CN107285627A - A kind of fluoride glass and preparation method thereof - Google Patents
A kind of fluoride glass and preparation method thereof Download PDFInfo
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- CN107285627A CN107285627A CN201710616513.9A CN201710616513A CN107285627A CN 107285627 A CN107285627 A CN 107285627A CN 201710616513 A CN201710616513 A CN 201710616513A CN 107285627 A CN107285627 A CN 107285627A
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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
- C03C3/00—Glass compositions
- C03C3/32—Non-oxide glass compositions, e.g. binary or ternary halides, sulfides or nitrides of germanium, selenium or tellurium
- C03C3/325—Fluoride glasses
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
- C03B25/02—Annealing glass products in a discontinuous way
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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
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/80—Non-oxide glasses or glass-type compositions
- C03B2201/82—Fluoride glasses, e.g. ZBLAN glass
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Abstract
The invention discloses a kind of fluoride glass and preparation method thereof, fluoride glass includes the ZrF that molar percentage is 16%~70%4, 13%~32% BaF2, 5%~18% MF, 0%~14% MeF2With 0%~28% MfF3, wherein, M is one or both of Na, Li, and Me is the one or more in Zn, Mg, Ca, and Mf is one or both of Al, La.The low cost of the fluoride glass of the present invention, it is adaptable in the optical window of near ultraviolet to middle-infrared band.Gained glass cutoff wavelength of the invention is more than 6um, good into glass properties, is adapted to prepare infrared laser optical fiber and fiber amplifier host glass and other optical materials.The present invention obtains glass with well into glass properties, and good chemical stability, theoretical loss is low, is adapted to prepare fine and doped fiber the matrix of low loss fluorinated object light.
Description
Technical field
The invention belongs to glass art, more particularly, to a kind of fluoride glass and preparation method thereof.
Background technology
Glass optical fiber using fluoride as main material has the scope (0.2- of broader spectrum compared to traditional optical fiber
7um), and preferably mid-infrared light transmitance, it means that bigger bandwidth can be obtained in the system of fiber optic communication；This
Outside, fluoride glass has low-refraction, high Abbe number and low nonlinearity refractive index, is preferable optical window material and ultra-low loss
Infrared optical material, with larger application value.The optical fiber that such fluoride glass is pulled out, can carry bigger light belt
Width, simultaneously because its extremely low theoretical loss limit (0.001dB/km), in the fiber optic communication of long range, especially transoceanic communication
In have a wide range of applications.Further, since its high-permeability in infrared band, also great latent in infrared acquisition field
Power.
Due to technique and technical reason, prepared by current fluoride glass generally uses a variety of fluorides, also simultaneously
Add the rare elements such as La, Ce；On the other hand, people are in order to reduce in environment OH foundation group to fluoride glass permeability
Influence is much more general to keep drying in glass melting process, nothing by vacuumizing case or by way of waiting and aiding in atmosphere
Oxygen environment, this undoubtedly adds the cost and difficulty that prepare fluoride glass.Current fluoride glass chemical stability is low, reason
It is high by loss height and cost.
As can be seen here, there is the technology that chemical stability is low, theoretical loss is high and cost is high in existing fluoride glass
Problem, the preparation method of existing fluoride glass, which exists, is difficult to economic, the efficient fluoride glass for preparing high transmittance
Technical problem.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of fluoride glass and its preparation side
Method, thus solves existing fluoride glass and there is the technical problem that chemical stability is low, theoretical loss is high and cost is high, and
And the preparation method of existing fluoride glass is solved in the presence of the fluoride glass for being difficult to economy, efficiently preparing high transmittance
The technical problem of glass.
To achieve the above object, according to one aspect of the present invention, there is provided a kind of fluoride glass, including Mole percent
Than the ZrF for 16%~70%4, 13%~32% BaF2, 5%~18% MF, 0%~14% MeF2With 0%~28%
MfF3, wherein, M is one or both of Na, Li, and Me is the one or more in Zn, Mg, Ca, and Mf is one in Al, La
Plant or two kinds.
Further, BaF2Molar percentage be x, 20%≤x≤32%, ZrF4Molar percentage be 2x ± y, and
0%≤y≤40%.
Further, BaF2Molar percentage be x, 20%≤x≤25%, ZrF4Molar percentage be 2x ± y, and
0%≤y≤40%, MF molar percentage is 5%~8%, MeF2Molar percentage be 4%~14%, MfF3Moles hundred
Divide than being 3%~8%.
Further, the molar percentage of fluoride glass is preferably：48%ZrF4, 24%BaF2, 8%NaF, 14%
ZnF2And 6%AlF3。
Further, the molar percentage of fluoride glass is preferably：58%ZrF4, 28%BaF2, 8%NaF, 6%AlF3
Or 60%ZrF4, 30%BaF2, 10%NaF.
It is another aspect of this invention to provide that there is provided a kind of preparation method of fluoride glass, including found, be molded and move back
Firer's sequence, adds the fluorination treatment stage, i.e., in melting process：
Auxiliary reagent NH is added in the 20%-40% ratios of raw material gross mass4HF2, auxiliary reagent be added to raw material it
It is preceding, it is necessary to first carry out heating 10min-40min, temperature be 100 DEG C -200 DEG C, be put into after cooling in raw material, then rise to 320
DEG C -400 DEG C of intervals, NH during this4HF2Thermal decomposition produces hydrogen fluoride and ammonia atmosphere, keeps 20min-40min；Then, protect
Fluorination atmosphere is held, 850 DEG C -1200 DEG C interval heating 30min-40min is warming up to, completes melting process.
Further, annealing operation is：Mould is placed in 100 DEG C of -250 DEG C of Muffle furnaces, 10min- is individually preheated
30min, makes the full and uniform heating of mould；After after raw material completely melting, glass metal is poured into mould rapidly, melted down, 100
Stop heating after heating 30min-100min at DEG C -250 DEG C, allow mould and glass metal to naturally cool to room temperature.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show
Beneficial effect：
(1) dispensing that the present invention is used is fewer, and just glass can be made using minimum three kinds of compounds, reduces rare earth member
The use of element, while using these three compounds as ultimate constituent, addition other compositions can also be fabricated to glass, improve
Transmitance.
(2) low cost of fluoride glass of the invention, it is adaptable in the optical window of near ultraviolet to middle-infrared band.This
Invention gained glass cutoff wavelength is more than 6um, good into glass properties, is adapted to prepare infrared laser optical fiber and fiber amplifier matrix
Glass and other optical materials.The present invention obtains glass with good into glass properties, and good chemical stability, theory is damaged
Consumption is low, is adapted to prepare fine and doped fiber the matrix of low loss fluorinated object light.
(3) present invention first heats fluorination reagent, can remove the moisture mixed in raw material so that the absworption peak drop of hydroxyl
It is low, improve the transmitance of fluoride glass.The selection of annealing temperature of the present invention can reduce the crystallization of glass, can produce big
The fluoride glass of size.
Brief description of the drawings
Fig. 1 be fluoride glass provided in an embodiment of the present invention near ultraviolet to the transmittance curve to middle-infrared band
Figure.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Not constituting conflict each other can just be mutually combined.
The embodiments of the invention provide a kind of fluoride glass, including the ZrF that molar percentage is 16%~70%4、
13%~32% BaF2, 5%~18% MF, 0%~14% MeF2With 0%~28% MfF3, wherein, M is Na, Li
One or both of, Me is the one or more in Zn, Mg, Ca, and Mf is one or both of Al, La.
The embodiment of the present invention is preferred, BaF2Molar percentage be x, 20%≤x≤32%, ZrF4Molar percentage
For 2x ± y, and 0%≤y≤40%.
The embodiment of the present invention is preferred, BaF2Molar percentage be x, 20%≤x≤25%, ZrF4Molar percentage
It is 5%~8%, MeF for 2x ± y, and 0%≤y≤40%, MF molar percentage2Molar percentage be 4%~14%,
MfF3Molar percentage be 3%~8%.
Several groups of composition of raw materials involved in embodiment are given below, it is necessary to particularly point out：The present invention relates to formula rate,
Use molar percentage.1-10 of embodiment of the present invention formula is as shown in table 1 below.
Table 1
Embodiment 1
The molar percentage of frit is respectively 16%ZrF4, 24%BaF2, 16%NaF, 2%LiF, 10%ZnF2、
2%MgF2, 2%CaF2, 24%AlF3And 4%LaF3, auxiliary reagent NH is added in 20% ratio of frit gross mass4HF2,
Auxiliary reagent is, it is necessary to first carry out heating 10min before raw material is added to, and temperature is 200 DEG C, is put into after cooling in raw material,
Then 320 DEG C of intervals, NH during this are risen to4HF2Thermal decomposition produces hydrogen fluoride and ammonia atmosphere, keeps 40min；Then, keep
Atmosphere is fluorinated, 850 DEG C of interval heating 40min is warming up to, completes melting process.Mould is placed in 100 DEG C of Muffle furnaces, individually
30min is preheated, makes the full and uniform heating of mould；After after raw material completely melting, glass metal is poured into mould rapidly, melted down,
Heated at 100 DEG C and stop heating after 100min, allow mould and glass metal to naturally cool to room temperature.Obtained fluoride glass exists
The transmitance of middle-infrared band reaches 75%.
Embodiment 2
The molar percentage of frit is respectively 70%ZrF4, 20%BaF2, 5%NaF and 5%AlF3, by frit
30% ratio of gross mass adds auxiliary reagent NH4HF2, auxiliary reagent is before raw material is added to, it is necessary to first be heated
20min, temperature is 180 DEG C, is put into after cooling in raw material, then rises to 350 DEG C of intervals, NH during this4HF2Thermal decomposition production
Raw hydrogen fluoride and ammonia atmosphere, keep 30min；Then, fluorination atmosphere is kept, 950 DEG C of interval heating 30min is warming up to, completes
Melting process.Mould is placed in 150 DEG C of Muffle furnaces, 20min is individually preheated, makes the full and uniform heating of mould；Treat that raw material is complete
After full-fusing, glass metal is poured into mould rapidly, melted down, at 150 DEG C heat 80min after stop heating, allow mould and
Glass metal naturally cools to room temperature.Obtained fluoride glass reaches 64% in the transmitance of middle-infrared band.
Embodiment 3
The molar percentage of frit is respectively 58%ZrF4, 32%BaF2, 5%NaF and 5%LiF, by frit
40% ratio of gross mass adds auxiliary reagent NH4HF2, auxiliary reagent is before raw material is added to, it is necessary to first be heated
40min, temperature is 100 DEG C, is put into after cooling in raw material, then rises to 400 DEG C of intervals, NH during this4HF2Thermal decomposition production
Raw hydrogen fluoride and ammonia atmosphere, keep 20min；Then, fluorination atmosphere is kept, 1200 DEG C of interval heating 20min is warming up to, completes
Melting process.Mould is placed in 250 DEG C of Muffle furnaces, 10min is individually preheated, makes the full and uniform heating of mould；Treat that raw material is complete
After full-fusing, glass metal is poured into mould rapidly, melted down, at 250 DEG C heat 30min after stop heating, allow mould and
Glass metal naturally cools to room temperature.Obtained fluoride glass reaches 65% in the transmitance of middle-infrared band.
Embodiment 4
The molar percentage of frit is respectively 48%ZrF4, 13%BaF2, 18%NaF, 7%MgF2, 10%AlF3With
4%LaF3, auxiliary reagent NH is added in 25% ratio of frit gross mass4HF2, auxiliary reagent before raw material is added to,
Need first to carry out heating 30min, temperature is 130 DEG C, is put into raw material after cooling, then rises to 360 DEG C of intervals, during this
NH4HF2Thermal decomposition produces hydrogen fluoride and ammonia atmosphere, keeps 28min；Then, fluorination atmosphere is kept, 1050 DEG C of intervals are warming up to
30min is heated, melting process is completed.Mould is placed in 100 DEG C of Muffle furnaces, 30min is individually preheated, makes mould full and uniform
Heating；After after raw material completely melting, glass metal is poured into mould rapidly, melted down, heated and stop after 100min at 100 DEG C
Heating, allows mould and glass metal to naturally cool to room temperature.Obtained fluoride glass reaches in the transmitance of middle-infrared band
73%.
Embodiment 5
The molar percentage of frit is respectively 56%ZrF4, 28%BaF2, 8%NaF, 2%ZnF2, 3%AlF3With
3%LaF3, auxiliary reagent NH is added in 20% ratio of frit gross mass4HF2, auxiliary reagent before raw material is added to,
Need first to carry out heating 10min, temperature is 200 DEG C, is put into raw material after cooling, then rises to 320 DEG C of intervals, during this
NH4HF2Thermal decomposition produces hydrogen fluoride and ammonia atmosphere, keeps 40min；Then, fluorination atmosphere is kept, 850 DEG C of intervals is warming up to and adds
Hot 40min, completes melting process.Mould is placed in 100 DEG C of Muffle furnaces, 30min is individually preheated, makes mould is full and uniform to add
Heat；After after raw material completely melting, glass metal is poured into mould rapidly, melted down, heated at 100 DEG C and stop adding after 100min
Heat, allows mould and glass metal to naturally cool to room temperature.Obtained fluoride glass reaches 66% in the transmitance of middle-infrared band.
Embodiment 6
The molar percentage of frit is respectively 58%ZrF4, 28%BaF2, 8%NaF and 6%AlF3, by frit
20% ratio of gross mass adds auxiliary reagent NH4HF2, auxiliary reagent is before raw material is added to, it is necessary to first be heated
10min, temperature is 200 DEG C, is put into after cooling in raw material, then rises to 320 DEG C of intervals, NH during this4HF2Thermal decomposition production
Raw hydrogen fluoride and ammonia atmosphere, keep 40min；Then, fluorination atmosphere is kept, 850 DEG C of interval heating 40min is warming up to, completes
Melting process.Mould is placed in 100 DEG C of Muffle furnaces, 30min is individually preheated, makes the full and uniform heating of mould；Treat that raw material is complete
After full-fusing, glass metal is poured into mould rapidly, melted down, at 100 DEG C heat 100min after stop heating, allow mould and
Glass metal naturally cools to room temperature.Obtained fluoride glass reaches 76% in the transmitance of middle-infrared band.
Embodiment 7
The molar percentage of frit is respectively 48%ZrF4, 24%BaF2, 8%NaF, 14%ZnF2And 6%AlF3,
Auxiliary reagent NH is added in 20% ratio of frit gross mass4HF2, auxiliary reagent is before raw material is added to, it is necessary to advanced
Row heating 10min, temperature is 200 DEG C, is put into after cooling in raw material, then rises to 320 DEG C of intervals, NH during this4HF2Heat
Decompose and produce hydrogen fluoride and ammonia atmosphere, keep 40min；Then, fluorination atmosphere is kept, 850 DEG C of interval heating are warming up to
40min, completes melting process.Mould is placed in 100 DEG C of Muffle furnaces, 30min is individually preheated, makes mould is full and uniform to add
Heat；After after raw material completely melting, glass metal is poured into mould rapidly, melted down, heated at 100 DEG C and stop adding after 100min
Heat, allows mould and glass metal to naturally cool to room temperature.Obtained fluoride glass reaches 86% in the transmitance of middle-infrared band.
Embodiment 8
The molar percentage of frit is respectively 60%ZrF4, 30%BaF2And 10%NaF, by frit gross mass
20% ratio add auxiliary reagent NH4HF2, auxiliary reagent is before raw material is added to, it is necessary to first carry out heating 10min, temperature
For 200 DEG C, it is put into after cooling in raw material, then rises to 320 DEG C of intervals, NH during this4HF2Thermal decomposition produce hydrogen fluoride and
Ammonia atmosphere, keeps 40min；Then, fluorination atmosphere is kept, 850 DEG C of interval heating 40min is warming up to, completes melting process.Will
Mould is placed in 100 DEG C of Muffle furnaces, individually preheats 30min, makes the full and uniform heating of mould；, will after raw material is melted completely
Glass metal is poured into mould rapidly, is melted down, and is heated at 100 DEG C and is stopped heating after 100min, makes mould and glass metal natural
It is cooled to room temperature.Obtained fluoride glass reaches 62% in the transmitance of middle-infrared band.
Embodiment 9
The molar percentage of frit is respectively 61%ZrF4, 30%BaF2, 5%NaF, 2%LiF and 2%AlF3, press
20% ratio of frit gross mass adds auxiliary reagent NH4HF2, auxiliary reagent is before raw material is added to, it is necessary to first carry out
10min is heated, temperature is 200 DEG C, is put into after cooling in raw material, then rises to 320 DEG C of intervals, NH during this4HF2Heat point
Solution produces hydrogen fluoride and ammonia atmosphere, keeps 40min；Then, fluorination atmosphere is kept, 850 DEG C of interval heating 40min are warming up to,
Complete melting process.Mould is placed in 100 DEG C of Muffle furnaces, 30min is individually preheated, makes the full and uniform heating of mould；Treat original
After material melting completely, glass metal is poured into mould rapidly, melted down, heated at 100 DEG C and stop heating after 100min, allow mould
Tool and glass metal naturally cool to room temperature.Obtained fluoride glass reaches 66% in the transmitance of middle-infrared band.
Embodiment 10
The molar percentage of frit is respectively 58%ZrF4, 25%BaF2, 5%LiF, 4%MgF2And 8%AlF3,
Auxiliary reagent NH is added in 20% ratio of frit gross mass4HF2, auxiliary reagent is before raw material is added to, it is necessary to advanced
Row heating 10min, temperature is 200 DEG C, is put into after cooling in raw material, then rises to 320 DEG C of intervals, NH during this4HF2Heat
Decompose and produce hydrogen fluoride and ammonia atmosphere, keep 40min；Then, fluorination atmosphere is kept, 850 DEG C of interval heating are warming up to
40min, completes melting process.Mould is placed in 100 DEG C of Muffle furnaces, 30min is individually preheated, makes mould is full and uniform to add
Heat；After after raw material completely melting, glass metal is poured into mould rapidly, melted down, heated at 100 DEG C and stop adding after 100min
Heat, allows mould and glass metal to naturally cool to room temperature.Obtained fluoride glass reaches 76% in the transmitance of middle-infrared band.
Choose excellent formula therein glass print grind after carry out optical performance test (FTIR tests).Such as table 2 below institute
Show.
Table 2
| Formula | Formula composition |
| a | 48%ZrF4, 24%BaF2, 8%NaF, 14%ZnF2And 6%AlF3 |
| b | 58%ZrF4, 28%BaF2, 8%NaF and 6%AlF3 |
| c | 60%ZrF4, 30%BaF2And 10%NaF |
It is formulated a and corresponds to embodiment 7, formula b corresponds to embodiment 6, and formula c corresponds to embodiment 8, to formula a, b and c
Prepared glass sample is selected, and selects that shape is intact, substantially transparent sample, is ground with 120-7000 abrasive paper for metallograph
Grind and be polished to the bright and clean parallel sheet glass in two sides, it is then right by each formula institute of Fourier's infrared microscopy instrument VERTEX70 tests
The optical transmittance of glass sample is answered, FTIR test result is shown in accompanying drawing 1.A fluoride glass is formulated in middle-infrared band
Transmitance reaches 86%.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not used to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the invention etc., it all should include
Within protection scope of the present invention.
Claims (7)
1. a kind of fluoride glass, it is characterised in that including the ZrF that molar percentage is 16%~70%4, 13%~32%
BaF2, 5%~18% MF, 0%~14% MeF2With 0%~28% MfF3, wherein, M is one kind or two in Na, Li
Kind, Me is the one or more in Zn, Mg, Ca, and Mf is one or both of Al, La.
2. a kind of fluoride glass as claimed in claim 1, it is characterised in that the BaF2Molar percentage be x, 20%
≤ x≤32%, ZrF4Molar percentage be 2x ± y, and 0%≤y≤40%.
3. a kind of fluoride glass as claimed in claim 2, it is characterised in that the BaF2Molar percentage be x, 20%
≤ x≤25%, ZrF4Molar percentage be 2x ± y, and 0%≤y≤40%, MF molar percentage be 5%~8%, MeF2
Molar percentage be 4%~14%, MfF3Molar percentage be 3%~8%.
4. a kind of fluoride glass as described in claim 1-3 is any, it is characterised in that moles the hundred of the fluoride glass
Point ratio is preferably：48%ZrF4, 24%BaF2, 8%NaF, 14%ZnF2And 6%AlF3。
5. a kind of fluoride glass as claimed in claim 1, it is characterised in that the molar percentage of the fluoride glass is excellent
Elect as：58%ZrF4, 28%BaF2, 8%NaF, 6%AlF3Or 60%ZrF4, 30%BaF2, 10%NaF.
6. a kind of preparation method of any described fluoride glasses of claim 1-5, including found, be molded and annealing operation,
Characterized in that, adding the fluorination treatment stage in melting process, i.e.,：
Auxiliary reagent NH is added in the 20%-40% ratios of raw material gross mass4HF2, auxiliary reagent, need to before raw material is added to
First to carry out heating 10min-40min, temperature is 100 DEG C -200 DEG C, is put into after cooling in raw material, then rise to 320 DEG C -
400 DEG C of intervals, NH during this4HF2Thermal decomposition produces hydrogen fluoride and ammonia atmosphere, keeps 20min-40min；Then, fluorine is kept
Change atmosphere, be warming up to 850 DEG C -1200 DEG C interval heating 30min-40min, complete melting process.
7. a kind of preparation method of fluoride glass according to claim 6, it is characterised in that the annealing operation is：
Mould is placed in 100 DEG C of -250 DEG C of Muffle furnaces, 10min-30min is individually preheated, makes the full and uniform heating of mould；Treat raw material
Completely after melting, glass metal is poured into mould rapidly, melted down, stopped after heating 30min-100min at 100 DEG C -250 DEG C
Only heat, allow mould and glass metal to naturally cool to room temperature.
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| CN109900700A (en) * | 2019-04-10 | 2019-06-18 | 南京邮电大学 | The detection method of Silver Clusters in a kind of silicate glass |
| CN109900700B (en) * | 2019-04-10 | 2021-11-12 | 南京邮电大学 | Method for detecting silver clusters in silicate glass |
| CN111146686A (en) * | 2019-12-27 | 2020-05-12 | 华中科技大学 | Near-mid infrared broadband light source based on multilayer special-shaped array hole structure |
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