凝胶制备方法
CN107460545B (zh) 一种棒状氧化锆晶须的制备方法
CN102108567A (zh) 一种超细氧化镁陶瓷纤维的制备方法
CN103643402B (zh) 一种锆酸镧陶瓷纤维毡的制备方法
CN102775143A (zh) 一种全稳定四方相氧化锆晶体纤维的制备方法
CN110282963B (zh) 一种高韧性含铁莫来石柔性纤维及其制备方法
CN107572539A (zh) 一种复合凝胶隔热材料的制备方法
CN102242407B (zh) 一种氧化硅/银纳米复合纤维的制备方法
CN107955998A (zh) 一种轻质高柔莫来石超细/纳米陶瓷纤维及其制备方法
CN103993365B (zh) 采用氧氯化锆制备氧化锆晶体纤维的方法
CN106835353A (zh) 一种石墨烯中空纤维的制备方法
CN104692403A (zh) 一种单相莫来石溶胶的制备方法
CN103757751B (zh) 一种超高温氧化锆陶瓷纤维的制备方法
CN111074426B (zh) 一种氧化铝-氧化锆复合纤维毯及其制备方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20170426