CN108570725B - A kind of melt spinning raw material of aluminium oxide continuous fiber, preparation method and aluminium oxide continuous fiber obtained - Google Patents
A kind of melt spinning raw material of aluminium oxide continuous fiber, preparation method and aluminium oxide continuous fiber obtained Download PDFInfo
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- CN108570725B CN108570725B CN201710135875.6A CN201710135875A CN108570725B CN 108570725 B CN108570725 B CN 108570725B CN 201710135875 A CN201710135875 A CN 201710135875A CN 108570725 B CN108570725 B CN 108570725B
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- 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
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
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- 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
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- 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
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- 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
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Abstract
The present invention relates to a kind of melt spinning raw material of aluminium oxide continuous fiber, preparation method and aluminium oxide continuous fibers obtained.It include: that 1) poly- aikyiaiurnirsoxan beta is placed in reaction kettle, it is heated to 60~100 DEG C, vacuum distillation, 110~140 DEG C are continuously heating to, heat preservation is finally warming up to 150~200 DEG C again, when sampling survey softening point reaches target softening point, stop heating, is down to room temperature, obtains solid alumina presoma PAO-P；2) by dispersing agent, body containing aluminium powder and solvent with mass ratio 1:(1.5~4): (3~6) mixing, grinding obtain powdery pulp；3) gained presoma is mixed with gained powdery pulp, is warming up to 150~200 DEG C of vacuum distillations and obtains melt spinning raw material.This method synthesized can melt-spun alumina precursor PAO-P, and provide alumina fibre precursor melt spinning and sintering process, overcome the defect that aluminium oxide continuous fiber can not be prepared by melt spinning.
Description
Technical field
The invention belongs to the preparation fields of ceramic fibre, specifically, it is related to the preparation of inorganic oxide ceramic fibre, it is special
It is not the melt spinning raw material for being related to a kind of aluminium oxide continuous fiber, preparation method and aluminium oxide continuous fiber obtained.
Background technique
Alumina fibre is a kind of development situation of high-performance inorganic fibers.It is with Al2O3For main component, some also contains other metals
Oxide such as ZrO2And SiO2Deng with diversified forms such as long fine, short fibre, whiskers.The outstanding advantages of alumina fibre are high-strength
Degree, high-modulus, and excellent mechanical property under 1000~1200 DEG C of air atmospheres, while also having thermal conductivity small, heat is swollen
The advantages that swollen coefficient is low, good thermal shock.In addition, aluminium oxide is fine compared with other development situation of high-performance inorganic fibers such as silicon carbide fibre
It is low to tie up cost of material, and simple production process, there are huge market prospects in aerospace and civilian high end materials field.
Viscosity is low after aluminium oxide ceramics fusing point height and thawing, can not be produced with traditional melt drawing technique.Various countries thus
Researcher develops several different production lines using chemical method successively, and wherein precursor process is preparation of industrialization aluminium oxide
The main method of continuous fiber.According to precursor material Species differences, particularly may be divided into organic fiber infusion process, inorganic salts method,
Sol-gel method, organic polymer precursor body method and mud solution method etc..3M company uses sol-gel method, to crystallize chlorine
Changing aluminium, acetic acid, aluminium powder, deionized water etc. is raw material, forms the sticky hydrosol that main body is aluminium chloride by multistep reaction.
By preparation can wire drawing colloid presoma precursor is formed after continuous dry spinning is dry, pass through continuous heat and control crystallization side
To and speed, be transformed into oxide fibre (H.G.Sowman in'Sol-Gel Technology for Thin Films,
Fibers,Preforms,Electronics,and Specialty Shapes'(edited by L.C.Klein),Noyes,
Park Ridge,NJ,U.S.A,1988,p.140).The shortcomings that dry spinning is the volatilization of solvent caused by solution-polymerized SBR is dried again
Environmental pollution and solvent volatilization process is caused to be influenced by environment temperature, humidity, strand quality is not easy to control.And it melts and spins
Silk technique avoids the use of solvent, solves problem above at all, therefore become the spinning technique of chemical fibre industry first choice.
E.I.Du Pont company uses mud solution method, with partial size < 500nm α-Al2O3Powder main material, Al2(OH)5Cl·2H2O aqueous solution is auxiliary rheological agents, and obtaining diameter through melt-spun, aging, cracking, ceramic is 20um, and the trade mark is the oxidation of FP
Aluminium continuous fiber, since fiber is thicker, mechanical property is horizontal (ALUMINA FIBER~US 3,808,015) not as good as 3M company.
The country is only able to achieve the industrialized production of alumina fibre cotton at present, and product temperature resistant grade only has 800 DEG C, continuous fine
Dimension was developed still in the laboratory research stage, and Shandong University is using aluminium chloride, aluminum nitrate and aluminium isopropoxide as raw material, using colloidal sol-
Gel method is prepared for aluminium oxide continuous fiber (CN2012140454976.7), and properties of product are horizontal close to external middle end product, by
Synthetic method is limited to, and remaining sodium potassium ion, influences the mechanical behavior under high temperature of fiber in fiber.
Melt spinning is to squeeze out raw material heating melting by spinneret orifice, and cooling and solidifying forms the spinning of fiber in air
Silk method.The advantages of this method be it is simple to equipment requirement, be not necessarily to solvent, pollute it is small, working environment is good.But due to Al atom
With stronger metallicity, it is difficult to prepare the alumina precursor that can be melted, therefore there is no melted using presoma at present
Spinning prepares the report of alumina fibre, and the viscosity of aluminium oxide ceramics fusing point height and melt is low, therefore can not be as quartz fibre
It is produced like that using traditional melt-drawing method.
For these reasons, the present invention is specifically proposed.
Summary of the invention
The technical problem to be solved in the present invention is that overcoming the deficiencies of the prior art and provide a kind of aluminium oxide continuous fiber
Spinning material, preparation method and aluminium oxide continuous fiber obtained.
To achieve the purpose of the present invention, the present invention adopts the following technical scheme:
A kind of preparation method of the melt spinning raw material of aluminium oxide continuous fiber, wherein the preparation method includes such as
Lower step:
1) preparation of melt spinning type alumina precursor: poly- aikyiaiurnirsoxan beta is placed in reaction kettle, is heated to 60 under stirring
~100 DEG C, it is evaporated under reduced pressure 30min~3h, is continuously heating to 110~140 DEG C, 30min~3h is kept the temperature, is finally warming up to 150 again
~200 DEG C, softening point is surveyed in every 10min sampling, when reaching target softening point, stops heating, nitrogen protection drops to room temperature, obtains
To can melt-spun solid alumina presoma PAO-P；
2) preparation of powdery pulp: by dispersing agent, body containing aluminium powder and solvent with mass ratio 1:(1.5~4): (3~6) carry out
Mixing, grinding obtain powdery pulp；
3) the resulting presoma of step 1) and the resulting powdery pulp of step 2) preparation of melt spinning raw material: are pressed into quality
It is uniformly mixed than 100:0~15:85, preferably 80:20~30:70, then heats to 150~200 DEG C of vacuum distillation 20min~2h
Obtain melt spinning raw material.
Poly- aikyiaiurnirsoxan beta (PAO) used in the present invention is purchased from Suzhou Tu Na Materials Co., Ltd, and specific synthesis mode is referring to special
Sharp CN201610066594.5 further polymerize the work in poly- aikyiaiurnirsoxan beta strand by techniques such as vacuum distillation, producing high-moleculars
Property functional group to improve its molecular weight and softening point obtain the solid alumina presoma with favorable spinning quality.
Melt spinning is to squeeze out raw material heating melting by spinneret orifice, and cooling and solidifying forms the spinning of fiber in air
Silk method, it is simple to equipment requirement, good without solvent, the small and working environment of pollution to have the advantages that.And aluminium oxide ceramics fusing point
High and melt viscosity is low, therefore can not be produced as quartz fibre using traditional melt-drawing method.And due to Al original
Son has stronger metallicity, makes it difficult to prepare the alumina precursor that can be melted, therefore there is no at present using forerunner
Body melt spinning prepares the report of alumina fibre.Present invention obtains the solid alumina forerunners with favorable spinning quality
Body overcomes aluminium oxide continuous fiber in the prior art and is difficult to the defect being prepared by melt spinning method.
Wherein, target softening point described in step 1) is 80~130 DEG C, preferably 90~125 DEG C.
It is ground to be put into sand mill described in step 2) and 2~8h is ground with 5Hz~46Hz frequency.
Dispersing agent described in step 2) is prepared with the following method: by poly- aikyiaiurnirsoxan beta and polyethylene glycol in solvent
1~3h of back flow reaction, decompression obtain dispersing agent (PAO-S) except solvent.
The mass ratio of the poly- aikyiaiurnirsoxan beta, polyethylene glycol and solvent is 1:(0.2~1): (1~5)；The poly- second two
The molecular weight of alcohol is 200~6000；The solvent is one of normal propyl alcohol, isopropanol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether
Or several mixture.
In step 2), the body containing aluminium powder is aluminium powder, glassy state Al2O3、γ-Al2O3、α-Al2O3, it is a kind of in mullite
Or several mixtures, diameter of particle are 30nm~500nm；In step 2), the solvent is normal propyl alcohol, isopropanol, anhydrous
The mixture of one or more of ethyl alcohol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, toluene.
The present invention also provides the melt spinning raw materials of the aluminium oxide continuous fiber of preparation method preparation.
The object of the invention is also to provide a kind of aluminium oxide continuous fiber, the aluminium oxide continuous fiber is using this
The invention melt spinning raw material is prepared.
The present invention furthermore provides the preparation method of the aluminium oxide continuous fiber, this method include melt spinning,
Non-fusible, cracking and firing.
Further, the melt spinning are as follows: spinning material is placed in the spinning cylinder of melt spinning device, nitrogen is protected
The lower heating of shield is heated to 150~180 DEG C, after its melting is uniform melt and removes residual bubbles, 110~155 DEG C into
Row melt spinning through boundling, receives silk, obtains continuous alumina fiber precursor.
Described is non-fusible are as follows: the resulting continuous alumina fiber precursor of step 1) is placed in climatic chamber, is first risen
Temperature keeps the temperature 20min~2h to 30~40 DEG C under 30~45% relative humidity, then is warming up to 60~95 DEG C, 60~95%
Humidity under keep the temperature 10min~2h, be cooled to room temperature to obtain fusion-free fibre.
The cracking and firing can be carried out according to method commonly used in the art, and as a preferred embodiment, described splits
Solution and firing carry out in the following manner:
The cracking are as follows: the resulting fusion-free fibre of step 2) is placed in high temperature furnace with 0.5~30 DEG C/min heating
To 500~800 DEG C, 20min~3h is kept the temperature, cracking atmosphere is the mixing of one or more of nitrogen, argon gas, helium, air
Gas；
The firing are as follows: fiber after cracking is warming up to 1000~1800 with the heating rate of 0.15~100 DEG C/min
DEG C processing 1min~10h, firing atmosphere is air.
Specifically, the preparation method includes the following steps:
1) melt spinning: spinning material is placed in the spinning cylinder of melt spinning device, and heating is heated under nitrogen protection
150~180 DEG C, after its melting is uniform melt and removes residual bubbles, in 110~155 DEG C of progress melt spinnings, through collecting
Beam receives silk, obtains continuous alumina fiber precursor；
2) non-fusible: the resulting continuous alumina fiber precursor of step 1) being placed in climatic chamber, is first warming up to 30
~40 DEG C, 20min~2h is kept the temperature under 30~45% relative humidity, then be warming up to 60~95 DEG C, in 60~95% humidity
Lower heat preservation 10min~2h, is cooled to room temperature to obtain fusion-free fibre；
3) it cracks: the resulting fusion-free fibre of step 2) is placed in high temperature furnace and is warming up to 500 with 0.5~30 DEG C/min~
800 DEG C, 20min~3h is kept the temperature, cracking atmosphere is the gaseous mixture of one or more of nitrogen, argon gas, helium, air；
4) it is burnt into: fiber after cracking is warming up to 1000~1800 DEG C of processing with the heating rate of 0.15~100 DEG C/min
1min~10h, firing atmosphere are air.
The key problem in technology of this method be to have synthesized can melt-spun solid alumina presoma PAO-P, and provide aluminium oxide
Fiber precursor melt spinning and sintering process.In order to further increase fibre strength, nanometer is added into spinning material and contains aluminium powder
Body, and the poly- aikyiaiurnirsoxan beta dispersing agent PAO-S of graft modification for improving dispersing uniformity.It is modified the another beneficial of poly- aikyiaiurnirsoxan beta
Effect is generation nano microcrystalline aluminium oxide after cracking, improves bulk ceramics yield and the densification of ceramic fibre of spinning material
Degree.Aluminium oxide continuous fiber preparation method provided by the invention is environmentally protective, and quality is stablized, and mechanical behavior under high temperature is excellent, and
Aluminium oxide continuous fiber large-scale industrial production can be fast implemented.
The novel processing step of aluminium oxide continuous fiber provided by the present invention, before type solid alumina can be spun by synthesis
Body is driven, realizes melt-spinning technology, reduces solvent contamination, improves production efficiency and fiber quality consistency, while this method is former
Sodium potassium ion is free of in material, avoids its chemical damage to fiber under high temperature.It is spun using presoma in conjunction with powder body melting containing aluminium
Silk effectively improves the aluminium content of fiber precursor, reduces the fiber volume in ceramming process and shrinks and mechanical property loss.
Technical characterstic of the invention is as follows, using the poly- aikyiaiurnirsoxan beta of modification (PAO-S) as dispersing agent with powder it is evenly dispersed it
It is mixed with spinning material with the alumina precursor of producing high-molecular (PAO-P) again afterwards, melt spinning prepares aluminium oxide fibre later
Tie up precursor.Modified poly- aikyiaiurnirsoxan beta is the compatibility of raising presoma PAO-P and powder as the beneficial effect of dispersing agent, and its
Aluminium oxide can be generated in subsequent cracking process, be conducive to the bulk ceramics yield for improving spinning material；The spinning material is homogeneously steady
It is fixed, it can at room temperature sealed storage 2 years or more.
Another beneficial effect of the present invention is the present invention prepares fiber precursor using melt spinning, and equipment is simple, operation side
Just, at low cost, it is pollution-free, suitable for fast implementing amplification large-scale production.
Detailed description of the invention
Fig. 1 is the SEM picture of fiber prepared by embodiment 1；
Fig. 2 is the XRD diagram piece of fiber prepared by embodiment 1；
Fig. 3 a is the SEM picture of fiber prepared by embodiment 3；
Fig. 3 b is the SEM amplification picture of fiber prepared by embodiment 3；
Fig. 4 is the XRD diagram piece of fiber prepared by embodiment 3；
Fig. 5 is the photo of fiber prepared by embodiment 3；
Fig. 6 is the photo of fiber prepared by comparative example 1；
Fig. 7 a is the photomacrograph of fiber after 7 gained fiber of embodiment handles 20min at 1550 DEG C；
Fig. 7 b is the micrograph of fiber after 7 gained fiber of embodiment handles 20min at 1550 DEG C；
Fig. 8 a is the photomacrograph of fiber after the nextel-610 fiber of commercialization handles 20min at 1550 DEG C；
Fig. 8 b is the micrograph of fiber after the nextel-610 fiber of commercialization handles 20min at 1550 DEG C.
It should be noted that these attached drawings and verbal description are not intended to the design model limiting the invention in any way
It encloses, but illustrates idea of the invention by referring to specific embodiments for those skilled in the art.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, the technical solution in embodiment is clearly and completely described, the following examples are intended to illustrate the invention, but
It is not intended to limit the scope of the invention.
Embodiment 1
It is added without powder, the direct melt spinning of PAO-P prepares alumina fibre
1. the preparation of melt spinning raw material:
The preparation of melt spinning type alumina precursor: the poly- aikyiaiurnirsoxan beta of 500g is placed in reaction kettle, is heated under stirring
80 DEG C, it is evaporated under reduced pressure 1h, is continuously heating to 120 DEG C, keeps the temperature 1h, is finally warming up to 160 DEG C again, softening point is surveyed in every 10min sampling,
When softening point reaches 90 DEG C, stop heating, nitrogen protection drops to room temperature and secures satisfactory grades the alumina precursor PAO-P of sub-ization；
2. the preparation of alumina fibre
(1) melt spinning: spinning material is placed in the spinning cylinder of melt spinning device, and heating is heated under nitrogen protection
150 DEG C, after its melting is uniform melt and removes residual bubbles, in 120 DEG C of progress melt spinnings, through boundling, silk is received, is obtained
Continuous alumina fiber precursor；
(2) non-fusible: continuous alumina fiber precursor obtained by step (1) being placed in climatic chamber, is first warming up to 40
DEG C, 30min is kept the temperature under 30% relative humidity, then be warming up to 90 DEG C, keep the temperature 20min under 80% humidity, be cooled to room
Temperature obtains fusion-free fibre；
(3) it cracks: fusion-free fibre obtained by step (3) being placed in high temperature furnace and is warming up to 600 DEG C with 1 DEG C/min, heat preservation
1h, cracking atmosphere are air；
(4) it is burnt into: fiber after cracking being warming up to 1000 DEG C of processing 20min with the heating rate of 30 DEG C/min, is burnt into gas
Atmosphere is air.
Fig. 1 is the SEM photograph of gained fiber, and as can be seen from Figure, fiber surface is smooth, of uniform size, fibre diameter 10
~12 μm.XRD shown in Fig. 2 the result shows that, the crystal phase group of fiber becomes γ-Al2O3。
Embodiment 2
It is added without powder, the direct melt spinning of PAO-P prepares alumina fibre
1. the preparation of melt spinning raw material:
The preparation of melt spinning type alumina precursor: the poly- aikyiaiurnirsoxan beta of 500g is placed in reaction kettle, is heated under stirring
85 DEG C, it is evaporated under reduced pressure 2h, is continuously heating to 140 DEG C, keeps the temperature 1h, is finally warming up to 170 DEG C again, softening point is surveyed in every 10min sampling,
When softening point reaches 120 DEG C, stop heating, nitrogen protection drops to room temperature and secures satisfactory grades the alumina precursor PAO-P of sub-ization；
2. the preparation of alumina fibre
(1) melt spinning: spinning material is placed in the spinning cylinder of melt spinning device, and heating is heated under nitrogen protection
180 DEG C, after its melting is uniform melt and removes residual bubbles, in 150 DEG C of progress melt spinnings, through boundling, silk is received, is obtained
Continuous alumina fiber precursor；
(2) non-fusible: continuous alumina fiber precursor obtained by step (1) being placed in climatic chamber, is first warming up to 40
DEG C, 1h is kept the temperature under 40% relative humidity, then be warming up to 85 DEG C, keep the temperature 30min under 90% humidity, be cooled to room temperature
To fusion-free fibre；
(3) it cracks: fusion-free fibre obtained by step (2) being placed in high temperature furnace and is warming up to 700 DEG C with 5 DEG C/min, heat preservation
2h, cracking atmosphere are helium；
(4) it is burnt into: fiber after cracking being warming up to 1200 DEG C of processing 10min with the heating rate of 10 DEG C/min, is burnt into gas
Atmosphere is air.
Fiber surface is smooth, of uniform size, and fibre diameter is 10~12 μm, and the crystal phase group of fiber becomes γ-Al2O3。
Embodiment 3
1. the preparation of melt spinning raw material:
(1) preparation of melt spinning type alumina precursor: the poly- aikyiaiurnirsoxan beta of 500g is placed in reaction kettle, stirs lower heating
To 80 DEG C, it is evaporated under reduced pressure 1h, is continuously heating to 120 DEG C, keeps the temperature 1h, is finally warming up to 180 DEG C again, softening is surveyed in every 10min sampling
Point stops heating when softening point reaches 113 DEG C, and nitrogen protection drops to room temperature and secures satisfactory grades the alumina precursor of sub-ization
PAO-P；
(2) preparation of powdery pulp: poly- aikyiaiurnirsoxan beta (PAO) and polyethylene glycol (PEG-200) is flowed back in normal propyl alcohol anti-
1h is answered, the mass ratio of poly- aikyiaiurnirsoxan beta (PAO), polyethylene glycol (PEG-200) and normal propyl alcohol is 1:0.2:1, and decompression is obtained except solvent
Dispersing agent (PAO-S)；By dispersing agent, the α-Al that partial size is 150nm2O3Powder and normal propyl alcohol are put into sand milling with mass ratio 1:1.5:3
Powdery pulp is obtained with 46Hz frequency grinding 5h in machine；
(3) step (1) resulting presoma and step (2) resulting powdery pulp the preparation of spinning material: are pressed into quality
Mixing more uniform than 70:30 then heats to 170 DEG C of vacuum distillation 30min and obtains spinning material；
2. the preparation of alumina fibre
(1) melt spinning: spinning material is placed in the spinning cylinder of melt spinning device, and heating is heated under nitrogen protection
175 DEG C, after its melting is uniform melt and removes residual bubbles, in 145 DEG C of progress melt spinnings, through boundling, silk is received, is obtained
Continuous alumina fiber precursor；
(2) non-fusible: continuous alumina fiber precursor obtained by step (1) being placed in climatic chamber, is first warming up to 30
DEG C, 50min is kept the temperature under 40% relative humidity, then be warming up to 80 DEG C, keep the temperature 10min under 90% humidity, be cooled to room
Temperature obtains fusion-free fibre；
(3) it cracks: fusion-free fibre obtained by step (3) being placed in high temperature furnace and is warming up to 800 DEG C with 10 DEG C/min, heat preservation
2h, cracking atmosphere are nitrogen；
(4) it is burnt into: fiber after cracking being warming up to 1550 DEG C of processing 20min with the heating rate of 10 DEG C/min, is burnt into gas
Atmosphere is air.
Fig. 3 a and Fig. 3 b are the SEM photograph and SEM enlarged photograph of gained fiber, and as can be seen from Figure, fiber surface is smooth, ruler
Very little uniformly particle size is less than 500nm, and fibre diameter is 10~12 μm.XRD shown in Fig. 4 the result shows that, the crystal phase group of fiber
As α-Al2O3。
Embodiment 4
1. the preparation of melt spinning raw material:
(1) preparation of melt spinning type alumina precursor: the poly- aikyiaiurnirsoxan beta of 500g is placed in reaction kettle, stirs lower heating
To 80 DEG C, it is evaporated under reduced pressure 1h, is continuously heating to 110 DEG C, keeps the temperature 3h, after being continuously heating to 180 DEG C, softening is surveyed in every 10min sampling
Point stops heating when softening point reaches 120 DEG C, and nitrogen protection drops to room temperature and secures satisfactory grades the alumina precursor of sub-ization
PAO-P；
(2) preparation of powdery pulp: poly- aikyiaiurnirsoxan beta (PAO) and polyethylene glycol (PEG-2000) is flowed back in isopropanol anti-
2h is answered, the mass ratio of poly- aikyiaiurnirsoxan beta (PAO), polyethylene glycol (PEG-2000) and isopropanol is 1:0.3:5, and decompression is obtained except solvent
Dispersing agent (PAO-S)；Dispersing agent, the mullite powder that partial size is 258nm and ethylene glycol ethyl ether are put into sand with mass ratio 1:2:4
Powdery pulp is obtained with 30Hz frequency grinding 8h in grinding machine；
(3) step (1) resulting presoma and step (2) resulting powdery pulp the preparation of spinning material: are pressed into quality
Mixing more uniform than 50:50 then heats to 180 DEG C of vacuum distillation 20min and obtains spinning material；
2. the preparation of alumina fibre
(1) melt spinning: spinning material is placed in the spinning cylinder of melt spinning device, and heating is heated under nitrogen protection
180 DEG C, after its melting is uniform melt and removes residual bubbles, in 155 DEG C of progress melt spinnings, through boundling, silk is received, is obtained
Continuous alumina fiber precursor；
(2) non-fusible: continuous alumina fiber precursor obtained by step (1) being placed in climatic chamber, is first warming up to 35
DEG C, 60min is kept the temperature under 45% relative humidity, then be warming up to 90 DEG C, keep the temperature 20min under 60% humidity, be cooled to room
Temperature obtains fusion-free fibre；
(3) it cracks: fusion-free fibre obtained by step (3) being placed in high temperature furnace and is warming up to 650 DEG C with 20 DEG C/min, heat preservation
3h, cracking atmosphere are air；
(4) it is burnt into: fiber after cracking is warming up to 1400 DEG C of processing 2h, firing atmosphere with the heating rate of 0.5 DEG C/min
For air.
Embodiment 5
1. the preparation of melt spinning raw material:
(1) preparation of melt spinning type alumina precursor: the poly- aikyiaiurnirsoxan beta of 500g is placed in reaction kettle, stirs lower heating
To 60 DEG C, it is evaporated under reduced pressure 3h, is continuously heating to 140 DEG C, keeps the temperature 30min, after being continuously heating to 150 DEG C, every 10min sampling is surveyed soft
Change point, when softening point reaches 110 DEG C, stop heating, nitrogen protection drops to room temperature and secures satisfactory grades the alumina precursor of sub-ization
PAO-P；
(2) preparation of powdery pulp: poly- aikyiaiurnirsoxan beta (PAO) and polyethylene glycol (PEG-6000) is returned in ethylene glycol ethyl ether
Stream reaction 2.5h, poly- aikyiaiurnirsoxan beta (PAO), polyethylene glycol (PEG-6000), ethylene glycol ethyl ether mass ratio be 1:0.8:4, decompression
Except solvent obtains dispersing agent (PAO-S)；By dispersing agent, the γ-Al that partial size is 50nm2O3Powder and ethylene glycol monomethyl ether are with mass ratio
1:4:6, which is put into sand mill, obtains powdery pulp with 20Hz frequency grinding 2h；
(3) step (1) resulting presoma and step (2) resulting powdery pulp the preparation of spinning material: are pressed into quality
Mixing more uniform than 20:80 then heats to 150 DEG C of vacuum distillation 2h and obtains spinning material；
2. the preparation of alumina fibre
(1) melt spinning: spinning material is placed in the spinning cylinder of melt spinning device, and heating is heated under nitrogen protection
150 DEG C, after its melting is uniform melt and removes residual bubbles, in 110 DEG C of progress melt spinnings, through boundling, silk is received, is obtained
Continuous alumina fiber precursor；
(2) non-fusible: continuous alumina fiber precursor obtained by step (1) being placed in climatic chamber, is first warming up to 30
DEG C, 40min is kept the temperature under 35% relative humidity, then be warming up to 60 DEG C, keep the temperature 2h under 85% humidity, be cooled to room temperature
To fusion-free fibre；
(3) it cracks: fusion-free fibre obtained by step (3) being placed in high temperature furnace and is warming up to 800 DEG C with 0.5 DEG C/min, protect
Warm 20min, cracking atmosphere are argon gas；
(4) it is burnt into: fiber after cracking is warming up to 1800 DEG C of processing 1min, firing atmosphere with the heating rate of 30 DEG C/min
For air.
Embodiment 6
1. the preparation of melt spinning raw material:
(1) preparation of melt spinning type alumina precursor: the poly- aikyiaiurnirsoxan beta of 500g is placed in reaction kettle, stirs lower heating
To 100 DEG C, it is evaporated under reduced pressure 30min, is continuously heating to 125 DEG C, keeps the temperature 2h, after being continuously heating to 200 DEG C, every 10min sampling is surveyed
Softening point stops heating when softening point reaches 125 DEG C, and nitrogen protection drops to room temperature and secures satisfactory grades the aluminum oxide precursor of sub-ization
Body PAO-P；
(2) preparation of powdery pulp: poly- aikyiaiurnirsoxan beta (PAO) and polyethylene glycol (PEG-6000) is returned in ethylene glycol monomethyl ether
Stream reaction 3h, the mass ratio of poly- aikyiaiurnirsoxan beta (PAO), polyethylene glycol (PEG-6000) and ethylene glycol monomethyl ether is 1:0.4:2, and decompression removes
Solvent obtains dispersing agent (PAO-S)；By dispersing agent, the γ-Al that partial size is 30nm2O3Powder and ethylene glycol monomethyl ether are with mass ratio 1:
4:6, which is put into sand mill, obtains powdery pulp with 5Hz frequency grinding 4h；
(3) step (1) resulting presoma and step (2) resulting powdery pulp the preparation of spinning material: are pressed into quality
Mixing more uniform than 15:85 then heats to 200 DEG C of vacuum distillation 1.5h and obtains spinning material；
2. the preparation of alumina fibre
(1) melt spinning: spinning material is placed in the spinning cylinder of melt spinning device, and heating is heated under nitrogen protection
160 DEG C, after its melting is uniform melt and removes residual bubbles, in 130 DEG C of progress melt spinnings, through boundling, silk is received, is obtained
Continuous alumina fiber precursor；
(2) non-fusible: continuous alumina fiber precursor obtained by step (1) being placed in climatic chamber, is first warming up to 30
DEG C, 20min is kept the temperature under 35% relative humidity, then be warming up to 95 DEG C, keep the temperature 45min under 95% humidity, be cooled to room
Temperature obtains fusion-free fibre；
(3) it cracks: fusion-free fibre obtained by step (3) being placed in high temperature furnace and is warming up to 500 DEG C with 30 DEG C/min, heat preservation
1h, cracking atmosphere are argon gas；
(4) it is burnt into: fiber after cracking being warming up to 1000 DEG C of processing 10h with the heating rate of 0.15 DEG C/min, is burnt into gas
Atmosphere is air.
Embodiment 7
1. the preparation of melt spinning raw material:
(1) preparation of melt spinning type alumina precursor: the poly- aikyiaiurnirsoxan beta of 500g is placed in reaction kettle, stirs lower heating
To 60 DEG C, it is evaporated under reduced pressure 3h, is continuously heating to 140 DEG C, keeps the temperature 30min, after being continuously heating to 200 DEG C, every 10min sampling is surveyed soft
Change point, when softening point reaches 130 DEG C, stop heating, nitrogen protection drops to room temperature and secures satisfactory grades the alumina precursor of sub-ization
PAO-P；
(2) preparation of powdery pulp: poly- aikyiaiurnirsoxan beta (PAO) and polyethylene glycol (PEG-6000) is flowed back in normal propyl alcohol anti-
1.5h is answered, the mass ratio of poly- aikyiaiurnirsoxan beta (PAO), polyethylene glycol (PEG-6000) and normal propyl alcohol is 1:0.5:3, and decompression is obtained except solvent
To dispersing agent (PAO-S)；By dispersing agent, the γ-Al that partial size is 500nm2O3Powder and toluene are put into sand with mass ratio 1:3.5:5
Powdery pulp is obtained with 15Hz frequency grinding 6h in grinding machine；
(3) step (1) resulting presoma and step (2) resulting powdery pulp the preparation of spinning material: are pressed into quality
Mixing more uniform than 25:75 then heats to 160 DEG C of vacuum distillation 45min and obtains spinning material；
2. the preparation of alumina fibre
(1) melt spinning: spinning material is placed in the spinning cylinder of melt spinning device, and heating is heated under nitrogen protection
160 DEG C, after its melting is uniform melt and removes residual bubbles, in 115 DEG C of progress melt spinnings, through boundling, silk is received, is obtained
Continuous alumina fiber precursor；
(2) non-fusible: continuous alumina fiber precursor obtained by step (1) being placed in climatic chamber, is first warming up to 30
DEG C, 2h is kept the temperature under 35% relative humidity, then be warming up to 60 DEG C, keep the temperature 2h under 85% humidity, be cooled to room temperature to obtain
Fusion-free fibre；
(3) it cracks: fusion-free fibre obtained by step (3) being placed in high temperature furnace and is warming up to 750 DEG C with 15 DEG C/min, heat preservation
1.5h, cracking atmosphere are argon gas；
(4) it is burnt into: fiber after cracking being warming up to 1300 DEG C of processing 1min with the heating rate of 100 DEG C/min, is burnt into gas
Atmosphere is air.
Embodiment 8
1. the preparation of melt spinning raw material:
(1) preparation of melt spinning type alumina precursor: the poly- aikyiaiurnirsoxan beta of 500g is placed in reaction kettle, stirs lower heating
To 60 DEG C, it is evaporated under reduced pressure 3h, is continuously heating to 140 DEG C, keeps the temperature 30min, after being continuously heating to 150 DEG C, every 10min sampling is surveyed soft
Change point, when softening point reaches 80 DEG C, stop heating, nitrogen protection drops to room temperature and secures satisfactory grades the alumina precursor of sub-ization
PAO-P；
(2) preparation of powdery pulp: poly- aikyiaiurnirsoxan beta (PAO) and polyethylene glycol (PEG-6000) is flowed back in normal propyl alcohol anti-
2.5h is answered, the mass ratio of poly- aikyiaiurnirsoxan beta (PAO), polyethylene glycol (PEG-6000) and normal propyl alcohol is 1:1:5, and decompression is obtained except solvent
Dispersing agent (PAO-S)；By dispersing agent, partial size be 50nm aluminium powder and dehydrated alcohol with mass ratio 1:4:6 be put into sand mill with
20Hz frequency grinding 2h obtains powdery pulp；
(3) step (1) resulting presoma and step (2) resulting powdery pulp the preparation of spinning material: are pressed into quality
Mixing more uniform than 80:20 then heats to 150 DEG C of vacuum distillation 2h and obtains spinning material；
2. the preparation of alumina fibre
(1) melt spinning: spinning material is placed in the spinning cylinder of melt spinning device, and heating is heated under nitrogen protection
150 DEG C, after its melting is uniform melt and removes residual bubbles, in 110 DEG C of progress melt spinnings, through boundling, silk is received, is obtained
Continuous alumina fiber precursor；
(2) non-fusible: continuous alumina fiber precursor obtained by step (1) being placed in climatic chamber, is first warming up to 30
DEG C, 40min is kept the temperature under 35% relative humidity, then be warming up to 60 DEG C, keep the temperature 2h under 85% humidity, be cooled to room temperature
To fusion-free fibre；
(3) it cracks: fusion-free fibre obtained by step (3) being placed in high temperature furnace and is warming up to 800 DEG C with 0.5 DEG C/min, protect
Warm 20min, cracking atmosphere are argon gas；
(4) it is burnt into: fiber after cracking is warming up to 1800 DEG C of processing 1min, firing atmosphere with the heating rate of 30 DEG C/min
For air.
Embodiment 9
1. the preparation of melt spinning raw material:
(1) preparation of melt spinning type alumina precursor: the poly- aikyiaiurnirsoxan beta of 500g is placed in reaction kettle, stirs lower heating
To 80 DEG C, it is evaporated under reduced pressure 1h, is continuously heating to 110 DEG C, keeps the temperature 3h, after being continuously heating to 180 DEG C, softening is surveyed in every 10min sampling
Point stops heating when softening point reaches 120 DEG C, and nitrogen protection drops to room temperature and secures satisfactory grades the alumina precursor of sub-ization
PAO-P；
(2) preparation of powdery pulp: poly- aikyiaiurnirsoxan beta (PAO) and polyethylene glycol (PEG-2000) is flowed back in isopropanol anti-
2h is answered, the mass ratio of poly- aikyiaiurnirsoxan beta (PAO), polyethylene glycol (PEG-2000) and isopropanol is 1:0.2:1, and decompression is obtained except solvent
Dispersing agent (PAO-S)；By dispersing agent, the glassy state Al that partial size is 258nm2O3Sand mill is put into mass ratio 1:2:4 with isopropanol
In with 30Hz frequency grinding 8h obtain powdery pulp；
(3) step (1) resulting presoma and step (2) resulting powdery pulp the preparation of spinning material: are pressed into quality
Mixing more uniform than 50:50 then heats to 180 DEG C of vacuum distillation 20min and obtains spinning material；
2. the preparation of alumina fibre
(1) melt spinning: spinning material is placed in the spinning cylinder of melt spinning device, and heating is heated under nitrogen protection
180 DEG C, after its melting is uniform melt and removes residual bubbles, in 155 DEG C of progress melt spinnings, through boundling, silk is received, is obtained
Continuous alumina fiber precursor；
(2) non-fusible: continuous alumina fiber precursor obtained by step (1) being placed in climatic chamber, is first warming up to 35
DEG C, 60min is kept the temperature under 45% relative humidity, then be warming up to 90 DEG C, keep the temperature 20min under 60% humidity, be cooled to room
Temperature obtains fusion-free fibre；
(3) it cracks: fusion-free fibre obtained by step (3) being placed in high temperature furnace and is warming up to 650 DEG C with 20 DEG C/min, heat preservation
3h, cracking atmosphere are air；
(4) it is burnt into: fiber after cracking is warming up to 1400 DEG C of processing 2h, firing atmosphere with the heating rate of 0.5 DEG C/min
For air.
Comparative example 1
Technical effect in order to illustrate the poly- aikyiaiurnirsoxan beta PAO-S of modification as dispersing agent, the present invention have done following comparative experiments:
The PAO-S in embodiment 3 is changed into common polyethylene glycol (PEG-200) as dispersing agent；Other conditions are constant.
As a result, it has been found that the dispersion of powder is very uneven in prepared spinning material, in spinning process, the powder of reunion is very
It is easy blocking spinneret orifice and causes fracture of wire.
The scanning electron microscope (SEM) photograph of 1 gained fiber precursor of embodiment 3 and comparative example is as shown in Figure 5 and Figure 6, will divide as can be seen from Figure
Occurs the region of powder aggregation after powder changes PEG-200 by PAO-S, in fiber precursor.
Table 1 gives the ceramic yield of the spinning material of embodiment and comparative example, it can be seen that the introducing of powdery pulp can be big
The big ceramic yield for improving spinning material, comparative example 3 and comparative example 1 can be seen that using PAO-S as dispersing agent to raising
The ceramic yield of spinning material is advantageous.
The ceramic yield of spinning material prepared by table 1, embodiment
| Specific embodiment | The ceramic yield of spinning material |
| Embodiment 1 | 30.2% |
| Embodiment 2 | 32.8% |
| Embodiment 3 | 39.0% |
| Embodiment 4 | 45.8% |
| Embodiment 5 | 64.6% |
| Embodiment 6 | 69.8% |
| Embodiment 7 | 61.1% |
| Embodiment 8 | 43.6% |
| Embodiment 9 | 44% |
| Comparative example 1 | 36.5% |
Comparative example 2
In order to compare the high temperature resistance of fiber prepared by this method, we are by the resulting fiber of the present embodiment 7 and quotient
The nextel-610 fiber of product, which is collectively disposed in Muffle furnace, is warming up to 1550 DEG C, keeps the temperature 20min, compares the macroscopical and micro- of the two
Pattern is seen, as a result as shown in Fig. 7 a, Fig. 7 b, Fig. 8 a and Fig. 8 b, if Fig. 7 a, Fig. 7 b can be seen that, the fiber warp of this method preparation
1550 DEG C, after the high-temperature process of 20min (left side), fiber is still more flexible, and synnema can bear the weight of the plastic hoop of 10g,
SEM figure (right side) display fiber tightly packed is made of the hundred nano-scale powder of size uniformity；It can be seen that by Fig. 8 a and Fig. 8 b, and quotient
The nextel-610 fiber of product is through 1550 DEG C, and viscous glutinous and silk, fiber occur after 20min high-temperature process (left side), between fiber
Become highly brittle, completely lose flexibility, the nanometer that SEM figure (right side) shows that fiber has size different is loose to micron-sized powder
It accumulates.The experiment show fiber prepared by the present invention in terms of high temperature resistance compared with the fiber with commercialization be have it is excellent
Gesture.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any to be familiar with technology people of the invention
Member without departing from the scope of the present invention, when the technology contents using above-mentioned prompt make it is a little variation or be modified to
The equivalent embodiment of equivalent variations, but anything that does not depart from the technical scheme of the invention content, it is right according to the technical essence of the invention
Any simple modification, equivalent change and modification made by above embodiments, in the range of still falling within the present invention program.
Claims (10)
1. a kind of preparation method of the melt spinning raw material of aluminium oxide continuous fiber, which is characterized in that the preparation method packet
Include following steps:
1) preparation of melt spinning type alumina precursor: poly- aikyiaiurnirsoxan beta is placed in reaction kettle, is heated to 60~100 under stirring
DEG C, it is evaporated under reduced pressure 30min~3h, is continuously heating to 110~140 DEG C, 30min~3h is kept the temperature, is finally warming up to 150~200 again
DEG C, softening point is surveyed in every 10min sampling, when reaching target softening point, stops heating, nitrogen protection drops to room temperature, and obtaining can
The solid alumina presoma PAO-P of melt-spun；The target softening point is 80~130 DEG C；
2) preparation of powdery pulp: by dispersing agent, body containing aluminium powder and solvent with mass ratio 1:(1.5~4): (3~6) are mixed
It closes, grinding obtains powdery pulp；
3) preparation of melt spinning raw material: in mass ratio by the resulting presoma of step 1) and the resulting powdery pulp of step 2)
100:0~15:85 is uniformly mixed, and is then heated to 150~200 DEG C of vacuum distillation 20min~2h and is obtained melt spinning raw material.
2. preparation method according to claim 1, which is characterized in that in step 3), the resulting presoma of step 1) and step
The mass ratio of rapid 2) resulting powdery pulp is 80:20~30:70.
3. preparation method according to claim 1, which is characterized in that target softening point described in step 1) be 90~
125℃。
4. preparation method according to claim 1, which is characterized in that be ground to be put into sand mill described in step 2)
2~8h is ground with 5Hz~46Hz frequency.
5. preparation method according to claim 1, which is characterized in that dispersing agent described in step 2) is with the following method
Be prepared: by poly- aikyiaiurnirsoxan beta and polyethylene glycol, 1~3h of back flow reaction, decompression obtain dispersing agent except solvent in solvent.
6. preparation method according to claim 5, which is characterized in that the poly- aikyiaiurnirsoxan beta, polyethylene glycol and solvent
Mass ratio is 1:(0.2~1): (1~5)；The molecular weight of the polyethylene glycol is 200~6000；The solvent is positive third
The mixture of one or more of alcohol, isopropanol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether.
7. preparation method according to claim 1, which is characterized in that in step 2), the body containing aluminium powder is aluminium powder, glass
Glass state Al2O3、γ-Al2O3、α-Al2O3, mixtures one or more of in mullite, diameter of particle is 30nm~500nm；Step
It is rapid 2) in, the solvent be one of normal propyl alcohol, isopropanol, dehydrated alcohol, ethylene glycol ethyl ether, ethylene glycol monomethyl ether, toluene
Or several mixture.
8. a kind of melt spinning of the aluminium oxide continuous fiber of the preparation method preparation as described in claim 1~7 any one
Raw material.
9. a kind of preparation method of aluminium oxide continuous fiber, which is characterized in that the preparation method is will be described in claim 8
Melt spinning raw material carry out melt spinning, it is non-fusible, cracking and firing.
10. preparation method according to claim 9, which is characterized in that the melt spinning are as follows: by claim 8 institute
The melt spinning raw material stated is placed in the spinning cylinder of melt spinning device, and heating is heated to 150~180 DEG C under nitrogen protection, to
It is melted for uniform melt and after removing residual bubbles, in 110~155 DEG C of progress melt spinnings, through boundling, is received silk, must be connected
Continuous alumina fibre precursor；
Described is non-fusible are as follows: the continuous alumina fiber precursor that melt spinning obtains is placed in climatic chamber, is first heated up
To 30~40 DEG C, 20min~2h is kept the temperature under 30~45% relative humidity, then be warming up to 60~95 DEG C, 60~95%
10min~2h is kept the temperature under humidity, is cooled to room temperature to obtain fusion-free fibre.
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| CN107904697A (en) * | 2017-11-20 | 2018-04-13 | 苏州图纳新材料科技有限公司 | The poly- aikyiaiurnirsoxan beta of solid-state, the preparation method of the poly- aikyiaiurnirsoxan beta of solid-state, alumina fibre cotton and preparation method thereof |
| CN110467439A (en) * | 2019-08-02 | 2019-11-19 | 中国航发北京航空材料研究院 | The preparation method of alumina fibre enhancing porous alumina ceramic based composites |
| CN110592724B (en) * | 2019-09-04 | 2021-01-26 | 中国科学院化学研究所 | Hf-Al-Si complex phase oxide ceramic fiber and preparation method thereof |
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| CN113968743B (en) * | 2020-07-22 | 2022-07-12 | 中国科学院化学研究所 | Al-Si co-polymerized oxide ceramic precursor and preparation method thereof |
| CN112409004B (en) * | 2020-11-12 | 2022-09-16 | 上海榕融新材料科技有限公司 | Preparation method of slurry for alumina continuous fiber reinforced ceramic composite material |
| CN113620693B (en) * | 2021-09-09 | 2022-08-23 | 成都海鑫高科技有限公司 | Preparation method of Gamma alumina fiber |
| CN115448340B (en) * | 2022-08-10 | 2024-06-21 | 杭州智华杰科技有限公司 | Method for improving heat conduction performance of alumina |
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