CN105174689B - A kind of preparation facilities of crucible and especial dispersion glass and preparation method thereof - Google Patents
A kind of preparation facilities of crucible and especial dispersion glass and preparation method thereof Download PDFInfo
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- CN105174689B CN105174689B CN201510662948.8A CN201510662948A CN105174689B CN 105174689 B CN105174689 B CN 105174689B CN 201510662948 A CN201510662948 A CN 201510662948A CN 105174689 B CN105174689 B CN 105174689B
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Abstract
The invention discloses preparation facilities of a kind of crucible and especial dispersion glass and preparation method thereof, wherein crucible includes crucible body and crucible cover, crucible body has the first annular groove for accommodating fluid-tight liquid, crucible cover has the first annular catch being adapted with first annular groove, is filled between crucible cover and crucible body by the insertion of first annular catch and sealing is realized in the first annular groove of fluid-tight liquid；Crucible cover is equipped with charge door, and charge door is equipped with the second annular groove for accommodating fluid-tight liquid for feeding and being passed through gas around charge door on crucible cover；Crucible cover is equipped with exhaust outlet, and exhaust outlet is equipped with the third annular groove for accommodating fluid-tight liquid for discharging gas around exhaust outlet on crucible cover；Crucible cover is equipped with stirring port, is equipped with the fourth annular groove for accommodating fluid-tight liquid on crucible cover around the stirring port；Crucible body bottom is equipped with material leakage pipe.There is higher optical homogeneity and batch consistency by especial dispersion glass prepared by the crucible.
Description
Technical field
The present invention relates to optical glass fields, and in particular to the preparation facilities and system of a kind of crucible and especial dispersion glass
Preparation Method.
Background technology
There are dispersion phenomenon, i.e. refractive index reductions with wavelength increase for optical glass.The difference of any two wavelength refractive rate
Referred to as partial dispersionPartial dispersion and middle part dispersion (nF-nC) ratio be known as relative partial dispersionThe relative partial dispersion of most of optical glass meets Abbe formula with Abbe number ν relationships, similar to
Linear relation, this straight line are referred to as " normal line " of optical glass.Especial dispersion glass is that one kind deviates normal line farther out
Optical glass.Especial dispersion glass not only has the universal performance of optical glass, such as particular optical constant, high optical transmittance, excellent
Different optical homogeneity and good chemical stability etc., but also there is property, i.e., larger relative partial dispersion deviation value,
It is the preferred material of long-focus, big visual field and high-precision optical system.Therefore, carrying out the research of especial dispersion glass not only can be rich
Rich optical glass kind, and with significant application value.
At present, there are mainly two types of the preparation methods of the especial dispersion glass of report：First, the preparation of common oxide glasses
Method carries out high temperature melting using Pt crucibles under atmospheric environment, acquisition is formed after agitated, clarification and homogenization, should
Method is mainly for the preparation of B2O3Content is high, ZrO2The low especial dispersion glass of content, glass melting temperature are less than 1400 DEG C, this is helped
In realization volatile components such as B2O3、Na2O、Ta2O5Deng control；Second is that using high frequency preparation method, i.e., in special high-frequency device
It is interior that glass raw material is melted, it is obtained after clarified and homogenizing by shaping, this method is mainly for the preparation of refractory components
Such as SiO2、ZrO2、HfO2And WO2The especial dispersion glass that equal size is high, volatile fusible component is few, glass melting temperature is higher, can be high
Up to 1800 DEG C.But above two preparation method is difficult to prepare the especial dispersion glass that " volatile components-refractory components " coexist
Glass is low because of volatile components requirement glass smelting temperature, and refractory components requirement glass smelting temperature is high, how to solve
Certainly this, which prepares contradiction, has become the focus of especial dispersion glass research.
Invention content
The preparation facilities of the embodiment of the present application by providing a kind of crucible and especial dispersion glass and preparation method thereof solves
The preparation problem of especial dispersion glass coexists in " volatile components-refractory components " in the prior art, both realizes especial dispersion
The control of volatile components during glass preparation also ensures the abundant melting of refractory components.
In order to achieve the above objectives, present invention generally provides following technical solutions：
On the one hand, the embodiment of the present application provides a kind of crucible, and the crucible includes crucible body and crucible cover, the crucible
On body there is the first annular groove for accommodating fluid-tight liquid, have on the crucible cover and be adapted with the first annular groove
First annular catch, fill the first of fluid-tight liquid by the first annular catch insertion between the crucible cover and crucible body
Sealing is realized in annular groove；
The crucible cover is equipped with charge door, and the charge door surrounds for feeding and being passed through gas on the crucible cover
The charge door is equipped with the second annular groove for accommodating fluid-tight liquid；
The crucible cover is equipped with exhaust outlet, and the exhaust outlet surrounds the row for discharging gas on the crucible cover
Gas port is equipped with the third annular groove for accommodating fluid-tight liquid；
The crucible cover is equipped with stirring port, is equipped with to accommodate fluid-tight liquid around the stirring port on the crucible cover
Fourth annular groove；
The crucible body bottom is equipped with material leakage pipe.
Preferably, the crucible further includes the first plug, first plug has and the second annular groove phase
Second annular baffle of adaptation, the second annular that first plug fills fluid-tight liquid by second annular baffle insertion are recessed
The charge door is sealed in slot.
Preferably, the crucible further includes the second plug, second plug has and the third annular groove phase
The third annular baffle of adaptation, the third annular that second plug fills fluid-tight liquid by third annular baffle insertion are recessed
The exhaust outlet is sealed in slot.
Preferably, the crucible further includes blender, the blender includes rotary shaft and mixing part, the rotary shaft
Across the stirring port, the rotary shaft is equipped with first seal, and the first seal has and fourth annular groove phase
The fourth annular catch of adaptation, the first seal fill the fourth annular of fluid-tight liquid by fourth annular catch insertion
The sealing between blender and crucible cover is realized in groove.
On the other hand, the embodiment of the present application provides a kind of preparation facilities of especial dispersion glass, including crucible, the earthenware
Crucible is above-mentioned crucible.
Preferably, the preparation facilities further includes snorkel, the outer wall of the snorkel is equipped with second seal, institute
Stating second seal has the 5th annular baffle being adapted with the second annular groove, and the second seal passes through described
The insertion of 5th annular baffle fills the sealing realized in the second annular groove of fluid-tight liquid between snorkel outside wall surface and crucible cover.
In addition, the embodiment of the present application additionally provides a kind of preparation method of especial dispersion glass, the method utilizes above-mentioned
Preparation facilities complete, the described method comprises the following steps：
(1) glass raw material weighed is mixed, fusing obtains glass metal；
(2) glass metal is imported into crucible；
(3) after the completion of feeding, oxygen is passed through into crucible, glass metal is stirred under conditions of oxygen is passed through, it is real
The clarification and homogenization of existing glass metal；
(4) after glass metal homogenizing completely, material leakage forming.
Preferably, in the step (2) and the step (3) before material leakage forming is carried out to glass metal, material leakage pipe
Interior temperature is maintained at 1250-1300 DEG C, so that glass metal is solidified in material leakage pipe without leaking out, while prevents glass metal from leaking
Crystallization occurs in expects pipe.
Preferably, before glass metal is imported into crucible, N is used in crucible2、O2, He or Ar gas carry out atmosphere protection.
Preferably, the glass metal that the fluid-tight liquid that the crucible uses is obtained for the step (1).
Preferably, after the completion of charging, oxygen is passed through into crucible and is divided into twice, be passed into oxygen when ventilating for the first time
Under glass metal liquid level；First time starts second of ventilation after ventilating, and oxygen is passed into glass metal liquid when ventilating for the second time
On face, second of ventilation is until glass metal clarification and homogenization.
Preferably, water content≤2ppm of the oxygen；The flow for being passed through oxygen for the first time is 2-6L/min, for the first time
The time for being passed through oxygen is 0.5-3h；The flow for being passed through oxygen for the second time is 0.5-2L/min.
Preferably, during into crucible, charging is passed through oxygen with first time, temperature is maintained at 1350- in crucible
1450℃。
Preferably, since being passed through oxygen for the second time into crucible, the temperature of glass metal is first increased 100-200 DEG C,
0.5-1h is stood, then start to be stirred glass metal after the temperature of glass metal is stablized；The stirring carried out to glass metal is divided into
Twice, the rotating speed of stirring is 60-100rpm, mixing time 4-8h for the first time；Stop stirring 2-5h after stirring for the first time, simultaneously
The temperature of glass metal is gradually cooled to 1300-1350 DEG C, then carry out second of stirring；The rotating speed of second of stirring is 10-
20rpm, mixing time 2-4h；Stop being passed through oxygen at the end of second of stirring.
Preferably, the temperature in material leakage pipe is maintained at 1280-1330 DEG C when carrying out the material leakage forming, and keep being somebody's turn to do
Material leakage again after temperature 0.5h.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages：
1st, the crucible that the application provides is sealed using the fluid-tight structure that annular groove and annular baffle are used cooperatively, energy
It realizes the elevated-temperature seal in especial dispersion glass melting process, the volatilization of volatile components can be efficiently controlled；
2nd, by being equipped with the charge door that can realize fluid-tight, exhaust outlet and stirring on the crucible cover for the crucible that the application provides
Mouthful, it can realize and feed, ventilate and stir under air-proof condition, can not only completely cut off outside air, but also can be in predetermined protective gas atmosphere
Melted glass metal down, it is ensured that the abundant melting of refractory components in glass metal has by the especial dispersion glass of the crucible melting
There are higher optical homogeneity and batch consistency.
Description of the drawings
Fig. 1 is the structure diagram of the crucible of the embodiment of the present invention；
Fig. 2 is the structure diagram of the especial dispersion glass preparation device of the embodiment of the present invention；
Fig. 3 is the structure diagram of the snorkel of the embodiment of the present invention；
Fig. 4 is the structure diagram of the passage of the embodiment of the present invention.
Specific embodiment
The present invention is described in further detail, but not as a limitation of the invention with reference to specific embodiment.
In the description below, what different " embodiment " or " embodiment " referred to is not necessarily the same embodiment.In addition, one or more are implemented
Special characteristic, structure or feature in example can be combined by any suitable form.
Fig. 1 is the structure diagram of the crucible of the embodiment of the present invention.As shown in Figure 1, the crucible is used for glass smelting, including
Crucible body 9 and crucible cover 7 have the first annular groove for accommodating fluid-tight liquid on crucible body, have on crucible cover and first
The first annular catch that annular groove is adapted fills fluid-tight liquid between crucible cover and crucible body by the insertion of first annular catch
First annular groove in realize sealing；Crucible cover is equipped with charge door 2, and charge door is used to feeding and being passed through gas, crucible cover
The upper second annular groove being equipped with around charge door for accommodating fluid-tight liquid；Crucible cover is equipped with exhaust outlet 6, and exhaust outlet is used to arrange
Go out gas, be equipped with the third annular groove for accommodating fluid-tight liquid on crucible cover around exhaust outlet；Crucible cover is equipped with stirring port
4, the fourth annular groove for accommodating fluid-tight liquid is equipped with around stirring port on crucible cover；Crucible body bottom is equipped with material leakage pipe 3.
When crucible provided in an embodiment of the present invention is used for glass smelting, fluid-tight liquid is filled by the insertion of first annular catch
The dynamic sealing between crucible cover and crucible body is realized in first annular groove, outside air, volatile group of control can be completely cut off
The pressure in vaporization at high temperature and balance crucible divided, the optical homogeneity improved after especial dispersion glass smelting are consistent with batch
Property；Crucible cover is equipped with charge door, for feeding and being passed through gas, is equipped with to accommodate fluid-tight liquid around charge door on crucible cover
Second annular groove, the second annular groove can with the passage equipped with annular baffle, snorkel or plug be used cooperatively with
It is peaceful to play isolation outside air, control volatile components vaporization at high temperature for charging, ventilation or dynamic sealing under the conditions of realization fluid-tight
The effect of pressure, can be passed through protective gas by the charge door into crucible, under protective gas atmosphere, can improve in weighing apparatus crucible
The optical homogeneity of glass smelting；The exhaust outlet that crucible cover is equipped with can be passed through protection gas into crucible for discharging gas
During body, the air in crucible is discharged, it, should around exhaust outlet equipped with the third annular groove for accommodating fluid-tight liquid on crucible cover
Third annular groove it is extraneous can to play isolation with the plug with annular baffle with the use of the dynamic sealing to realize exhaust outlet
Air, control volatile components vaporization at high temperature and the effect for balancing pressure in crucible can improve the optical homogeneity of glass smelting；
Crucible body bottom is equipped with material leakage pipe, is shaped for material leakage after glass smelting.
As the preferred of above-described embodiment, above-mentioned crucible further includes the first plug 1, which has and above-mentioned second
The second annular baffle that annular groove is adapted, the first plug fill the second of fluid-tight liquid by the insertion of above-mentioned second annular baffle
Above-mentioned charge door is sealed in annular groove.The embodiment of the present invention fills the of fluid-tight liquid by the insertion of above-mentioned second annular baffle
The dynamic sealing of charge door is realized in second ring groove, can both completely cut off outside air and control volatile components vaporization at high temperature, and carry
The optical homogeneity of high glass smelting, and pressure in crucible can be balanced, prevent pressure in crucible excessive.
As the preferred of above-described embodiment, the crucible further includes the second plug 5, which has and above-mentioned third
The third annular baffle that annular groove is adapted, second plug by the insertion of above-mentioned third annular baffle by filling fluid-tight liquid
Above-mentioned exhaust outlet is sealed in third annular groove.The embodiment of the present invention passes through the fluid-tight structure between the second plug and exhaust outlet
It realizes the dynamic sealing of exhaust outlet, can both completely cut off outside air and control volatile components vaporization at high temperature, and improve glass smelting
Optical homogeneity, and pressure in crucible can be balanced, prevent pressure in crucible excessive.
As the preferred of above-described embodiment, above-mentioned crucible further includes blender 8, which includes rotary shaft and stirring
Portion, the rotary shaft pass through above-mentioned stirring port, and rotary shaft is equipped with first seal, which has recessed with fourth annular
The fourth annular catch that slot is adapted, the first seal fill the Fourth Ring of fluid-tight liquid by the insertion of above-mentioned fourth annular catch
The sealing between blender and crucible cover is realized in connected in star.The embodiment of the present invention sets blender on crucible, the blender
For the stirring to glass metal, glass metal can be accelerated to be homogenized, improve the optical homogeneity of glass；The embodiment of the present invention passes through stirring
Fluid-tight structure between first seal and poke hole in the rotary shaft of device realizes that the dynamic between blender and crucible cover is close
Envelope, guarantee blender play preferable sealing effect when rotating, and outside air is prevented, which to enter in crucible, influences the melted of glass metal
Effect；The preferred closed-in construction agitator of the embodiment of the present invention, since the viscosity of glass metal in especial dispersion glass melting process is small,
The optical homogeneity of glass can be improved using closed-in construction agitator.Between blender and crucible cover in the embodiment of the present invention into
During row fluid-tight, can first by rotary shaft pass through crucible cover stirring port, then by first seal welding on the rotary shaft, blender with
After crucible cover forms non-removable external member, then the fluid-tight being stirred between device and crucible cover；Or the rotary shaft of blender
It is dismountable assembly with mixing part, the rotary shaft equipped with first seal is first passed through into stirring port, by rotary shaft and stirring
After portion is assembled, then the fluid-tight being stirred between device and crucible cover.
Fig. 2 is the structure diagram of the especial dispersion glass preparation device of the embodiment of the present invention, which includes upper
State crucible.
As the preferred of above-described embodiment, as shown in figure 3, above-mentioned preparation facilities further includes snorkel, outside the snorkel
Wall is equipped with second seal, which has the 5th annular baffle being adapted with above-mentioned second annular groove, the
Two sealing elements filled by the insertion of above-mentioned 5th annular baffle realized in the second annular groove of fluid-tight liquid snorkel outside wall surface and
Sealing between crucible cover.The embodiment of the present invention passes through the fluid-tight knot ventilated between second seal and charge door in pipe outer wall
Structure realizes the dynamic sealing in gap between snorkel and charge door, and outside air and control can be completely cut off when being passed through gas into crucible
Volatile components vaporization at high temperature processed improves the optical homogeneity of glass smelting, while the snorkel is easy for installation and removal.
As the preferred of above-described embodiment, as shown in figure 4, above-mentioned preparation facilities further includes passage, the guide pipe outer wall
Rounded tabs or third sealing element are equipped with, wherein rounded tabs, which can be suspended on charge door, prevents passage from sliding or tilting；
Wherein third sealing element has the 6th annular baffle that is adapted with above-mentioned second annular groove, and third sealing element passes through above-mentioned the
The insertion of six annular baffles fills the sealing realized in the second annular groove of fluid-tight liquid between passage outside wall surface and crucible cover.This
Inventive embodiments preferably by fluid-tight structure between the third sealing element and charge door in guide pipe outer wall realize passage and
The dynamic sealing in gap between charge door can prevent outside air from entering in crucible, so as to improve when feeding into crucible
The optical homogeneity of glass smelting, while the passage is easy for installation and removal.
As the preferred of above-described embodiment, above-mentioned preparation facilities further includes melting furnace 12 and auxiliary stove 13, and crucible is placed in fusing
In stove, auxiliary stove is located at fusing furnace bottom, and material leakage pipe is located in auxiliary stove.Melting furnace maintains glass metal for being heated to crucible
Required temperature is melted；The effect of auxiliary stove is that the temperature of material leakage pipe is maintained when being shaped to glass metal material leakage, is prevented in material leakage pipe
Glass metal occur crystallization.
The preparation method of especial dispersion glass provided in an embodiment of the present invention is prepared using above-mentioned preparation facilities.Wherein
It is heat-resistance stainless steel plate outside melting furnace, inside is mullite refractory, and lower part is steel structure support；Earthenware is equipped in melting furnace
Crucible set 10 heats crucible by crucible sleeve, and the material of crucible sleeve is clay or quartz-ceramics material；First is equipped in melting furnace
Heating element 11, first heating element are Si-Mo rod, and the temperature in melting furnace can be made to be up to 1650 DEG C；It is equipped in auxiliary stove
Second heating element 14, second heating element are Elema, and the temperature in auxiliary stove can be made to be up to 1400 DEG C；Crucible cover,
Passage, material leakage pipe, the first plug, the second plug, first to fourth annular groove, first to third sealing element and first
It is pure Pt materials to the 6th annular baffle；The material of crucible body, blender and snorkel is strengthens Pt materials.
The preparation facilities of the especial dispersion glass of the embodiment of the present invention can be not only used for preparing especial dispersion glass, it is also possible to
It is prepared in the atmosphere protection of other glass.
The embodiment of the present invention carries out the preparation of especial dispersion glass, system using the preparation facilities of above-mentioned especial dispersion glass
Preparation Method is illustrated by specific examples below：
Embodiment 1
It is as follows that the present embodiment prepares the step of especial dispersion glass：
(1) following glass raw material is accurately weighed：Quartz sand 1.22kg, boric acid 6.39kg, tantalum pentoxide 2.64kg, dioxy
Change zirconium 1.80kg, soda ash 0.62kg, potassium carbonate 1.76kg, zinc oxide 0.24Kg, hafnium oxide 0.84kg and antimony oxide
0.12kg after mixing, is placed in conventional fused stove, is fused into glass metal in atmospheric conditions；
(2) crucible is placed in melting furnace, opens charge door and exhaust outlet on crucible cover, reheat melting furnace and auxiliary
Stove makes the temperature in crucible be maintained at 1400 DEG C, and the temperature in material leakage pipe is maintained at 1300 DEG C；It is close by first on blender
Gap of the fluid-tight structure between blender and poke hole between sealing and crucible cover carries out fluid-tight, and fluid-tight liquid used is above-mentioned
The glass metal that step (1) obtains；It is realized between crucible cover and crucible body by the fluid-tight structure between crucible cover and crucible body
Fluid-tight, fluid-tight liquid used are the glass metal that above-mentioned steps (1) obtain；Snorkel is inserted into charge door, and pass through second seal
Gap of the fluid-tight structure between snorkel and charge door between crucible cover carries out fluid-tight, and fluid-tight liquid used is above-mentioned steps
(1) glass metal obtained will be full of N by snorkel in crucible2Gas；Pass through the fluid-tight structure between the second plug and crucible cover
Fluid-tight is carried out to exhaust outlet, fluid-tight liquid used is the glass metal that above-mentioned steps (1) obtain；Snorkel is removed, passage is placed
At charge door, glass metal is imported by passage in crucible；
(3) after the completion of feeding, passage is removed, snorkel is inserted into charge door, and pass through second seal and crucible cover
Between gap of the fluid-tight structure between snorkel and charge door carry out fluid-tight, fluid-tight liquid used is above-mentioned steps (1) acquisition
Glass metal, open exhaust outlet, oxygen be passed through into crucible by snorkel, ventilation is divided into twice：When ventilating for the first time, use
End can be deep into the snorkel under metal level, and oxygen is passed under metal level, be passed through the water content of oxygen for the first time
≤ 2ppm, the flow for being passed through oxygen is 4L/min, and the time for being passed through oxygen is 1h；It carries out leading to for second after ventilating for the first time
Gas first passes through the fluid-tight structure between the second plug and crucible cover and fluid-tight is carried out to exhaust outlet, and fluid-tight liquid used is above-mentioned steps
(1) glass metal obtained, then change the snorkel that end is located on metal level into, while between the snorkel and charge door
Gap carries out fluid-tight, and fluid-tight liquid used is the glass metal that above-mentioned steps (1) obtain, then oxygen is passed on metal level.From
It is passed through oxygen for the second time to start, the temperature of glass metal is first increased 100 DEG C to 1500 DEG C and keeps, treats that the temperature of glass metal is stablized
Static 1h afterwards, then start to be stirred glass metal, wherein being passed through water content≤2ppm of oxygen for the second time, it is passed through the stream of oxygen
It measures as 0.5L/min；The stirring of glass metal is divided into twice, the rotating speed of stirring is 80rpm, mixing time 6h for the first time；First
Stop to stir 2h, while the temperature of glass metal is gradually cooled to 1350 DEG C, then carry out second of stirring after secondary stirring, stirring turns
Speed is 20rpm, mixing time 2h；At the end of second is stirred, glass metal complete clarification and homogenization stop being passed through at this time
Oxygen.
(4) temperature in material leakage pipe is risen to 1330 DEG C, and material leakage, forming is carried out to get spy after keeping temperature 0.5h
Different dispersive glass.
Embodiment 2
It is as follows that the present embodiment prepares the step of especial dispersion glass：
(1) following glass raw material is accurately weighed：Quartz sand 1.71kg, boric acid 4.26kg, tantalum pentoxide 3.60kg, dioxy
Change zirconium 1.44kg, potassium carbonate 2.29kg, lithium carbonate 0.3kg, zinc oxide 0.12kg, calcium carbonate 0.22kg, barium carbonate 0.31kg, oxygen
Change hafnium 0.6kg and antimony oxide 0.12kg, after mixing, be placed in conventional fused stove, be fused into glass in atmospheric conditions
Glass liquid；
(2) crucible is placed in melting furnace, opens charge door and exhaust outlet on crucible cover, reheat melting furnace and auxiliary
Stove makes the temperature in crucible be maintained at 1350 DEG C, and the temperature in material leakage pipe is maintained at 1250 DEG C；It is close by first on blender
Gap of the fluid-tight structure between blender and poke hole between sealing and crucible cover carries out fluid-tight, and fluid-tight liquid used is above-mentioned
The glass metal that step (1) obtains；It is realized between crucible cover and crucible body by the fluid-tight structure between crucible cover and crucible body
Fluid-tight, fluid-tight liquid used are the glass metal that above-mentioned steps (1) obtain；Snorkel is inserted into charge door, and pass through second seal
Gap of the fluid-tight structure between snorkel and charge door between crucible cover carries out fluid-tight, and fluid-tight liquid used is above-mentioned steps
(1) glass metal obtained will be full of O by snorkel in crucible2Gas；Pass through the fluid-tight structure between the second plug and crucible cover
Fluid-tight is carried out to exhaust outlet, fluid-tight liquid used is the glass metal that above-mentioned steps (1) obtain；Snorkel is removed, passage is placed
At charge door, glass metal is imported by passage in crucible；
(3) after the completion of feeding, passage is removed, snorkel is inserted into charge door, and pass through second seal and crucible cover
Between gap of the fluid-tight structure between snorkel and charge door carry out fluid-tight, fluid-tight liquid used is above-mentioned steps (1) acquisition
Glass metal, open exhaust outlet, oxygen be passed through into crucible by snorkel, ventilation is divided into twice：When ventilating for the first time, use
End can be deep into the snorkel under metal level, and oxygen is passed under metal level, be passed through the water content of oxygen for the first time
≤ 2ppm, the flow for being passed through oxygen is 2L/min, and the time for being passed through oxygen is 3h；It carries out leading to for second after ventilating for the first time
Gas first passes through the fluid-tight structure between the second plug and crucible cover and fluid-tight is carried out to exhaust outlet, and fluid-tight liquid used is above-mentioned steps
(1) glass metal obtained, then change the snorkel that end is located on metal level into, while between the snorkel and charge door
Gap carries out fluid-tight, and fluid-tight liquid used is the glass metal that above-mentioned steps (1) obtain, then oxygen is passed on metal level.From
It is passed through oxygen for the second time to start, the temperature of glass metal is first increased 100 DEG C to 1450 DEG C and keeps, treats that the temperature of glass metal is stablized
Static 0.5h afterwards, then start to be stirred glass metal, wherein being passed through water content≤2ppm of oxygen for the second time, it is passed through oxygen
Flow is 1L/min；The stirring of glass metal is divided into twice, the rotating speed of stirring is 60rpm, mixing time 8h for the first time；First
Stop to stir 4h, while the temperature of glass metal is gradually cooled to 1300 DEG C, then carry out second of stirring after secondary stirring, stirring turns
Speed is 10rpm, mixing time 4h；At the end of second is stirred, glass metal complete clarification and homogenization stop being passed through at this time
Oxygen.
(4) temperature in material leakage pipe is risen to 1280 DEG C, and material leakage, forming is carried out to get spy after keeping temperature 0.5h
Different dispersive glass.
Embodiment 3
It is as follows that the present embodiment prepares the step of especial dispersion glass：
(1) following glass raw material is accurately weighed：Quartz sand 1.83kg, boric acid 5.33kg, tantalum pentoxide 1.80kg, dioxy
Change zirconium 2.16kg, soda ash 2.89kg, barium carbonate 0.31kg, hafnium oxide 1.2kg and antimony oxide 0.12kg, after mixing,
It is placed in conventional fused stove, is fused into glass metal in atmospheric conditions；
(2) crucible is placed in melting furnace, opens charge door and exhaust outlet on crucible cover, reheat melting furnace and auxiliary
Stove makes the temperature in crucible be maintained at 1450 DEG C, and the temperature in material leakage pipe is maintained at 1300 DEG C；It is close by first on blender
Gap of the fluid-tight structure between blender and poke hole between sealing and crucible cover carries out fluid-tight, and fluid-tight liquid used is above-mentioned
The glass metal that step (1) obtains；It is realized between crucible cover and crucible body by the fluid-tight structure between crucible cover and crucible body
Fluid-tight, fluid-tight liquid used are the glass metal that above-mentioned steps (1) obtain；Snorkel is inserted into charge door, and pass through second seal
Gap of the fluid-tight structure between snorkel and charge door between crucible cover carries out fluid-tight, and fluid-tight liquid used is above-mentioned steps
(1) glass metal obtained will be full of He gas by snorkel in crucible；Pass through the fluid-tight structure between the second plug and crucible cover
Fluid-tight is carried out to exhaust outlet, fluid-tight liquid used is the glass metal that above-mentioned steps (1) obtain；Snorkel is removed, passage is placed
At charge door, glass metal is imported by passage in crucible；
(3) after the completion of feeding, passage is removed, snorkel is inserted into charge door, and pass through second seal and crucible cover
Between gap of the fluid-tight structure between snorkel and charge door carry out fluid-tight, fluid-tight liquid used is above-mentioned steps (1) acquisition
Glass metal, open exhaust outlet, oxygen be passed through into crucible by snorkel, ventilation is divided into twice：When ventilating for the first time, use
End can be deep into the snorkel under metal level, and oxygen is passed under metal level, be passed through the water content of oxygen for the first time
≤ 2ppm, the flow for being passed through oxygen is 6L/min, and the time for being passed through oxygen is 0.5h；It is carried out after ventilating for the first time second
Ventilation first passes through the fluid-tight structure between the second plug and crucible cover and fluid-tight is carried out to exhaust outlet, and fluid-tight liquid used is above-mentioned step
Suddenly the glass metal that (1) obtains, then change the snorkel that end is located on metal level into, while between the snorkel and charge door
Gap carry out fluid-tight, fluid-tight liquid used is the glass metal that above-mentioned steps (1) obtain, then oxygen is passed on metal level.
Since being passed through oxygen for the second time, the temperature of glass metal is first increased 200 DEG C to 1650 DEG C and is kept, treats that the temperature of glass metal is steady
Static 1h after fixed, then start to be stirred glass metal, wherein being passed through water content≤2ppm of oxygen for the second time, it is passed through oxygen
Flow is 2L/min；The stirring of glass metal is divided into twice, the rotating speed of stirring is 100rpm, mixing time 4h for the first time；The
Stop stirring 5h, while the temperature of glass metal is gradually cooled to 1330 DEG C, then carry out second of stirring after primary stirring, stir
Rotating speed is 15rpm, mixing time 3h；At the end of second is stirred, glass metal complete clarification and homogenization stop logical at this time
Enter oxygen.
(4) temperature in material leakage pipe is risen to 1300 DEG C, and material leakage, forming is carried out to get spy after keeping temperature 0.5h
Different dispersive glass.
Comparative example 1
This comparative example prepares especial dispersion glass using common crucible, the crucible of the common crucible and the use of embodiment 1
The difference lies in, between crucible cover and crucible body, between charge door and snorkel, between charge door and passage, blender
Between stirring port and the equal aneroid seal structure of exhaust ports, and the common crucible do not include plug, charge door and exhaust outlet without
Method is sealed by plug.In addition to more than structure, the other structures and material of the common crucible and the earthenware of the use of embodiment 1
Crucible it is identical.In addition to crucible, snorkel and passage, this comparative example using the preparation facilities identical with the embodiment of the present invention 1 come
Prepare especial dispersion glass.
It is as follows that this comparative example prepares the step of especial dispersion glass：
(1) following glass raw material is accurately weighed：Quartz sand 1.22kg, boric acid 6.39kg, tantalum pentoxide 2.64kg, dioxy
Change zirconium 1.80kg, soda ash 0.62kg, potassium carbonate 1.76kg, zinc oxide 0.24Kg, hafnium oxide 0.84kg and antimony oxide
0.12kg after mixing, is placed in conventional fused stove, is fused into glass metal in atmospheric conditions；
(2) common crucible is placed in melting furnace；Melting furnace and auxiliary stove are heated, the temperature in crucible is made to be maintained at 1400
DEG C, the temperature in material leakage pipe is maintained at 1300 DEG C；Common snorkel is inserted into charge door, will be filled in crucible by the snorkel
Full N2Gas；Snorkel is removed, common passage is inserted into charge door, the glass metal that step (1) obtains is led by the passage
Enter into crucible；
(3) after the completion of feeding, passage is removed, snorkel is inserted into charge door, oxygen is passed through into crucible by snorkel
Gas, ventilation are divided into twice：When ventilating for the first time, the snorkel under metal level can be deep into using end, oxygen is passed into
Under metal level, it is passed through water content≤2ppm of oxygen for the first time, the flow for being passed through oxygen is 4L/min, is passed through the time of oxygen
For 1h；It carries out ventilating for second after ventilating for the first time, changes the snorkel that end is located on metal level into, oxygen is passed through
Onto metal level.Since being passed through oxygen for the second time, the temperature of glass metal is first increased 100 DEG C to 1500 DEG C and is kept, is treated
Static 1h after the temperature of glass metal is stablized, then start to be stirred glass metal, wherein be passed through for the second time the water content of oxygen≤
2ppm, the flow for being passed through oxygen are 0.5L/min；The stirring of glass metal is divided into twice, the rotating speed of stirring is 80rpm for the first time,
Mixing time is 6h；Stop stirring 2h, while the temperature of glass metal is gradually cooled to 1350 DEG C, then carry out after stirring for the first time
Second of stirring, speed of agitator 20rpm, mixing time 2h；At the end of second is stirred, stopping is passed through oxygen.
(4) temperature in material leakage pipe is risen to 1330 DEG C, and material leakage, forming is carried out to get spy after keeping temperature 0.5h
Different dispersive glass.
Comparative example 2
It is as follows that this comparative example prepares the step of especial dispersion glass：
(1) following glass raw material is accurately weighed：Quartz sand 1.22kg, boric acid 6.39kg, tantalum pentoxide 2.64kg, dioxy
Change zirconium 1.80kg, soda ash 0.62kg, potassium carbonate 1.76kg, zinc oxide 0.24Kg, hafnium oxide 0.84kg and antimony oxide
0.12kg after mixing, is placed in conventional fused stove, is fused into glass metal in atmospheric conditions；
(2) operation of the step and condition are the same as (2) the step of embodiment 1；
(3) in the step in addition to the gas being passed through twice into crucible is nitrogen, other operations and condition are the same as embodiment 1
Step (3)；
(4) operation of the step and condition are the same as (4) the step of embodiment 1.
The especial dispersion glass prepared by detecting the embodiment of the present invention and comparative example, finds prepared by the embodiment of the present invention
Especial dispersion glass in each component content be predetermined constituent content, and with higher optical homogeneity and batch consistency,
And volatile components content largely reduces in the especial dispersion glass prepared by comparative example 1, and optical homogeneity is poor, comparative example
Each component content is predetermined constituent content in especial dispersion glass prepared by 2, but optical homogeneity is poor.Pass through embodiment 1
Comparison with comparative example 1 is found, can be efficiently controlled using the crucible of the embodiment of the present invention volatile in especial dispersion glass
The volatilization of component also ensures that the abundant melting of refractory components, and the special color of high optical homogeneity and high batch consistency can be made
Glass is dissipated, and the preparation that especial dispersion glass coexists in " volatile components-refractory components " cannot be completed using common crucible.Pass through
The comparison of embodiment 1 and comparative example 2 finds, oxygen is passed through into crucible, and to realize that the oxygen atmosphere protection of glass metal can improve special
The optical homogeneity of dispersive glass, and other gases are acted on without this.
The embodiment of the present invention to glass metal in step (2) and step (3) before material leakage forming is carried out, the temperature in material leakage pipe
Degree is maintained at 1250-1300 DEG C, so that glass metal is solidified in material leakage pipe without leaking out, while prevents glass metal in material leakage pipe
Crystallization occurs, influences the optical homogeneity after the forming of glass metal material leakage.When the temperature in material leakage pipe is higher than 1300 DEG C, glass metal
It cannot be solidified in into material leakage pipe, when the temperature in material leakage pipe is less than 1250 DEG C, glass metal crystallization in material leakage pipe, and material leakage
Manage, destructible Pt material too big with the temperature difference of crucible.
The embodiment of the present invention uses N before glass metal is imported into crucible in crucible2、O2, He or Ar gas carry out atmosphere guarantor
Shield, the purpose is to prevent the moisture in air from entering in glass metal, influences the optical homogeneity of glass.
The glass metal that the fluid-tight liquid that the crucible of the embodiment of the present invention uses is obtained for step (1).Due to especial dispersion glass
Stablize at a temperature of glass smelting for liquid and relatively, using treating that melted especial dispersion glass metal as fluid-tight liquid, can both realize
The high temperature dynamic sealing of especial dispersion glass smelting device, and will not be introduced into other impurity to crucible, influence the group of glass metal
Point.
The embodiment of the present invention is passed through oxygen into crucible, its purpose is that：First, glass metal is made to keep oxygen-enriched state, be conducive to
Glass metal high temperature is clarified；Second is that the component for making proportion larger such as ZrO2And HfO2Deng in suspended state, prevent them from sinking to the bottom, promote
It is homogenized into glass metal；Third, under oxygen-enriched environment, glass metal is smaller to the corrosion of Pt crucibles.The embodiment of the present invention is passed through into crucible
Oxygen is divided into twice, exhaust outlet is opened when being passed through oxygen for the first time, and oxygen is passed under metal level, makes oxygen and glass
Liquid comes into full contact with, and other gases in crucible are discharged rapidly, and glass metal is made to be under oxygen-enriched state, promotes the equal of glass metal
Change；Fluid-tight is carried out to exhaust outlet by the fluid-tight structure between the second plug and crucible cover when being passed through oxygen for the second time, be in order to
Outside air is prevented to enter in crucible, avoids influencing being melted for glass metal, oxygen is passed into glass when being passed through oxygen for the second time
On liquid level, until glass metal clarification and homogenization.It is in order under conditions of oxygen is passed through that oxygen, which is passed on metal level,
Stirring, realizes the clarification and homogenization of glass metal, wherein can accelerate glass metal clarification and homogenization by stirring, in the item for being passed through oxygen
Stirring can make glass metal still in oxygen-enriched state, be conducive to the homogenizing of glass metal while agitating under part.
The embodiment of the present invention is passed through water content≤2ppm of oxygen, is the moisture that glass metal absorbs in oxygen in order to prevent
And influence optical homogeneity；The embodiment of the present invention is passed through the flow of oxygen as 2-6L/min for the first time, and the time for being passed through oxygen is
0.5-3h；The flow for being passed through oxygen for the second time is 0.5-2L/min；The flow for being wherein passed through oxygen for the first time is big, and the time is short, is
In order to rapidly discharge other gases in crucible, the flow for being passed through oxygen for the second time is small, and the time is long, until glass metal clarification and
Homogenizing, be in order to have been filled with oxygen in crucible in the case of continue with relatively small oxygen flow maintain crucible in it is oxygen-enriched
State is conducive to the homogenizing of glass metal.
During the charging into crucible and being passed through oxygen for the first time, the temperature in crucible is maintained at the embodiment of the present invention
1350-1450 DEG C, purpose make glass metal imported into crucible after still in molten state and not crystallization, be conducive to glass metal
It is further melted, while avoids charging and be passed through the volatilization of volatile components in oxygen process for the first time.
Since the embodiment of the present invention first increase 100-200 being passed through oxygen for the second time into crucible by the temperature of glass metal
DEG C, the static 0.5-1h after the temperature of glass metal is stablized, then start to be stirred glass metal.Relative to being passed through oxygen for the first time
When, the temperature of glass metal is increased 100-200 DEG C, the purpose is to make the refractory components in glass metal abundant at higher temperatures
Melting, it is in order to which the bubble in glass metal is made gradually to eliminate that glass metal, which stands 0.5-1h, glass metal is made voluntarily to restore to clarify, favorably
It is homogenized in the stirring of next step.The stirring that the embodiment of the present invention carries out glass metal is divided into twice, and the rotating speed of stirring is for the first time
60-100rpm, mixing time 4-8h；Stop stirring 2-5h, while gradually cooling down the temperature of glass metal into after stirring for the first time
To 1300-1350 DEG C, then carry out second of stirring；The rotating speed of second of stirring is 10-20rpm, mixing time 2-4h.First
The rotating speed of secondary stirring is very fast, and glass metal can be made to accelerate homogenizing；Stop stirring 2-5h after stirring for the first time, make glass metal voluntarily clear
Clearly；The temperature of glass metal is gradually cooled to 1300-1350 DEG C again, is to make glass metal that there is suitable viscosity, be conducive to
Material leakage shapes, and when the temperature of glass metal is higher than 1350 DEG C, viscosity of glass metal is small, easily splashed out during material leakage forming, works as glass
When the temperature of liquid is less than 1300 DEG C, viscosity of glass metal is larger, and crystallization easily occurs；It is needed again after temperature of glass liquid reduction
It is stirred, so that glass metal reaches best homogenizing state before material leakage forming；After the temperature of glass metal reduces, glass metal glues
Degree increase, then need to be stirred with relatively low rotating speed.
Temperature in material leakage pipe is first maintained at 1280- by the embodiment of the present invention when carrying out material leakage forming to glass metal
1330 DEG C, and keep after the temperature 0.5h material leakage again.During relative to glass smelting, temperature when material leakage shapes in material leakage pipe is
Raising can be such that the glass metal in material leakage pipe is leaked out after melting.When the temperature in material leakage pipe is less than 1280 DEG C, glass metal cannot
Fusing and leak out, can generate secondary bubble during higher than 1330 DEG C, in glass metal, influence the optical homogeneity of glass.
Crucible cover, passage, material leakage pipe, the first plug, the second plug, first to fourth annular are recessed in the embodiment of the present invention
The annular baffle of slot, first to third sealing element and first to the 6th is pure Pt materials, is due to the fusing point of pure Pt materials
Height can meet the temperature requirement of especial dispersion glass smelting, and will not cause the pollution of glass metal；Crucible body, blender and logical
The material of tracheae, since reinforcing Pt is more more stable and anticorrosive than pure Pt, contacts for a long time to strengthen Pt materials with glass metal
Crucible body, blender and snorkel can avoid glass metal from being contaminated using Pt materials are strengthened.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
The present invention is described in detail in good embodiment, it will be understood by those of ordinary skill in the art that, it can be to the skill of the present invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the right of invention.
Claims (13)
1. the preparation facilities of especial dispersion glass that a kind of volatile components-refractory components coexist, including crucible and snorkel,
It is characterized in that, the crucible includes crucible body and crucible cover, has to accommodate the first annular of fluid-tight liquid on the crucible body
Groove has the first annular catch being adapted with the first annular groove, the crucible cover and crucible on the crucible cover
It is filled between body by the first annular catch insertion and sealing is realized in the first annular groove of fluid-tight liquid；
The crucible cover is equipped with charge door, and the charge door is equipped with for feeding on the crucible cover around the charge door
For accommodating the second annular groove of fluid-tight liquid；
The crucible cover is equipped with exhaust outlet, and the exhaust outlet surrounds the exhaust outlet for discharging gas on the crucible cover
Equipped with for accommodating the third annular groove of fluid-tight liquid；
The crucible cover is equipped with stirring port, be equipped with around the stirring port on the crucible cover for accommodate fluid-tight liquid the 4th
Annular groove；
The crucible body bottom is equipped with material leakage pipe；
The snorkel is inserted into charge door, and for being passed through first gas, the first gas includes oxygen.
2. preparation facilities according to claim 1, which is characterized in that the crucible further includes the first plug, and described first
Plug has the second annular baffle being adapted with the second annular groove, and first plug is kept off by the described second annular
Piece insertion, which fills, seals the charge door in the second annular groove of fluid-tight liquid.
3. preparation facilities according to claim 1, which is characterized in that the crucible further includes the second plug, and described second
Plug has the third annular baffle being adapted with the third annular groove, and second plug is kept off by the third annular
Piece insertion, which fills, seals the exhaust outlet in the third annular groove of fluid-tight liquid.
4. preparation facilities according to claim 1, which is characterized in that the crucible further includes blender, the blender
Including rotary shaft and mixing part, the rotary shaft passes through the stirring port, and the rotary shaft is equipped with first seal, and described the
One sealing element has the fourth annular catch being adapted with fourth annular groove, and the first seal passes through the fourth annular
Catch insertion fills the sealing realized in the fourth annular groove of fluid-tight liquid between blender and crucible cover.
5. the preparation facilities of especial dispersion glass according to claim 1, which is characterized in that on the outer wall of the snorkel
Equipped with second seal, the second seal has the 5th annular baffle being adapted with the second annular groove, described
Second seal is filled by the 5th annular baffle insertion and snorkel outside wall surface is realized in the second annular groove of fluid-tight liquid
Sealing between crucible cover.
6. a kind of preparation method of especial dispersion glass, which is characterized in that the method utilizes any one of claim 1-5 institutes
The preparation facilities stated is completed, and the described method comprises the following steps：
(1) glass raw material weighed is mixed, fusing obtains glass metal；
(2) glass metal is imported into crucible；
(3) after the completion of feeding, oxygen is passed through into crucible, glass metal is stirred under conditions of oxygen is passed through, realize glass
The clarification and homogenization of glass liquid；
(4) after glass metal homogenizing completely, material leakage forming,
The fluid-tight liquid is the glass metal in step (1).
7. the preparation method of especial dispersion glass according to claim 6, which is characterized in that material leakage is being carried out to glass metal
In the step (2) and the step (3) before forming, the temperature in material leakage pipe is maintained at 1250-1300 DEG C, so that glass metal
Solidification is without leaking out in material leakage pipe, while prevents glass metal from crystallization occurs in material leakage pipe.
8. the preparation method of especial dispersion glass according to claim 6, which is characterized in that glass metal is imported into crucible
Before, N is used in crucible2、O2, He or Ar gas carry out atmosphere protection.
9. the preparation method of especial dispersion glass according to claim 6, which is characterized in that after the completion of charging, to crucible
It is inside passed through oxygen to be divided into twice, oxygen is passed under glass metal liquid level when ventilating for the first time；Start after ventilating for the first time
Oxygen is passed on glass metal liquid level by ventilation for the second time when ventilating for the second time, is ventilated for the second time up to glass metal is clarified and equal
Change.
10. the preparation method of especial dispersion glass according to claim 9, which is characterized in that the water content of the oxygen
≤2ppm；The flow for being passed through oxygen for the first time is 2-6L/min, and the time for being passed through oxygen for the first time is 0.5-3h；It is passed through for the second time
The flow of oxygen is 0.5-2L/min.
11. the preparation method of especial dispersion glass according to claim 9, which is characterized in that the charging and the into crucible
During being once passed through oxygen, temperature is maintained at 1350-1450 DEG C in crucible.
12. the preparation method of especial dispersion glass according to claim 11, which is characterized in that from second into crucible
It is passed through oxygen to start, the temperature of glass metal is first increased 100-200 DEG C, 0.5-1h is stood after the temperature of glass metal is stablized, then
Start to be stirred glass metal；The stirring carried out to glass metal is divided into twice, and the rotating speed of stirring is 60-100rpm for the first time,
Mixing time is 4-8h；Stop stirring 2-5h, while the temperature of glass metal is gradually cooled to 1300-1350 after stirring for the first time
DEG C, then carry out second of stirring；The rotating speed of second of stirring is 10-20rpm, mixing time 2-4h；Second of stirring terminates
When stop be passed through oxygen.
13. the preparation method of especial dispersion glass according to claim 6, which is characterized in that carry out the material leakage forming
When the temperature in material leakage pipe is maintained at 1280-1330 DEG C, and keep after the temperature 0.5h material leakage again.
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| CN108395074A (en) * | 2018-04-10 | 2018-08-14 | 湖北新华光信息材料有限公司 | A kind of glass stock crucible and stock method |
| CN110255898B (en) * | 2019-06-28 | 2021-09-28 | 中国建筑材料科学研究总院有限公司 | Deep ultraviolet transparent glass, preparation method, application and melting device thereof |
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| US3656924A (en) * | 1969-11-17 | 1972-04-18 | Owens Illinois Inc | Apparatus and methods for melting glass compositions for glass laser rods |
| JPH02311319A (en) * | 1989-05-24 | 1990-12-26 | Shin Etsu Chem Co Ltd | Production of optical glass, equipment therefor and sealing composition used in the same equipment |
| CN101486530A (en) * | 2009-02-27 | 2009-07-22 | 中国科学院上海光学精密机械研究所 | 2 mu m luminous rare earth ion doped germanate laser glass and preparation thereof |
| CN203173958U (en) * | 2013-03-28 | 2013-09-04 | 湖北新华光信息材料有限公司 | Optical glass smelting crucible |
| CN104445921B (en) * | 2014-11-13 | 2017-03-15 | 中国建筑材料科学研究总院 | A kind of high zirconium borosilicate glass and preparation method thereof |
| CN205045976U (en) * | 2015-10-14 | 2016-02-24 | 中国建筑材料科学研究总院 | Crucible and special chromatic dispersion glass's preparation facilities |
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