CN102358697B - Preparation method of long fiber containing mullite alumina crystal phase - Google Patents
Preparation method of long fiber containing mullite alumina crystal phase Download PDFInfo
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- CN102358697B CN102358697B CN 201110201023 CN201110201023A CN102358697B CN 102358697 B CN102358697 B CN 102358697B CN 201110201023 CN201110201023 CN 201110201023 CN 201110201023 A CN201110201023 A CN 201110201023A CN 102358697 B CN102358697 B CN 102358697B
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Abstract
The invention relates to a preparation method for alumina based long fiber containing a mullite crystal phase. The preparation method comprises preparing a basic aluminum chloride sol, a precursor sol, a spinnable sol, original alumina based long fiber and the alumina based long fiber containing the mullite crystal phase, and has advantages of easy preparation and low cost. The prepared long fiber has advantages of long length, small diameter, high strength and good softness.
Description
Technical field
The present invention relates to a kind of reinforcement of matrix material, be specifically related to contain mullite and the long stapled method of aluminum oxide crystalline phase a kind of the preparation.
Background technology
The alumina base macrofiber is a kind of high-performance ceramic fiber, and its major ingredient is aluminum oxide and silicon-dioxide, and principal mode has staple fibre, macrofiber and fiber polymer.At present, there be Altex series and the continuous fibre of Sumica series and the Saffil series staple fibre of Britain ICI company of the FP of Nextel series macrofiber, E.I.Du Pont Company of 3M company and PRD-166 series macrofiber, Japanese Sumitomo company in the preparation alumina base long stapled company of open report.The preparation method of its fiber is difference to some extent also, as the FP fiber type of E.I.Du Pont Company, with α-Al of 15 μ m
2O
3Micro mist and Al
2(OH)
5Cl2H
2O and a small amount of MgCl
2Be made into gelating soln, after reaching certain viscosity, be spun into continuous mullite continuous fiber.In 1500 ℃ of oxyhydrogen flames, calcining forms mullite fiber through the several seconds; The handy sol-gel method production of Nextel series fiber of 3M company, it is to contain HCOO-and CH
3The aluminium colloidal sol of the negatively charged ion such as COO-mixes by suitable proportion with silica gel and boric acid, the concentrated suitable spinning solution of viscosity that makes under certain condition, through the spinning-drawing machine wire drawing become continuous fibre (US 4,047,965; Johnson, D.D Nextel 312ceramic fiber from 3M.J.Coated fabrics, 1981,11,282-296); The Safill series staple fibre of the ICI company of Britain is with Al
2(OH)
5Cl2H
2O or Al
2(OH)
5Cl2H
2The O aqueous solution mixes with water miscible organosilane, and adds polyvinyl alcohol, forms spinnable colloidal sols, and the spinning solution high velocity air is jetted into the cotton shape staple fibre, and in thermal treatment below 1000 ℃, obtains polymorph A l
2O
3Fiber (US 4,320,074).
The FP fiber type that E.I.Du Pont Company obtains, its diameter is large, and intensity is low, is unsuitable for industrial production; And the fiber that the ICI company of Britain obtains is staple fibre, without continuity; The Nextel series fiber of 3M company is owing to having adopted advanced industrial means, and fibre property is good, but the preparation trouble, and the too much organic over-all properties of having damaged to a great extent fiber that is added in.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide contain mullite and the long stapled method of aluminum oxide crystalline phase a kind of the preparation, this contains mullite and aluminum oxide crystalline phase macrofiber and has that preparation is easy, with low cost, length is long, diameter is little, and has advantages of that intensity is high, flexibility good.
To achieve these goals, the technical solution used in the present invention is:
Contain mullite and the long stapled method of aluminum oxide crystalline phase a kind of the preparation, comprises the steps:
Step 1: preparation aluminium chlorohydroxide colloidal sol: with molecular formula be at first: [Al
2(OH)
nCl
6-n]
m, the polymerize aluminum chloride of 0＜n＜6 is soluble in water, then with the 1:2-6 mixing in molar ratio of Al powder, with mixing solutions return stirring 4-10h at 40-90 ℃ of temperature, obtains aluminium chlorohydroxide colloidal sol at last;
Step 2: the preparation precursor sol: at first acidic silicasol is added in the aluminium chlorohydroxide colloidal sol that step 1 prepares, the add-on of acidic silicasol is with SiO
2The content 1-35% that accounts for the quality of burning till fiber convert, stir 0.5-5h, obtain two-phase colloidal sol, then add the high molecular polymer spin finish aid in this two-phase colloidal sol, high molecular polymer spin finish aid addition accounts for Al in the macrofiber that finally burns till
2O
3The 2%-12% of quality stirs 0.2-10h, obtains precursor sol;
Step 3: preparation spinnable colloidal sols: the precursor sol that step 2 is obtained obtains spinnable colloidal sols under normal pressure or negative pressure and concentrated polymerization under temperature 20-90 ℃;
Step 4: prepare primary alumina base macrofiber: at first with the spinnable colloidal sols that obtains in step 3, inject the spinning-drawing machine hold-up vessel, after deaeration is processed, then obtain primary alumina base macrofiber through dry-spinning, and reel with cylinder and collect;
Step 5: preparation contains the alumina base macrofiber of mullite crystalline phase: at first the primary alumina base macrofiber heat-up rate with 1-10 ℃/min in air that obtains in step 4 is heated to 1000-1500 ℃, then be incubated 10-60min, obtain containing the alumina base macrofiber of mullite crystalline phase.
The described polymerize aluminum chloride of step 1 is powder or solution state, the purity of described aluminium powder 〉=95%, particle 〉=10 μ m.
The Al of the aluminium chlorohydroxide colloidal sol that step 1 prepares
2O
3The quality percentage composition greater than 20%, pH value is 2-6, basicity 30-90%.
The acidic silicasol pH value that step 2 adds is 1-3.5, contained SiO
2Mass percent is greater than 20%, and particle is 5-20nm.
The high molecular polymer spin finish aid that adds in step 2 is that to be made into mass percent be that the form of the transparent aqueous solution of 1%-10% adds.
The high molecular polymer spin finish aid that adds in step 2 is PVAC polyvinylalcohol, and the polymerization degree is 1700-2400, and alcoholysis degree is 30%-99%.
The pressure range of the described negative pressure of step 3 is 400pa-0.1Mpa.
The viscosity that step 3 obtains spinnable colloidal sols is 0.01-200Pas.
The described dry-spinning pressure of step 4 is 0.13-10.0MPa, and winding speed is 10-100rpm.
Compared with prior art, the invention has the beneficial effects as follows:
1, the fiber that obtains is continuous fibre, the length of its protofibre is greater than 30m, burn till the length of fiber greater than 20m, length considerably beyond the present single fiber of reporting out, and the diameter of the protofibre that obtains is between 1-50 μ m, and its tensile property is good, and flexibility is good, make the present invention can well be applied to suitability for industrialized production, the extremely well-adapted of its technique;
2, this experiment aluminium source used and silicon source can long storage time, generation precipitation or gelation that its aqueous solution can be not spontaneous.In this experiment, various raw materials used all are easy to preparation, and be water-soluble, with respect to pure dissolubility system not only prepare simple and cost also low;
3, add silicon sol and spin finish aid in the colloidal sol in aluminium source after, can be by controlling temperature, the experiment conditions such as negative pressure obtain spinnable colloidal sols fast.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details.
Embodiment one
A kind of mullite and aluminum oxide crystalline phase macrofiber of containing of the present embodiment, its crystalline structure is comprised of mullite and two kinds of crystalline forms of aluminum oxide, wherein the mullite crystalline phase accounts for 2.6%, wherein the aluminum oxide crystalline form is unsetting aluminum oxide crystalline form and Alpha-alumina crystalline form, and two kinds of crystal formations are any ratio, and described long stapled protofibre mean diameter is 1 μ m, and length is for surpassing 31m, the diameter that burns till fiber is 0.5 μ m, and length is 21m.
The present embodiment contains mullite and the long stapled method of aluminum oxide crystalline phase a kind of the preparation, comprises the steps:
Step 1: with molecular formula be at first: [Al
2(OH)
nCl
6-n]
mThe polymerize aluminum chloride 339g of 0＜n＜6 is dissolved in 2L distilled water, and pour into 54.5g is housed, particle 10 μ m, purity is to mix in the round-bottomed flask of 95% aluminium powder, and the mol ratio 1:2 of polymerize aluminum chloride and Al powder is then with mixed solution return stirring 10h at 40 ℃ of temperature, obtain aluminium chlorohydroxide colloidal sol, the Al of the aluminium chlorohydroxide colloidal sol that obtains
2O
3The quality percentage composition be 20%, pH value is 6, basicity is 30%-80%;
Step 2: be at first 1 with pH value, contained SiO
2Mass percent is 25%, particle is that the acidic silicasol 6.903ml of 5nm adds in the aluminium chlorohydroxide colloidal sol that step 1 prepares, stir 5h, obtain two-phase colloidal sol, then add PVA in this two-phase colloidal sol, the polymerization degree is 2400, alcoholysis degree is 99%, mass percent is 1% PVA solution 204g, stirs 10h, obtains precursor sol;
Step 3: the precursor sol that step 2 is obtained obtains the transparent uniform spinnable colloidal sols of viscosity 9Pas in normal pressure and concentrated polymerization at 20 ℃ of temperature;
Step 4: at first with the spinnable colloidal sols that obtains in step 3, inject the spinning-drawing machine hold-up vessel, after standing 1h processes by vacuum defoamation, then extrude colloidal sol through spinning top, pressure is 3.0MPa, reels with 10rpm speed and receives silk, obtain mean diameter at 1 μ m, filament length surpasses the protofibre of 31m;
Step 5: at first the protofibre heat-up rate with 1 ℃/min in air that obtains in step 4 is heated to 1500 ℃, then is incubated 10min, the fiber furnace cooling finally obtains containing the alumina base macrofiber of mullite crystalline phase.
The present embodiment contains mullite and the long stapled diameter of aluminum oxide crystalline phase at 0.5 μ m through measuring, length 21m, and density is 3.1g/cm3, tensile strength 2.1GPa, Young's modulus 360GPa.In this fiber, the fiber section is fine and close, smooth surface, and no significant defect, crystal grain crystal formation are mainly Al2O3+Mullite, and crystal grain is at 25nm, and the mullite crystal formation accounts for 2.6%.In this fiber, the quality of alumina mark is 99%, and silicon-dioxide is 1%.Fibre diameter is measured by SEM, and tensile strength and Young's modulus are measured by the micro-force measurement instrument, and crystalline structure and content are measured by XRD analysis.
Embodiment two
A kind of mullite and aluminum oxide crystalline phase macrofiber of containing of the present embodiment, its crystalline structure is comprised of the mullite crystalline form, and described long stapled protofibre mean diameter is 5 μ m, and length is for surpassing 50m, and the diameter that burns till fiber is 3 μ m, length is 35m.
The present embodiment contains mullite and the long stapled method of aluminum oxide crystalline phase a kind of the preparation, comprises the steps:
Step 1: with molecular formula be at first: [Al
2(OH)
nCl
6-n]
mThe polymerize aluminum chloride 339g of 0＜n＜6 is dissolved in 2L distilled water, and pour into 109g is housed, particle 15 μ m, purity is to mix in the round-bottomed flask of 99% aluminium powder, and the mol ratio 1:4 of polymerize aluminum chloride and Al powder is then with mixed solution return stirring 6h at 60 ℃ of temperature, obtain aluminium chlorohydroxide colloidal sol, the Al of the aluminium chlorohydroxide colloidal sol that obtains
2O
3The quality percentage composition be 25%, pH value is 4, basicity is 30%-90%;
Step 2: be at first 2 with pH value, contained SiO
2Mass percent is 20%, particle is that the acidic silicasol 398mL of 10nm adds in the aluminium chlorohydroxide colloidal sol that step 1 prepares, stir 0.5h, obtain two-phase colloidal sol, then adding the polymerization degree in this two-phase colloidal sol is 1700, and alcoholysis degree is 30%, and mass percent is 10% PVA solution 367g, stir 0.2h, obtain precursor sol;
Step 3: the precursor sol that step 2 is obtained is in negative pressure 400pa and concentrated polymerization at 90 ℃ of temperature, and obtaining viscosity is the transparent uniform spinnable colloidal sols of 0.01Pas;
Step 4: at first with the spinnable colloidal sols that obtains in step 3, inject the spinning-drawing machine hold-up vessel, after standing 1h processes by vacuum defoamation, then extrude colloidal sol through spinning top, pressure is 0.13MPa, reel with 100rpm speed and receive silk, obtain mean diameter at 5 μ m, filament length surpasses the protofibre of 50m;
Step 5: at first the protofibre heat-up rate with 10 ℃/min in air that obtains in step 4 is added to 1000 ℃, then be incubated 60min, the fiber furnace cooling finally obtains containing the alumina base macrofiber of mullite crystalline phase.
The implementation case contains mullite and the long stapled diameter of aluminum oxide crystalline phase at 3 μ m through measuring, and density is 3.3g/cm3, tensile strength 2.3GPa, Young's modulus 360GPa.In this fiber, the fiber section is fine and close, smooth surface, and no significant defect, crystal grain crystal formation are mainly Al
2O
3+ Mullite, wherein the mullite crystal formation accounts for 99.9%.Crystal grain is at 24nm, and wherein aluminum oxide accounts for 72%, and silicon-dioxide accounts for 18%.Fibre diameter is measured by SEM, and tensile strength and Young's modulus are measured by the micro-force measurement instrument, and crystalline structure is measured by XRD analysis.
Embodiment three
A kind of mullite and aluminum oxide crystalline phase macrofiber of containing of the present embodiment, its crystalline structure is comprised of mullite and two kinds of crystalline forms of aluminum oxide, wherein the mullite crystalline form accounts for 99.9%, wherein the aluminum oxide crystalline form is the Alpha-alumina crystalline form, its protofibre mean diameter of described macrofiber is 40 μ m, length is for surpassing 150m, and the diameter that burns till fiber is 30 μ m, and length is 120m.
The present embodiment contains mullite and the long stapled method of aluminum oxide crystalline phase a kind of the preparation, comprises the steps:
Step 1: with molecular formula be at first: [Al
2(OH)
nCl
6-n]
mThe polymerize aluminum chloride 339g of 0＜n＜6 is dissolved in 2L distilled water, and pour into 163.5g is housed, particle 200 μ m, purity is to mix in the round-bottomed flask of 99.8% aluminium powder, and the mol ratio 1:6 of polymerize aluminum chloride and Al powder is then with mixed solution return stirring 4h at 90 ℃ of temperature, obtain aluminium chlorohydroxide colloidal sol, the Al of the aluminium chlorohydroxide colloidal sol that obtains
2O
3The quality percentage composition be 20%, pH value is 6, basicity is 60%-90%;
Step 2: be at first 3.5 with pH value, contained SiO
2Mass percent is 25%, particle is that the acidic silicasol 736mL of 20nm adds in the aluminium chlorohydroxide colloidal sol that step 1 prepares, stir 1h, obtain two-phase colloidal sol, then adding the polymerization degree in this two-phase colloidal sol is 2000, and alcoholysis degree is 88%, and mass percent is 5% PVA solution 408g, stir 6h, obtain colloidal sol;
Step 3: the colloidal sol that step 2 is obtained is in negative pressure 5000pa and concentrated polymerization at 80 ℃ of temperature, and obtaining viscosity is the transparent uniform spinnable colloidal sols of 0.9Pas;
Step 4: at first with the spinnable colloidal sols that obtains in step 3, inject the spinning-drawing machine hold-up vessel, after standing 1h processes by vacuum defoamation, then extrude colloidal sol through spinning top, pressure is 5.0MPa, reel with 60rpm speed and receive silk, obtain mean diameter at 40 μ m, filament length surpasses the protofibre of 150m;
Step 5: at first the protofibre heat-up rate with 3 ℃/min in air that obtains in step 4 is added to 1200 ℃, then be incubated 30min, the fiber furnace cooling finally obtains containing the alumina base macrofiber of mullite crystalline phase.
The implementation case contains the diameter of mullite and aluminum oxide crystalline phase fiber at 30 μ m through measuring, and density is 3.25g/cm3, tensile strength 3.6GPa, Young's modulus 376GPa.In this fiber, the fiber section is fine and close, smooth surface, and no significant defect, crystal grain crystal formation are mainly Al
2O
3+ Mullite, wherein the mullite crystal formation accounts for 99.9%.Crystal grain is at 24nm, and wherein aluminum oxide accounts for 65%, and silicon-dioxide accounts for 35%.Fibre diameter is measured by SEM, and tensile strength and Young's modulus are measured by the micro-force measurement instrument, and crystalline structure is measured by XRD analysis.
Embodiment four
A kind of mullite and aluminum oxide crystalline phase macrofiber of containing of the present embodiment, its crystalline structure is comprised of mullite and two kinds of crystalline forms of aluminum oxide, wherein the mullite crystalline phase accounts for 53.57%, wherein the aluminum oxide crystalline form is unsetting aluminum oxide crystalline form and Alpha-alumina crystalline form, and two kinds of crystal formations are any ratio, and its protofibre mean diameter of described macrofiber is 50 μ m, and length is for surpassing 40m, the diameter that burns till fiber is 40 μ m, and length is 30m.
The present embodiment contains mullite and the long stapled method of aluminum oxide crystalline phase a kind of the preparation, comprises the steps:
Step 1: with molecular formula be at first: [Al
2(OH)
nCl
6-n]
mThe polymerize aluminum chloride 339g of 0＜n＜6 is dissolved in 2L distilled water, and pour into 109g is housed, particle 500 μ m, purity is to mix in the round-bottomed flask of 96% aluminium powder, and the mol ratio 1:4 of polymerize aluminum chloride and Al powder is then with mixed solution return stirring 8h at 60 ℃ of temperature, obtain aluminium chlorohydroxide colloidal sol, the Al of the aluminium chlorohydroxide colloidal sol that obtains
2O
3The quality percentage composition be 20%, pH value is 3, basicity is 50%-90%;
Step 2: be at first 3 with pH value, contained SiO
2Mass percent is 30%, particle is that the acidic silicasol 180mL of 13nm adds in the aluminium chlorohydroxide colloidal sol that step 1 prepares, stir 1h, obtain two-phase colloidal sol, then add PVA in this two-phase colloidal sol, the polymerization degree is 2200, alcoholysis degree is 88%, massfraction is 5% PVA solution 428g, stirs 4h, obtains precursor sol;
Step 3: the precursor sol that step 2 is obtained concentrates polymerization at negative pressure 0.09Mpa and under temperature 60 C, and obtaining viscosity is the transparent uniform spinnable colloidal sols of 200Pas;
Step 4: at first with the spinnable colloidal sols that obtains in step 3, inject the spinning-drawing machine hold-up vessel, after standing 1h processes by vacuum defoamation, then extrude colloidal sol through spinning top, pressure is 10Mpa, reels with 40rpm speed and receives silk, obtain mean diameter at 50 μ m, filament length surpasses the protofibre of 40m;
Step 5: at first the protofibre heat-up rate with 7 ℃/min in air that obtains in step 4 is heated to 1400 ℃, then is incubated 20min, the fiber furnace cooling finally obtains containing the alumina base macrofiber of mullite crystalline phase.
The implementation case contains mullite crystalline substance and the long stapled diameter of aluminum oxide crystalline phase at 40 μ m through measuring, and density is 3.01g/cm
3, tensile strength 2.0GPa, Young's modulus 350GPa.In this fiber, the fiber section is fine and close, smooth surface, and no significant defect, crystal grain crystal formation are mainly Al
2O
3+ Mullite, wherein the mullite crystal formation accounts for 53.57%.Crystal grain is at 31nm, and wherein aluminum oxide accounts for 85%, and silicon-dioxide accounts for 15%.Fibre diameter is measured by SEM, and tensile strength and Young's modulus are measured by the micro-force measurement instrument, and crystalline structure is measured by XRD analysis.
Claims (9)
1. one kind prepares and contains mullite and the long stapled method of aluminum oxide crystalline phase, comprises the steps:
Step 1: preparation aluminium chlorohydroxide colloidal sol: with molecular formula be at first: [Al
2(OH)
nCl
6-n]
m, the polymerize aluminum chloride of 0＜n＜6 is soluble in water, then with the 1:2-6 mixing in molar ratio of Al powder, with mixing solutions return stirring 4-10h at 40-90 ℃ of temperature, obtains aluminium chlorohydroxide colloidal sol at last;
Step 2: the preparation precursor sol: at first acidic silicasol is added in the aluminium chlorohydroxide colloidal sol that step 1 prepares, the add-on of acidic silicasol is with SiO
2The content 1-35% that accounts for the quality of burning till fiber convert, stir 0.5-5h, obtain two-phase colloidal sol, then add the high molecular polymer spin finish aid in this two-phase colloidal sol, high molecular polymer spin finish aid addition accounts for Al in the macrofiber that finally burns till
2O
3The 2%-12% of quality stirs 0.2-10h, obtains precursor sol;
Step 3: preparation spinnable colloidal sols: the precursor sol that step 2 is obtained obtains spinnable colloidal sols under normal pressure or negative pressure and concentrated polymerization under temperature 20-90 ℃;
Step 4: prepare primary alumina base macrofiber: at first with the spinnable colloidal sols that obtains in step 3, inject the spinning-drawing machine hold-up vessel, after deaeration is processed, then obtain primary alumina base macrofiber through dry-spinning, and reel with cylinder and collect;
Step 5: preparation contains the alumina base macrofiber of mullite crystalline phase: at first the primary alumina base macrofiber heat-up rate with 1-10 ℃/min in air that obtains in step 4 is heated to 1000-1500 ℃, then be incubated 10-60min, obtain containing the alumina base macrofiber of mullite crystalline phase.
2. method according to claim 1, it is characterized in that: the described polymerize aluminum chloride of step 1 is powder or solution state, the purity of described aluminium powder 〉=95%, particle 〉=10 μ m.
3. method according to claim 1, is characterized in that: its Al of aluminium chlorohydroxide colloidal sol that step 1 prepares
2O
3The quality percentage composition greater than 20%, pH value is 2-6, basicity 30-90%.
4. method according to claim 1, it is characterized in that: the acidic silicasol pH value that step 2 adds is 1-3.5, contained SiO
2Mass percent is greater than 20%, and particle is 5-20nm.
5. method according to claim 1 is characterized in that: the high molecular polymer spin finish aid that adds in step 2 is that to be made into mass percent be that the form of the transparent aqueous solution of 1%-10% adds.
6. method according to claim 1 or 5, it is characterized in that: the high molecular polymer spin finish aid that adds in step 2 is PVAC polyvinylalcohol, and the polymerization degree is 1700-2400, and alcoholysis degree is 30%-99%.
7. method according to claim 1, it is characterized in that: the pressure range of the described negative pressure of step 3 is 400pa-0.1Mpa.
8. method according to claim 1, it is characterized in that: it is 0.01-200Pas that step 3 obtains spinnable colloidal sols viscosity.
9. method according to claim 1, it is characterized in that: the described dry-spinning pressure of step 4 is 0.13-10.0MPa, and winding speed is 10-100rpm.
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| CN102978745B (en) * | 2012-11-28 | 2014-11-05 | 西安交通大学 | Preparation method of alumina-based continuous long fiber containing mullite whisker second phase |
| CN103614808B (en) * | 2013-10-24 | 2015-05-27 | 西安交通大学 | Mullite fiber with villous whisker and preparation method thereof |
| CN104086200B (en) * | 2014-07-22 | 2017-03-22 | 南京理工宇龙新材料科技有限公司 | Preparation method of mullite fiber |
| CN105316786A (en) * | 2015-12-01 | 2016-02-10 | 仇颖超 | Preparation method of creep-resisting polycrystalline mullite fiber modified ultra-high-molecular-weight polyethylene fibers |
| CN110078482A (en) * | 2019-05-21 | 2019-08-02 | 山东大学 | A kind of α-Al2O3The preparation method of/mullite Multiphase ceramic fibre |
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