CN108358458A - A kind of cerium dopping iron phosphate alkali-resistant glass fibre and preparation method thereof - Google Patents
A kind of cerium dopping iron phosphate alkali-resistant glass fibre and preparation method thereof Download PDFInfo
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- CN108358458A CN108358458A CN201810193604.0A CN201810193604A CN108358458A CN 108358458 A CN108358458 A CN 108358458A CN 201810193604 A CN201810193604 A CN 201810193604A CN 108358458 A CN108358458 A CN 108358458A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
- C03C13/001—Alkali-resistant fibres
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/022—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from molten glass in which the resultant product consists of different sorts of glass or is characterised by shape, e.g. hollow fibres, undulated fibres, fibres presenting a rough surface
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Abstract
The invention discloses a kind of cerium dopping iron phosphate alkali-resistant glass fibres and preparation method thereof.Belong to rare earth doping phosphoric acid salt alkali-proof glass technical field.By raw material P2O5、Fe2O3、CaCO3、CeO2It is sufficiently mixed after being homogenized and melts, draws out cerium dopping Iron phosphate Glasses fiber.Fiberglass component indicates with the molar percentage that oxide converts, P2O545 ~ 60%, Fe2O327 ~ 42%, CaO 2 ~ 15%, CeO21 ~ 6%.The present invention is by optimizing phosphate glass component proportion, while ensureing glass ingredient purity, improves glass fiber high-temperature viscosity and alkaline resistance properties, obtaining low cost with traditional alkali-free glass fibre（E glass fibres）The comparable cerium dopping iron phosphate alkali-resistant glass fibre of alkali resistance is applied to resin composite materials etc. mainly as matrix reinforcing material and requires field to anticorrosive.
Description
Technical field
The invention belongs to rare earth doping phosphoric acid salt glass technology fields, specifically, are related to a kind of good forming ability, alkali resistance
Excellent a kind of cerium dopping iron phosphate alkali-resistant glass fibre and preparation method thereof.
Background technology
Alkali-resistant glass fibre is a kind of novel inorganic nonmetallic materials with excellent corrosion protection and mechanical performance.Using
Its alkaline resistance properties and excellent mechanical performance, alkali-resistant glass fibre can be used as reinforcing material in glass concrete
（GRC）, battery separator etc. require have practicability in resistant material, have a good application prospect.Alkaline resistance properties is preferable at present
Glass fibre be silicate alkali-resistant glass fibre, generally with high-silicon high zirconium component characteristic so that in glass fibre
Glass melting temperature in preparation process is high, and the operation temperature of wire drawing is high, while high temperature shortens the platinum bushing plate service life.Production technology it is tight
It is severe to keep fiber overall cost higher, limit the popularization and application of alkali-resistant glass fibre.
The current existing alkaline-resisting effect of silicate alkali-resisting glass fiber is preferable, but expensive, limits its popularization and application.Pass through
The alkali-resisting glass fiber that price is low and performance is good is developed, can solve the problems, such as this.For improving glass fibre chemistry stability and dropping
The cost of low glass fibre can improve the knot of glass by finding new system or mixing different oxide and its content
Structure and performance.The glass transition temperature and melting temperature of phosphate glass are relatively low, are led in solidification of radwaste, fast ion
There is extensive use in the fields such as body, glass and metalwork sealant.Since there are a double bonds in phosphatic structure so that
Ring molecule can be formed in its structure.Isolated ring molecule makes glass structure have good mobility, cause its is water-fast,
Alkalinity and thermal stability etc. are poor with magma cell.When phosphate glass fibre is immersed in lye, by lye
The principle of erosion is the cation of phosphate chain end by aquation, OH-The tetrahedral skeleton of phosphorus oxygen can be destroyed, orthophosphoric acid is generated
Salt simultaneously gradually dissolves.The chemical stability of glass generally has several determinants, such as the chemical composition of glass, heat treatment side
Formula and surface prescription formula.In terms of chemical composition, there is scholar the study found that with the big ion of the small field strength of a small amount of ionic radius
Instead of being conducive to reinforce glass network；When introducing some oxides in phosphorus oxide glass, it can be used as Network former or
Ectosome participates in the formation of glass.Such as a certain range introduces Fe in phosphate2O3It can form and be similar to [SiO4] structure
[FePO4] structure, so that chain structure is become rack-like structure, the chemical stability of glass can be improved.
Invention content
The present invention harsh, high cost problem for current high-silicon high zirconium alkali-resistant glass fibre production technology, provides one kind
Cerium dopping iron phosphate alkali-resistant glass fibre and preparation method thereof.Alkali-resistant glass fibre of the present invention belongs to iron phosphate glass
Glass system, this patent is in P2O5-Fe2O3-CaO-CeO2On the basis of system components, the ratio between adjusting and optimizing each component is led to
Cross restriction P2O5、Fe2O3, CaO, CeO each component content, improve its alkali resistance, thermal stability simultaneously, reduce crystallization rate and
Cost.The fiber can be used as fibre reinforced materials, be spiked into the basis material of corrosion-resistant requirement, increase its intensity with it is tough
Property.
Technical solution of the present invention.
A kind of cerium dopping iron phosphate alkali-resistant glass fibre raw material, according to oxide molar ratio meter by following oxide
Composition：
P2O545 ~ 60%；
Fe2O327 ~ 42%；
CaCO32 ~ 15%；
CeO21 ~ 6%；
The above raw material is mixed, is put into high temperature furnace after homogenizing, 3 ~ 7h of melted heat preservation obtains being homogenized clear at 1350 DEG C ~ 1450 DEG C
Glass metal pulls straight then when higher than 15 ~ 25 DEG C or so of forming temperature from casing, and drawing becomes threadiness.
By mole meter, the alkaline earth oxide R in the above raw material2O, R Na, K, total content are less than 0.1%,
SiO2Total content is less than 1.0%, Al2O3Total content is less than 0.3%.
Each composition of raw material purity is more than 98%, and more excellent is that each composition of raw material purity is more than 98.5%.
The above raw material by 1350 ~ 1450 DEG C melt system and clarification after, the glass fibre that finally draws out has following spy
Property：Forming temperature temperature is less than 1280 DEG C, forming temperature-liquidus temperature >=80 DEG C.Sample is in the aqueous slkali of PH=12 ~ 13.2
In, etch 20h is kept the temperature at 90 DEG C, mass loss rate is less than 3.5%；Sample is in pure water solution, 90 DEG C of heat preservation dipping 20h, matter
Amount loss rate is less than 1.00%.
The glass fibre composition of the present invention, is indicated, P with the molar percentage that oxide converts2O545 ~ 60%, Fe2O3
27 ~ 42%, CaO 2 ~ 15%, CeO21 ~ 6%.Wherein P2O5、Fe2O3、CaO、CeO2Total content is 98.5% or more.
The present invention has found by test of many times, under the premise of improving glass alkali resistance and thermal stability, increases CeO2's
Amount can reach conducive to thawing and clarification.
Invention effect：There is a large amount of CeO in a kind of cerium dopping iron phosphate alkali-resistant glass fibre ingredient of this patent2With
Fe2O3And with preferable alkali resistance and lower melt system, forming temperature.Therefore, the alkaline-resisting glass of cerium dopping iron phosphate of this patent
Glass fiber can be used as matrix reinforcing material in the composite material with corrosion-resistant requirement such as battery separator, increasing to matrix
Strong toughening.Simultaneously as fiberizing temperature is relatively low and has good productivity.
Description of the drawings
Fig. 1 is the XRD spectrum of sample example 5.
Fig. 2 is 5 fiber SEM figures of sample example
This patent is described in further detail with specific embodiment below with reference to attached drawing.
Specific implementation mode.
To be better understood from this patent, said below by way of the alkali-resistant glass fibre and preparation method thereof of specific embodiment
It is bright.But it should be noted that this patent content is not limited only to embodiment, embodiment is not construed as the limit to the scope of this patent
It is fixed.First, the effect of glass each component and its content in this patent are defined as illustrating in above range, meanwhile, form model
In enclosing, " % " indicates mole percent, and " ~ " indicates numberical range, refers to using numerical value comprising " ~ " front and back record as lower limiting value, the upper limit
Value.
A kind of cerium dopping iron phosphate alkali-resistant glass fibre requirement glass fibre alkali resistance is excellent.P in glass structure2O5It can
As Network former oxide, glass skeleton is constituted in the form of phosphorus oxygen tetrahedral structure.The P-O-P from configuration aspects, network
Key top angle connects and composes three-dimensional network.P2O5Content can influence the alkaline resistance properties and processability of glass fibre, the excessively few then shape of content
It is reduced at oxide body, causes network structure loose, be unfavorable for glass alkaline resistance properties；Too high levels can then increase cost.This is specially
P in profit2O5Content is in 45 ~ 60%, preferably 50 ~ 60%.
Due to there are a double bond, leading to will produce cyclic structure in its structure in phosphatic structure, increase structure stream
Dynamic property.To improve this architectural characteristic, by adding Fe2O3Structure is improved.In Iron phosphate Glasses, Fe3+It can
Enter phosphate glass network in the form of tetrahedral structure, forms P-O-Fe covalent bonds, enhance its water-fast, alkaline simultaneously, iron phosphorus
Silicate glass remains the relatively low advantage of its fusing point, viscosity, though too high levels can influence the tendency towards devitrification and heat penetration of glass, and it is right
Fiber production is unfavorable, but a certain amount of be added with is conducive to improve glass structure extent of polymerization, and then improves the alkaline-resisting of phosphate glass
Performance.Ferriferous oxide content improves it in 27 ~ 40%, preferably 32 ~ 37% while controlling devitrification of glass in the present invention
Alkaline resistance properties.
In addition, being indicated containing the mole percent to be converted with oxide in this patent, the CaO that content is 2 ~ 15%.As
The alkaline earth oxide CaO of network outer body makes glass be easier to obtain the low glassy state of increased devitrification resistance in melting, contributes to glass
Glass is melted, and alkali resistance and thermal stability are unaffected.Meanwhile appropriate addition, it can be conducive to contain Ca during caustic corrosion
The formation of protective film.CaO can be used as stabilizer, but adding too much, and glass brittleness can be made to increase, and especially be reduced in temperature
In the process.The introducing raw material of CaO is CaCO in this patent3, content is in 2 ~ 15%, preferably 7 ~ 12%.
The CeO for being 1 ~ 6% containing molar content in the present invention2It is added, the addition of high field strength ions can reinforcing glass
Network structure improves its alkali resistance and thermal stability, and CeO2Addition can reduce the bubble in melten glass, to reduce
The generation of doughnut improves fiber quality.A small amount of CeO2Addition, big field strength ion network aggregation effect, be conducive to plus
Strong glass network, but introducing can excessively destroy network structure, increase tendency towards devitrification, lead to the reduction of glass alkali resistance.In the present invention
CeO2Content is in 1 ~ 6%, preferably 1 ~ 3%.
1 ~ 6 raw material of embodiment composition is shown in Table 1
Each sample glass is made according to raw material composition table 1.
By raw material phosphorus pentoxide, di-iron trioxide, calcium carbonate, ceria in above-mentioned table 1, height is put into after cooperation uniformly
3 ~ 7h of heat preservation is melted at 1350 DEG C ~ 1450 DEG C and obtains being homogenized clear glass metal, then higher than forming temperature for warm stove（Molding
Temperature temperature corresponding when viscosity of glass metal being taken to be moored for 1000）It at 15 ~ 25 DEG C or so, pulls straight, is shaped to from casing
Threadiness.Measure sample chemical composition data such as the following table 2.
1 ~ 6 sample analysis chemical composition of embodiment is shown in Table 2
1 ~ 6 sample performance of embodiment is shown in Table 3
Each test specimens are made as follows in table 3.
First, each batch composition is uniform in ratio batch mixing in table 1, it is put into high temperature furnace, is melted and protects at 1350 ~ 1450 DEG C
3 ~ 7h of temperature obtains being homogenized clear glass metal, pours into the high graphite jig of heat conduction rate, obtains the glass containing a small amount of bubble
Test block is placed in and keeps the temperature 2 ~ 4 hours at 550 ~ 650 DEG C and anneal, to eliminate thermal stress by test block.
In this patent, the fibre-forming performance of experiment test fiber is drawn by laboratory monofilament.It will homogenizing, clear melting glass
Glass liquid is supplied in casing, pulls straight fiber from the nozzle of its bottom surface.By scanning electron microscope to the monofilament table that is drawn
Face pattern is observed.Monofilament pattern such as Fig. 2.
Density measurement is carried out to glass test block using Archimedes's drainage, measurement medium is deionized water, is tested normal
Temperature is lower to be carried out.To reduce error, the average value of 3 measurements is taken.
Both bulk glasses are subjected to crushing grinding, obtain 180 ~ 250um of grain diameter and are less than 75um glass powders.To each examination
Sample carries out XRD, scanning, differential thermal, water resistance, alkali resistance, liquidus temperature and forming temperature test analysis.
XRD test analysis is as follows.To glass powder sample（Less than 75um）Material phase analysis is carried out, radiographic source is copper target, test
Condition：Step-length is 0.02,10 ° ~ 80 ° of angle.Test result analysis obtains, and sample occurs without crystallization peak, illustrates all samples
Product are in glassy state.The XRD spectrum of sample example 5 is shown in Fig. 1.
Sweep test measures as follows.One layer of gold is sprayed in sample surfaces（Thickness is about 10nm）Afterwards, it is carried out with scanning electron microscope
Observation.It is found after testing glass fiber single filament surface topography：Glass fiber single filament surfacing, no significant defect, diameter are small
In 20um（Monofilament pattern such as Fig. 2）.
Water resistance measures as follows.It is that 180 ~ 250um samples 3.00g is put into centrifuge tube by grain diameter, injection 30ml is pure
Water, at 90 DEG C etch keep the temperature 20h, be put into 100 DEG C of baking ovens drying after carrying out eccentric cleaning, measure and calculate sample mass loss.
Alkaline resistance properties measures as follows.It is that 180 ~ 250um samples 3.00g is put into centrifuge tube by grain diameter, injection 30ml is mixed
Close aqueous slkali submerge sample, mixed ammonium/alkali solutions by a concentration of 1mol/L NaOH and 0.5mol/L Na2CO3Solution 1:1 volume is mixed
Conjunction obtains.Taken out after etch 20h at 90 DEG C, eccentric cleaning carried out to sample, after be put into 100 DEG C of baking ovens and dry, measure and count
Calculate sample mass loss.
Differential thermal analysis measures as follows.Grain size is put into less than 75um samples in alumina crucible first, by heating process
Sample crucible and thermal change of the comparison crucible in temperature-rise period, detecting Process of absorption or liberation of heat variation in sample temperature-rise period can be
DTA differential thermal analysis collection of illustrative plates upper body is existing.Starting recrystallization temperature can be obtained by energy absorption difference（Tx）, glass transition temperature
(Tg), further thermal stability is analyzed, embodies the variation of structure.
Thermal stability parameter △ T1（△T1=Tx-Tg）Numerical value is bigger, embodies the stronger thermal stability of glass.
Forming temperature measures as follows.It is put into alumina crucible after glass test block is crushed to suitable dimension, it is poor according to DTA
The guidance of heating curve is heated to 1450 DEG C to alumina crucible, obtains molten condition sample, and each sample surveyed by rotary process is viscous
Corresponding temperature, i.e. forming temperature when degree is moored for 1000.
Crystallization ceiling temperature measures as follows.It takes powder sample to be filled into platinum boat, is accumulated to suitable density state.It will
Platinum boat is put into the thermal gradient furnace to heat up in advance（1250 DEG C of maximum temperature）In, keep the temperature 2 ~ 4 hours（Air atmosphere）.By taking-up
Sample is put to be cooled to room temperature in air atmosphere, is determined that position occurs in crystal using petrographic microscope, is recycled heat in thermal gradient furnace
Galvanic couple is determined this position temperature, and then determines crystallization ceiling temperature, i.e. liquidus temperature.
The difference of liquidus temperature and forming temperature（Forming temperature-liquidus temperature）According to the two numerical computations.
By table 1 ~ 3 it is found that the forming temperature for measuring each sample is less than 1280 DEG C, the difference of liquidus temperature and forming temperature is not
Less than 80 DEG C.
The mass loss rate of resistance to water enchroachment (invasion) is less than 1%, and the optimal alkaline-resisting mass loss rate of sample is 0.78%；Alkaline erosion quality is damaged
Mistake rate is less than 3.5%, and optimal sample water resistant quality loss late is 2.85%, the same alkali-free glass fibre of alkaline resistance properties（E glass fibers
Dimension）Quite.
Above-mentioned performance parameter and its assay method are known to the art technology talent.
Industrial applicibility：This patent is illustrated by the above content, can prove a kind of cerium dopping iron of this patent
Phosphate alkali-resistant glass fibre and preparation method thereof has feasibility, is that can be realized by existing production technology.The present invention's
Alkali-resistant glass fibre can be applied preferably in GRC, external-wall heat-insulation material, battery separator etc. require corrosion-resistant environment.
Claims (10)
1. a kind of cerium dopping iron phosphate alkali-resistant glass fibre is formed as glass, it is characterized in that, mole to be converted with oxide
Percentage expression, P2O545 ~ 60%, Fe2O327 ~ 42%, CaO 2 ~ 15%, CeO21 ~ 6%；
Wherein P2O5、Fe2O3、CaO、CeO2Total content is 98.5% or more；
Also, 1=CeO of ratio C2/P2O5It is 0.017 ~ 0.067.
2. alkali-resistant glass fibre as described in claim 1, it is characterized in that, Fe2O3Molar percentage be 39% forming temperature from
1130 DEG C are rapidly increased to 1165 DEG C；Limit Fe2O3/P2O5Molar percentage C2 is 0.49 ~ 0.86, ensures processability.
3. alkali-resistant glass fibre as claimed in claim 2, it is characterized in that, O/P molar ratios C3 is 3.30-3.62.
4. the alkali-resistant glass fibre as described in claim 1-3, it is characterized in that, including FeO and Fe2O3Two oxides, moles hundred
Divide and compares Fe3+/Fe2+≥16.7。
5. alkali-resistant glass fibre as claimed in claim 2 or claim 3, it is characterized in that, be free of fluorine element, high temperature in glass fibre composition
Corresponding temperature is less than 1280 DEG C when viscosity is 1000 pool, forming temperature-liquidus temperature >=80 DEG C.
6. the alkali-resistant glass fibre as described in claim 1-3, it is characterized in that, aqueous slkali of the sample at 90 DEG C（PH=12~13.2）
Middle heat preservation etch 20h, mass loss rate are less than 3.5%.
7. the alkali-resistant glass fibre as described in claim 1-3, it is characterized in that, sample keeps the temperature dipping in 90 DEG C of pure water solutions
20h, mass loss rate are less than 1.00%.
8. a kind of cerium dopping iron phosphate alkali-resistant glass fibre, it is characterized in that, fibre diameter is less than 20um.
9. a kind of cerium dopping iron phosphate alkali-resistant glass fibre preparation method, it is characterized in that, glass fibre is modulated into raw material
Oxide molar percentages contain P2O545 ~ 60%, Fe2O327 ~ 42%, CaCO32 ~ 15%, CeO21 ~ 6%, it is put into height
3 ~ 7h of heat preservation is melted at 1350 DEG C ~ 1450 DEG C and obtains being homogenized clear glass metal, then higher than forming temperature 15 ~ 25 for warm stove
DEG C or so when, pulled straight from casing, be shaped to threadiness.
10. the preparation method of alkali-resistant glass fibre as claimed in claim 9, it is characterized in that, it is raw materials used by mole
Meter includes P2O545 ~ 60%, Fe2O327 ~ 42%, CaCO32 ~ 15%, CeO21 ~ 6%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020139147A1 (en) * | 2001-01-30 | 2002-10-03 | Janas Victor F. | Glass scaffolds with controlled resorption rates and methods for making same |
| US20060093645A1 (en) * | 2001-01-30 | 2006-05-04 | Janas Victor F | Glass scaffolds with controlled resorption rates and methods for making same |
| US20070243991A1 (en) * | 2006-04-18 | 2007-10-18 | Brow Richard K | Alkaline resistant phosphate glasses and method of preparation and use thereof |
-
2018
- 2018-03-09 CN CN201810193604.0A patent/CN108358458A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020139147A1 (en) * | 2001-01-30 | 2002-10-03 | Janas Victor F. | Glass scaffolds with controlled resorption rates and methods for making same |
| US20060093645A1 (en) * | 2001-01-30 | 2006-05-04 | Janas Victor F | Glass scaffolds with controlled resorption rates and methods for making same |
| US20070243991A1 (en) * | 2006-04-18 | 2007-10-18 | Brow Richard K | Alkaline resistant phosphate glasses and method of preparation and use thereof |
Non-Patent Citations (1)
| Title |
|---|
| JIAWANJUN SHI: "《University of Missouri-Rolla Masters Theses》", 31 December 2007 * |
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Application publication date: 20180803 |