CN106007385A - Method for preparing surface crystallization glass ceramics - Google Patents
Method for preparing surface crystallization glass ceramics Download PDFInfo
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- CN106007385A CN106007385A CN201610319303.9A CN201610319303A CN106007385A CN 106007385 A CN106007385 A CN 106007385A CN 201610319303 A CN201610319303 A CN 201610319303A CN 106007385 A CN106007385 A CN 106007385A
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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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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Abstract
The invention relates to the technical field of glass, in particular to a method for preparing surface crystallization glass ceramics. The method comprises the steps of 1, providing raw materials and grinding and evenly mixing the raw materials, wherein the raw materials are zinc oxide, boron oxide and silicon dioxide which are mixed based on the molar ratio of (25-60):(5-50):(5-30); 2, heating and melting the product generated in step 1 to obtain glass metal; 3, conducting molding and annealing on the glass metal generated in step 2 to obtain an intermediate product; 4, conducting heat treatment on the intermediate product generated in step 3 to obtain the surface crystallization glass ceramics. According to the method, no crystallization agent is required, processes are simple, steps are clear, cost is low, and surface crystallization effect is good.
Description
Technical field
The present invention relates to glass technology field, particularly to the preparation method of Surface Crystallization devitrified glass.
Background technology
The intensity of general glass is not the highest, and about at about 50MP, but theoretical strength value is the most about
Between 9810～29420MPa.Reason is that glass surface also exists what countless optical microscope be can't see
Crackle, is referred to as Griffith crack.These crackles are the effect that half elliptic plays center of stress,
When glass is plus load, fracture process, first from the beginning of cracks, occurs than not having defective glass
Early.Here it is the reason that the actual strength of glass surface and theoretical strength differ greatly.Lacking on glass surface
Fall into fragile more than inside glass many, so wanting to increase substantially the intensity of glass, must be first to glass table
Face takes measures.Surface Crystallization glass is expected to improve the intensity of glass, if allowing glass surface crystallization make
The minimum crystal of high-volume fractional is there are, in order to limit the lattice Lifei caused by stress inside glass body
This crackle, thus can make the intensity of glass bring up to more than 200MPa.
Surface Crystallization glass is as plated layer protecting film at glass surface, and mechanical strength is high, and hardness is big,
Wearability is fine, chemical stability and good thermal stability, it is possible to adapt to severe use environment；Electricity is absolutely
Edge function admirable, dielectric constant is stable, and dielectric loss is little；With the metal material with identical mechanical property
Comparing, Surface Crystallization glass material quality is fine and close, has the premium properties such as airtight, waterproof.And,
The glass that can also utilize different composition prepares has special optical, calorifics, magnetics, electricity and biology
The Surface Crystallization glass of etc. functions so that this material has extraordinary economic benefit, and is expected to generation
For traditional material.
Glass surface crystallize has been carried out certain work, such as University Of Ji'nan Liu generation power et al. by relevant scholar
The patent of application: CN102849952A, discloses a kind of method promoting glass surface crystallize.Step is
When preparing glass, in glass, introduce the Nucleating Agent promoting crystallize, to promote the Surface Crystallization of gained glass.
The described Nucleating Agent promoting crystallize includes titanium oxide, chromic oxide or the mixture of both.Logical
Cross simple method and promote the Surface Crystallization of glass, in the case of without carrying out glass crushing, add
Glass Nucleating Agent (the TiO used when adding traditional overall crystallize2、Cr2O3) just can improve the surface of glass
Crystal content in crystallize speed or Surface Crystallization layer, the method is simple for process, imitates Surface Crystallization
Fruit is notable.And it is possible to by regulation TiO2、Cr2O3Consumption obtain different crystallize layer thickness and crystal
The crystallize glass of content, meets various different demand.
But, the method for above-mentioned Surface Crystallization is required to introduce crystallize agent in glass to reach surface analysis
Crystalline substance, inefficient.
Summary of the invention
In order to solve above technical problem, the present invention provides the preparation method of a kind of Surface Crystallization devitrified glass.
The present invention provides the preparation method of a kind of Surface Crystallization devitrified glass, including:
Step 1, offer raw material, described raw material includes that mol ratio is (25～60): (5～50): (5～30)
Zinc oxide, boron oxide and silicon dioxide；Described raw mill is mixed；
The heating of step 2, raw material step 1 obtained is founded, and obtains vitreous humour；
Step 3, vitreous humour step 2 obtained are shaped and make annealing treatment, and obtain intermediate products；
Step 4, intermediate products step 3 obtained carry out heat treatment, obtain Surface Crystallization devitrified glass.
Further, described raw material also includes aluminium oxide and/or sodium oxide；Described aluminium oxide and described oxidation
The mol ratio of zinc is (0～4): (25～60)；Described sodium oxide is (0～20) with the mol ratio of described zinc oxide:
(25～60).
Further, described step 2 particularly as follows:
Raw material step 1 obtained is heated to 1100 DEG C～1500 DEG C, is incubated 0.5h～3h, obtains vitreous humour.
Further, described step 3 particularly as follows:
The vitreous humour that step 2 is obtained molding on preheated graphite jig, after molding
It is incubated 0.5h～2h at 450 DEG C～580 DEG C, is then cooled to room temperature, obtains intermediate products.
Further, described step 4 particularly as follows:
Intermediate products step 3 obtained are warming up to 590 DEG C～680 DEG C, are incubated 0.5h～70h.
Further, described step 4 particularly as follows:
Intermediate products step 3 obtained are heat treatment 0.5h～3h at 450 DEG C～630 DEG C；Heat up the most again
Carrying out secondary heat treatment to 590 DEG C～680 DEG C, the time of described secondary heat treatment is 0.5h～50h.
Further, described in be warming up in the step of 590 DEG C～680 DEG C, heating rate is 5 DEG C/min
～10 DEG C/min.
Further, also including impurity in described raw material, described impurity includes sulfate, chloride, phosphorus
Hydrochlorate, calcium, lead and ferrum, its content summation is not more than the 2wt% of raw material；Or, described raw material includes nitre
Hydrochlorate, chloride, sulfate, manganese, lead and ferrum, its content summation is not more than the 2wt% of raw material；Or,
Described raw material includes chloride, ferrum and Fluohydric acid. non-volatile matter, and its content summation is not more than the 4wt% of raw material.
The present invention provides the preparation method of a kind of Surface Crystallization devitrified glass, and the method is with zinc oxide, oxidation
The frit fusion cast glass such as boron and silicon dioxide, obtains Surface Crystallization micro-under suitable heat treating regime
Crystal glass, can obtain the Surface Crystallization crystallite of different crystallize layer thickness by control heat treatment temperature and time
Glass, with the needs of satisfied different purposes.The preparation method of this Surface Crystallization devitrified glass need not add appoint
What crystallize agent, technique is simple, and step understands, with low cost, Surface Crystallization is effective.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to reality
Execute the required accompanying drawing used in example or description of the prior art to be briefly described.
Fig. 1 is the Surface Crystallization devitrified glass of the embodiment of the present invention 12 preparation；
Fig. 2 is the XRD figure of the Surface Crystallization devitrified glass of the embodiment of the present invention 1 to 5 preparation.
Detailed description of the invention
The invention discloses the preparation method of a kind of Surface Crystallization devitrified glass, those skilled in the art are permissible
Use for reference present disclosure, be suitably modified technological parameter and realize.Special needs to be pointed out is, all similar replacing
Changing and change apparent to those skilled in the art, they are considered as being included in the present invention.
Method and the application of the present invention are described by preferred embodiment, and related personnel substantially can be not
In disengaging present invention, spirit and scope, method described herein and application it is modified or suitably becomes
More with combination, realize and apply the technology of the present invention.
The present invention provides the preparation method of a kind of Surface Crystallization devitrified glass, comprising:
Step 1, offer raw material, this raw material includes that mol ratio is (25～60): (5～50): (5～30)
Zinc oxide, boron oxide and silicon dioxide；Raw mill is mixed；
The heating of step 2, raw material step 1 obtained is founded, and obtains vitreous humour；
Step 3, vitreous humour step 2 obtained are shaped and make annealing treatment, and obtain intermediate products；
Step 4, intermediate products step 3 obtained carry out heat treatment, obtain Surface Crystallization devitrified glass.
In above-mentioned raw materials, the mol ratio of zinc oxide, boron oxide and silicon dioxide is preferably (30～60):
(25～40): (5～20), more preferably 60:30:10.As the preferred version of the present invention, this raw material
In also include aluminium oxide and/or sodium oxide；Aluminium oxide is (0～4) in the mol ratio of zinc oxide: (25～60)；
Sodium oxide is (0～20) with the mol ratio of zinc oxide: (25～60).Aluminium oxide is added according to aforementioned proportion
And/or the effect of sodium oxide is: so that glass formation range increases after adding said components, enter one
Step optimizing surface crystallization property.
Further, this raw material includes sodium oxide and aluminium oxide the most simultaneously, zinc oxide in raw material,
The mol ratio of boron oxide, silicon dioxide, sodium oxide and aluminium oxide is 30:50:15:4:1.
In above-mentioned raw materials allow content trace impurity, this impurity include sulfate, chloride, phosphate,
Calcium, lead and ferrum, its content summation is not more than the 2wt% of raw material；Or, raw material includes nitrate, chlorination
Thing, sulfate, manganese, lead and ferrum, its content summation is not more than the 2wt% of raw material；Or, raw material includes
Chloride, ferrum and Fluohydric acid. non-volatile matter, its content summation is not more than the 4wt% of raw material.
Above-mentioned steps 2 is particularly preferred as: raw material step 1 obtained is heated to 1100 DEG C～1500 DEG C, protects
Temperature 0.5h～3h, obtains vitreous humour.This step is preferably carried out in high temperature melting stove.
Above-mentioned steps 3 is particularly preferred as: vitreous humour step 2 obtained is on preheated graphite jig
Molding, is incubated 0.5h～2h at 450 DEG C～580 DEG C, is then cooled to room temperature, obtain middle product after molding
Product.The operation of above-mentioned heating and thermal insulation, the operation i.e. annealed can be carried out in annealing furnace.The speed heated up
It is preferably 5 DEG C/min～10 DEG C/min.
The process carrying out heat treatment of above-mentioned steps 4, can control by controlling heat treatment temperature and time
The thickness of glass surface crystallize.
Step 4 is particularly preferred as: product step 3 obtained is warming up to 590 DEG C～680 DEG C, insulation
0.5h～70h.This step can be carried out in electric furnace.
Or, step 4 is particularly preferred as: product step 3 obtained is heat treatment at 450 DEG C～630 DEG C
0.5h～3h；It is warming up to the most again at 590 DEG C～680 DEG C carry out secondary heat treatment, the time of secondary heat treatment
For 0.5h～50h.This step can be carried out in electric furnace.The advantage of this step operation is: use two steps
Crystallize method, before this nucleation stage then nucleus growth stage, crystallize is respond well.Above-mentioned steps 4 rises
Warm to the step of 590 DEG C～680 DEG C, heating rate is 5 DEG C/min～10 DEG C/min.
The preparation method of the Surface Crystallization devitrified glass that the present invention provides, with zinc oxide, silicon dioxide and oxygen
Change the frit fusion cast glass such as boron, under suitable heat treating regime, obtain Surface Crystallization glass, can lead to
Cross and control heat treatment temperature and time and obtain the Surface Crystallization glass of different crystallize layer thickness, with satisfied difference
The needs of purposes.The preparation method of this Surface Crystallization devitrified glass need not add any crystallize agent, technique letter
Single, step understands, with low cost, Surface Crystallization is effective.
Below in conjunction with embodiment, the present invention is expanded on further.Raw material components in following example is and rubs
That percentage composition.
Embodiment 1
Glass components is 60%ZnO, 30%B2O3, 10%SiO2, weigh 120g frit,
Raw material mix homogeneously is placed in platinum-rhodium alloy crucible, puts in 1400 DEG C of high temperature furnaces melted 2 hours, so
After melt poured into molding on preheated graphite jig, send into rapidly in annealing furnace after molding, at 550 DEG C
It is incubated 2 hours, cools to room temperature afterwards with the furnace.The glass blocks that glass is cut into 5*5*20mm subsequently is put
Enter at 650 DEG C, to be incubated 5h and obtain Surface Crystallization devitrified glass.With the crystallize layer thickness of scanning electron microscope survey about
53μm.What powder XRD surveyed the thing is become to be mutually heat-treated surface crystallize glass grinding
Zn3(BO3)2, as shown in the embodiment 1 in Fig. 2.
Embodiment 2
Glass components is 60%ZnO, 30%B2O3, 10%SiO2, weigh 120g frit,
Raw material mix homogeneously is placed in platinum-rhodium alloy crucible, puts in 1400 DEG C of high temperature furnaces melted 2 hours, so
After melt poured into molding on preheated graphite jig, send into rapidly in annealing furnace after molding, at 550 DEG C
It is incubated 2 hours, cools to room temperature afterwards with the furnace standby.Subsequently glass is cut into the glass of 5*5*20mm
Block is put into be incubated at 585 DEG C and is raised at 650 DEG C be incubated 5h with 5 DEG C/min again after 2h and obtains Surface Crystallization
Glass, crystallize layer thickness about 65 μm surveyed with scanning electron microscope.Heat-treated surface crystallize glass is ground
Clay into power with XRD survey thing mutually for Zn3(BO3)2, as shown in the embodiment 2 in Fig. 2.
Embodiment 3
Glass components is 60%ZnO, 30%B2O3, 10%SiO2, weigh 120g frit,
Raw material mix homogeneously is poured in platinum-rhodium alloy crucible, puts in 1400 DEG C of high temperature furnaces melted 2 hours, so
After melt poured into molding on preheated graphite jig.Subsequently glass is cut into the glass of 5*5*20mm
Block is put into insulation 10h at 650 DEG C and is obtained Surface Crystallization glass, with the crystallize layer thickness of scanning electron microscope survey about
120μm.What powder XRD surveyed the thing is become to be mutually heat-treated surface crystallize glass grinding
Zn3(BO3)2, as shown in the embodiment 3 in Fig. 2.
Embodiment 4
Glass components is 60%ZnO, 30%B2O3, 10%SiO2, weigh 120g frit,
Raw material mix homogeneously is poured in platinum-rhodium alloy crucible, puts in 1300 DEG C of high temperature furnaces and melt 2.5 hours,
Then melt is poured into molding on preheated graphite jig.Subsequently glass is cut into the glass of 5*5*20mm
Glass block is put into insulation 15h at 650 DEG C and is obtained Surface Crystallization glass, and the crystallize layer thickness surveyed with scanning electron microscope is big
About 156 μm.What powder XRD surveyed the thing is become to be mutually heat-treated surface crystallize glass grinding
Zn3(BO3)2, as shown in the embodiment 4 in Fig. 2.
Embodiment 5
Glass components is 60%ZnO, 30%B2O3, 10%SiO2, weigh 120g frit,
Raw material mix homogeneously is poured in platinum-rhodium alloy crucible, puts in 1500 DEG C of high temperature furnaces melted 2 hours, so
After melt poured into molding on preheated graphite jig, send into rapidly in annealing furnace after molding, at 550 DEG C
It is incubated 2 hours, cools to room temperature afterwards with the furnace standby.Subsequently glass is cut into the glass of 5*5*20mm
Block is put into insulation 20h at 650 DEG C and is obtained Surface Crystallization glass, with the crystallize layer thickness of scanning electron microscope survey about
360μm.What powder XRD surveyed the thing is become to be mutually heat-treated surface crystallize glass grinding
Zn3(BO3)2, as shown in the embodiment 5 in Fig. 2.
By in Fig. 2 it can be seen that under conditions of heat treatment temperature determines, along with the increasing of heat treatment time
The intensity adding devitrification of glass is increasing, such as embodiment 1,3,4,5.It can also be seen that from Fig. 2:
When other conditions are identical, two-step method heat treatment is higher than the crystal intensity that one-step method heat treatment separates out, and ratio is strictly according to the facts
Execute example 1 and embodiment 2.
Embodiment 6
Glass components is 55%ZnO, 35%B2O3, 5%SiO2, 5%Na2O, weighs 200g glass
Glass raw material, pours into raw material mix homogeneously in platinum-rhodium alloy crucible, puts into and melts 1 in 1400 DEG C of high temperature furnaces
Hour, then melt is poured into molding on preheated graphite jig, sends into rapidly in annealing furnace after molding,
It is incubated 0.5～2 hour at 530 DEG C, cools to room temperature afterwards with the furnace.Subsequently glass is cut into 5*5*20mm
Glass blocks put at 640 DEG C be incubated 20h obtain Surface Crystallization glass, with scanning electron microscope survey crystallize thickness
Degree about 180 μm.
Embodiment 7
Glass components is 50%ZnO, 30%B2O3, 10%SiO2, 10%Na2O, weighs 200g
Frit, pours into raw material mix homogeneously in platinum-rhodium alloy crucible, puts in 1350 DEG C of high temperature furnaces melted
1 hour into, then melt is poured molding on preheated graphite jig, sends into rapidly in annealing furnace after molding,
It is incubated 0.5～2 hour at 550 DEG C, cools to room temperature afterwards with the furnace.Subsequently glass is cut into 5*5*20mm
Glass blocks put at 640 DEG C be incubated 30h obtain Surface Crystallization glass, with scanning electron microscope survey crystallize thickness
Degree about 385 μm.
Embodiment 8
Glass components is 60%ZnO, 20B2O3, 8%SiO2, 10%Na2O, 2%Al2O3, weigh
120g frit, pours into raw material mix homogeneously in platinum-rhodium alloy crucible, puts in 1500 DEG C of high temperature furnaces
Melted 1 hour into, then melt is poured molding on preheated graphite jig, send into rapidly after molding and move back
In stove, it is incubated 0.5～2 hour at 560 DEG C, cools to room temperature afterwards with the furnace.Subsequently glass is cut into
The glass blocks of 5*5*20mm is put into insulation 5h at 660 DEG C and is obtained Surface Crystallization glass, surveys with scanning electron microscope
Crystallize layer thickness about 150 μm.
Embodiment 9
Glass components is 45%ZnO, 40%B2O3, 15%SiO2, weigh 120g frit,
Raw material mix homogeneously is poured in platinum-rhodium alloy crucible, puts in 1500 DEG C of high temperature furnaces melted 3 hours, so
After melt poured into molding on preheated graphite jig, send into rapidly in annealing furnace after molding, at 550 DEG C
It is incubated 0.5～2 hour, cools to room temperature afterwards with the furnace.Subsequently glass is cut into the glass blocks of 5*5*20mm
Put into be incubated at 585 DEG C and be raised at 660 DEG C be incubated 10h with 5 DEG C/min after 2h and obtain Surface Crystallization glass,
Crystallize layer thickness about 290 μm surveyed with scanning electron microscope.
Embodiment 10
Glass components is 45%ZnO, 40%B2O3, 5%SiO2, 6%Na2O, 4%Al2O3, claim
Take 120g frit, raw material mix homogeneously is poured in platinum-rhodium alloy crucible, put into 1500 DEG C of high temperature furnaces
In melted 3 hours, then melt is poured into molding on preheated graphite jig, sends into rapidly after molding
In annealing furnace, it is incubated 2 hours at 550 DEG C, cools to room temperature afterwards with the furnace.Subsequently glass is cut into
The glass blocks of 5*5*20mm is put into insulation 15h at 660 DEG C and is obtained Surface Crystallization glass, surveys with scanning electron microscope
Crystallize layer thickness about 642 μm.
Embodiment 11
Glass components is 60%ZnO, 30%B2O3, 10%SiO2, weigh 120g frit,
Raw material mix homogeneously is poured in platinum-rhodium alloy crucible, puts in 1350 DEG C of high temperature furnaces melted 2 hours, so
After melt poured into molding on preheated graphite jig, send into rapidly in annealing furnace after molding, at 550 DEG C
It is incubated 2 hours, cools to room temperature afterwards with the furnace.The glass blocks that glass is cut into 5*5*20mm subsequently is put
Enter to put into be incubated at 585 DEG C and be raised at 660 DEG C be incubated 20h with 5 DEG C/min after 2h and obtain Surface Crystallization glass
Glass, crystallize layer thickness about 857 μm surveyed with scanning electron microscope.
Embodiment 12
Glass components is 30%ZnO, 50%B2O3, 15%SiO2, 4%Na2O, 1%Al2O3, claim
Take 120g frit, raw material mix homogeneously is poured in platinum-rhodium alloy crucible, put into 1500 DEG C of high temperature rise
Fall stove melts 2 hours, then melt is poured into molding on preheated graphite jig, after molding rapidly
In feeding annealing furnace, it is incubated 2 hours at 550 DEG C, cools to room temperature afterwards with the furnace.Subsequently glass is cut into
The glass blocks of 5*5*20mm is put into insulation 30h at 660 DEG C and is obtained Surface Crystallization glass, surveys with scanning electron microscope
Crystallize layer thickness about 1052 μm.Referring to Fig. 1 is Surface Crystallization glass prepared by the present embodiment, should
In figure, A represents crystallize layer, and B represents mother glass.
Embodiment 13
Glass components is 30%ZnO, 50%B2O3, 15%SiO2, 4%Na2O, 1%Al2O3, claim
Take 120g frit, raw material mix homogeneously is poured in platinum-rhodium alloy crucible, put into 1500 DEG C of high temperature furnaces
In melted 2 hours, then melt is poured into molding on preheated graphite jig, sends into rapidly after molding
In annealing furnace, it is incubated 2 hours at 550 DEG C, cools to room temperature afterwards with the furnace.Subsequently glass is cut into
The glass blocks of 5*5*20mm is put into insulation 50h at 650 DEG C and is obtained Surface Crystallization glass, surveys with scanning electron microscope
Crystallize layer thickness about 80 μm.
Embodiment 14
Glass components is 30%ZnO, 50%B2O3, 15%SiO2, 4%Na2O, 1%Al2O3, claim
Take 120g frit, raw material mix homogeneously is poured in platinum-rhodium alloy crucible, put into 1500 DEG C of high temperature furnaces
In melted 2 hours, then melt is poured into molding on preheated graphite jig.Subsequently glass is cut into
The glass blocks of 5*5*20mm is put into insulation 70h at 620 DEG C and is obtained Surface Crystallization glass, surveys with scanning electron microscope
Crystallize layer thickness about 100 μm.
The above is only the preferred embodiment of the present invention, it is noted that general for the art
For logical technical staff, under the premise without departing from the principles of the invention, it is also possible to make some improvement and profit
Decorations, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (8)
1. the preparation method of a Surface Crystallization devitrified glass, it is characterised in that including:
Step 1, offer raw material, described raw material includes that mol ratio is (25～60): (5～50): (5～30)
Zinc oxide, boron oxide and silicon dioxide；Described raw mill is mixed；
The heating of step 2, raw material step 1 obtained is founded, and obtains vitreous humour；
Step 3, vitreous humour step 2 obtained are shaped and make annealing treatment, and obtain intermediate products；
Step 4, intermediate products step 3 obtained carry out heat treatment, obtain Surface Crystallization devitrified glass.
Preparation method the most according to claim 1, it is characterised in that described raw material also includes oxidation
Aluminum and/or sodium oxide；Described aluminium oxide is (0～4) with the mol ratio of described zinc oxide: (25～60)；
Described sodium oxide is (0～20) with the mol ratio of described zinc oxide: (25～60).
Preparation method the most according to claim 1, it is characterised in that described step 2 particularly as follows:
Raw material step 1 obtained is heated to 1100 DEG C～1500 DEG C, is incubated 0.5h～3h, obtains vitreous humour.
Preparation method the most according to claim 1, it is characterised in that described step 3 particularly as follows:
The vitreous humour that step 2 is obtained molding on preheated graphite jig, after molding
It is incubated 0.5h～2h at 450 DEG C～580 DEG C, is then cooled to room temperature, obtains intermediate products.
Preparation method the most according to claim 1, it is characterised in that described step 4 particularly as follows:
Intermediate products step 3 obtained are warming up to 590 DEG C～680 DEG C, are incubated 0.5h～70h.
Preparation method the most according to claim 1, it is characterised in that described step 4 particularly as follows:
Intermediate products step 3 obtained are heat treatment 0.5h～3h at 450 DEG C～630 DEG C；Heat up the most again
Carrying out secondary heat treatment to 590 DEG C～680 DEG C, the time of described secondary heat treatment is 0.5h～50h.
7. according to the preparation method described in claim 5 or 6, it is characterised in that described in be warming up to
In the step of 590 DEG C～680 DEG C, heating rate is 5 DEG C/min～10 DEG C/min.
Preparation method the most according to claim 1, it is characterised in that also include miscellaneous in described raw material
Matter, described impurity includes sulfate, chloride, phosphate, calcium, lead and ferrum, and its content summation is little
2wt% in raw material；Or, described raw material includes nitrate, chloride, sulfate, manganese, lead and ferrum,
Its content summation is not more than the 2wt% of raw material；Or, described raw material includes chloride, ferrum and Fluohydric acid. not
Volatile matter, its content summation is not more than the 4wt% of raw material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106746676A (en) * | 2017-01-19 | 2017-05-31 | 内蒙古科技大学 | A kind of Surface Crystallization devitrified glass containing rare earth and preparation method and application |
| CN111592226A (en) * | 2019-02-21 | 2020-08-28 | 佛山市顺德区美的电热电器制造有限公司 | Preparation method of high borosilicate glass, high borosilicate glass and application thereof |
| US20220250970A1 (en) * | 2019-06-14 | 2022-08-11 | Nipro Corporation | Coating film-attached glass, production method therefor, and modified glass substrate |
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| US4322205A (en) * | 1980-11-26 | 1982-03-30 | The United States Of America As Represented By The United States Department Of Energy | Regenerative air heater |
| CN102992628A (en) * | 2012-11-29 | 2013-03-27 | 江苏宜达光电科技有限公司 | Preparation method for microcrystalline glass without nucleation agent |
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| CN106746676A (en) * | 2017-01-19 | 2017-05-31 | 内蒙古科技大学 | A kind of Surface Crystallization devitrified glass containing rare earth and preparation method and application |
| CN111592226A (en) * | 2019-02-21 | 2020-08-28 | 佛山市顺德区美的电热电器制造有限公司 | Preparation method of high borosilicate glass, high borosilicate glass and application thereof |
| US20220250970A1 (en) * | 2019-06-14 | 2022-08-11 | Nipro Corporation | Coating film-attached glass, production method therefor, and modified glass substrate |
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