CN109293246A - A kind of preparation method of high insulated heat seal glass - Google Patents
A kind of preparation method of high insulated heat seal glass Download PDFInfo
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- CN109293246A CN109293246A CN201811266354.5A CN201811266354A CN109293246A CN 109293246 A CN109293246 A CN 109293246A CN 201811266354 A CN201811266354 A CN 201811266354A CN 109293246 A CN109293246 A CN 109293246A
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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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
Abstract
The present invention relates to a kind of preparation methods of high insulated heat seal glass, belong to glass material preparation technical field.Calcined product is made using poplar sawdust and Adlerika as raw material first in the present invention, calcined product is mixed with tetra isopropyl two (dioctyl phosphito acyloxy) titanate esters and carries out microbial fermentation and obtains modified filter cake, high insulated heat seal glass finally is made in modified filter cake and the melting of each metal oxide high-temperature, the present invention mixes magnesium sulfate with poplar sawdust, copper powder is then added, generate porous magnesia, copper oxide, utilize magnesia and the good electrical insulating property of copper oxide, thermal insulation is to enhance the insulating properties and thermal insulation of seal glass, using titanate esters to porous modified oxidized magnesium, copper oxide is coated, improve the molecule cross-link density of seal glass, titanate esters have good insulating properties and heat-proof quality simultaneously, further increase the electrical isolation and heat insulation of seal glass, it has a good application prospect.
Description
Technical field
The present invention relates to a kind of preparation methods of high insulated heat seal glass, belong to glass material preparation technical field.
Background technique
It is largely each using thermal resistance, heating device and signal connector etc. with the high speed development of modern industrial production
Kind function element, carries out the control and measurement of the parameters such as temperature, pressure, electromagnetism, this is allowed for encapsulating material and sealing technique
Requirement it is higher and higher, it is desirable that it is with high reliability, high temperature resistant, high pressure resistant, anti-oxidant, corrosion-resistant, high sealing, high insulation etc.
Advantage, especially compared with fields such as harsh environments such as high temperature, high pressure, oil-gas mining.
Currently used encapsulating method has glue sealing, metal welded seal, ceramic welding sealing and glass solder sealing
Deng.The main components such as glue and epoxy glue are organic material, exist or grow or short digestion period, old with organic material
Change, just will affect the sealing performance of sealing material.Metal welded seal needs to pass through tin again after optical fiber surface to be plated to metal layer
Weldering is sealed, and technology difficulty is big, at high cost.Compared to other seal, sealing materials, seal glass is because of the features such as durable, secured, quilt
It is widely used in sealing-in instrument and meter or electronic component.
Seal glass be it is a kind of be commonly used in sealing of metal, nonmetallic or ceramic material, be glass, ceramics, gold
The middle layer glass that category and composite material etc. seal up each other, can be divided into low temperature sealing glass and high temperature seal glass.
Seal glass mainly has the glass of the systems such as lead boron, phosphate, vanadate, bismuthates, tellurate.Wherein, due to the pollution of lead
Problem, unleaded sealing-in solder is the following inevitable development trend.Resistance to pressure, the insulating properties, height of common barium crown sealed glass at present
Warm leakproofness, long-time stability and reliability are poor, and thermal expansion coefficient is smaller.Vanadate, bismuthates, tellurate seal glass
Due to resource and price problem, there are certain disadvantages.The seal glass of phosphate system is most promising, but phosphate glass
That there are chemical stabilization is poor for glass, and is combined with silicate glass sealing that there are the coefficients of expansion and the plate glass of sealing-in not to match that,
The problems such as easy to crack after encapsulation.
Therefore, it needs to develop a kind of barium crown sealed glass, it, can while not to human health and environmental effects
Applied to high-pressure electronic field.
Summary of the invention
The technical problems to be solved by the invention:, mechanical property bad for current seal glass heat-insulating property, electric conductivity
The defect of energy difference, provides a kind of preparation method of high insulated heat seal glass.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of high insulated heat seal glass, it is characterised in that specific preparation step are as follows:
(1) it weighs in poplar sawdust and Adlerika 1:5 in mass ratio investment reaction kettle, reactor temperature is increased to,
It is filled with nitrogen and increases air pressure in kettle, closed reactor, constant temperature and pressure, which reacts, is made mixed serum；
(2) the fine copper powder of mixed serum quality 5~8% is added into reaction kettle, is mixed with blender and mixed liquor is made,
It is added dropwise sodium carbonate liquor into reaction kettle in whipping process, adjusts pH value to 9~10, thermostatic reaction in heating kettle, instead
Should after filter residue is obtained by filtration；
(3) above-mentioned filter residue is placed in Muffle furnace for 3~5 times wash with distilled water, increases temperature progress high temperature in Muffle furnace and forges
It burns, mixed grinding in planetary ball mill is put into after calcining, calcined product is made；
(4) according to parts by weight, 8~10 parts of above-mentioned calcined products, 1.0~1.2 parts of two (dioctyl phosphitos of tetra isopropyl are weighed
Acyloxy) in titanate esters and 15~17 parts of acetone investment beakers, sonic oscillation in sonic oscillation instrument is placed the beaker, mixing is made
Product；
(5) above-mentioned mix products are placed in tube furnace, argon gas is passed through into tube furnace, increased thermostatic reaction in managing and be made
Reaction product weighs 8~10 parts of reaction products, 2~3 parts of starch, 4~6 portions of soybean and 16~18 parts of water and throws according to parts by weight
Enter in fermentor, fermentor is placed in a greenhouse ferment at constant temperature, modified filter cake is obtained by filtration after fermentation；
(6) according to parts by weight, 9~11 parts of above-mentioned modified filter cakes, 16~18 parts of silica, 2~3 part of three oxidation two are weighed
Grinding is equal in antimony, 1~2 part of bismuth oxide, 1.5~1.7 parts of aluminium oxide, 5~7 parts of boric acid and 6~8 parts of water investment corundum crucibles
It is even, corundum crucible is placed in Elema resistance furnace, in-furnace temperature preheating is increased, heating progress calcining at constant temperature obtains after preheating
To molten product, molten product is poured into mold, cooled to room temperature is up to high insulated heat seal glass.
The mass fraction of Adlerika as described in step (1) is 14~16%, and the temperature in reaction kettle is increased to 220
~240 DEG C, air pressure is increased to 2.2~2.4MPa in kettle, and constant temperature and pressure reacts 30~40min.
The revolving speed of blender described in step (2) is 500~550r/mi, and mixing time is 40~50min, carbon
The mass fraction of acid sodium solution is 15~17%, and reactor temperature is increased to 280~300 DEG C, the isothermal reaction time is 50~
60min。
Temperature is increased to 600~650 DEG C in Muffle furnace described in step (3), and the high-temperature calcination time is 40~50min,
Revolving speed in planetary ball mill is 400~450r/min, and the mixed grinding time is 150~160min.
Frequency in sonic oscillation instrument described in step (4) is 32~34kHz, and the sonic oscillation time is 3~4h.
The rate that argon gas is passed through in tube furnace described in step (5) is 8~10 DEG C/min, is warming up to 300 in tube furnace
~350 DEG C, the isothermal reaction time is 60~80min, and the temperature in greenhouse is 38~42 DEG C, and the ferment at constant temperature time is 7~9 days.
Temperature is increased to 950~1000 DEG C in Elema resistance furnace described in step (6), and preheating time is 50~
60min, for warming temperature to 1200~1300 DEG C, the calcining at constant temperature time is 60~80min again.
The method have the benefit that:
(1) present invention, which first mixes poplar sawdust with Adlerika, carries out the obtained mixed serum of high temperature high pressure process, then
The stirring of fine copper powder is added into mixed serum, then adjusts pH value to alkalinity and is heated at high temperature, filter residue is obtained by filtration, then will
Calcined product is made in filter residue high-temperature calcination, and calcined product and (dioctyl phosphito acyloxy) titanate esters of tetra isopropyl two is mixed
It closes, carries out pyroreaction after mixing, be mixed into soybean, starch progress microbial fermentation, modified filter cake is obtained by filtration, will finally be modified
Filter cake and each metal oxide high-temperature melting mixing, are made high insulated heat seal glass after natural cooling, and the present invention is by sulphur
Sour magnesium is mixed with poplar sawdust, and high temperature and pressure decomposes sawdust, generates furfural substance, decomposes lignin, generates carboxyl, hydroxyl etc.
Hat can roll into a ball, and magnesium ion generation complexing and ionic bond absorption, make magnesium ion sufficiently with the organic substance that is decomposed in sawdust
In conjunction with, copper powder is then added, using displacement react, displace part magnesium ion, make copper ion be incorporated into sawdust decompose gained have
In machine object, being overregulated pH value to alkalinity makes magnesium ion, copper ion generate magnesium hydroxide, Kocide SD, makes by high-temperature heating
Magnesium hydroxide, Kocide SD, which decompose, generates magnesia and copper oxide, while high-temperature heating makes organic material decomposition generate titanium dioxide
Carbon volatilization, generates porous magnesia, copper oxide, improves degree of roughness, increases other molecules in specific surface area, with seal glass
Exposure level increase, using magnesia and the good electrical insulating property of copper oxide, thermal insulation with enhance seal glass insulating properties and
Thermal insulation；
(2) present invention coats porous modified oxidized magnesium, copper oxide using titanate esters, makes to seal using the stability of titanyl key
The stability for connecing glass is improved, and magnesia oxidizes metal its in object and seal glass by metatitanic acid is ester modified with copper oxide
The contact action of its molecule is reinforced, and the molecule cross-link density of seal glass is improved, to effectively reinforce the mechanical property of seal glass
Can, while titanate esters have good insulating properties and heat-proof quality, further increase the electrical isolation and heat insulation of seal glass,
It has a good application prospect.
Specific embodiment
The Adlerika 1:5 in mass ratio that poplar sawdust and mass fraction are 14~16% is weighed to put into reaction kettle, it will
Reactor temperature is increased to 220~240 DEG C, and being filled with air pressure in nitrogen raising kettle, to 2.2~2.4MPa, closed reactor is permanent
Warm constant pressure reacts 30~40min, and mixed serum is made；The fine copper powder of mixed serum quality 5~8% is added into reaction kettle, uses
Blender is mixed 40~50min with the revolving speed of 500~550r/min and mixed liquor is made, in whipping process into reaction kettle
The sodium carbonate liquor that mass fraction is 15~17% is added dropwise, adjusts pH value to 9~10, heating temperature in the kettle is permanent to 280~300 DEG C
Temperature 50~60min of reaction, is obtained by filtration filter residue after reaction；Above-mentioned filter residue is placed on Muffle furnace 3~5 times wash with distilled water
In, it increases temperature in Muffle furnace and is put into planetary ball mill after calcining with 400 to 600~650 DEG C, 40~50min of high-temperature calcination
Calcined product is made in 150~160min of revolving speed mixed grinding of~450r/min；According to parts by weight, weigh 8~10 parts it is above-mentioned
Calcined product, 1.0~1.2 parts of (dioctyl phosphito acyloxy) titanate esters of tetra isopropyl two and 15~17 parts of acetone put into beaker
In, it places the beaker in sonic oscillation instrument, 3~4h is vibrated with the frequency ultrasound of 32~34kHz, mix products are made；It will be above-mentioned
Mix products are placed in tube furnace, and argon gas is passed through into tube furnace, are warming up to 300~350 DEG C with the rate of 8~10 DEG C/min,
Reaction product is made after 60~80min of isothermal reaction and weighs 8~10 parts of reaction products, 2~3 parts of starch, 4 according to parts by weight
~6 portions of soybean and 16~18 parts of water put into fermenter, and fermentor are placed in the greenhouse that temperature is 38~42 DEG C, ferment at constant temperature
7~9 days, modified filter cake is obtained by filtration after fermentation；According to parts by weight, 9~11 parts of above-mentioned modified filter cakes, 16~18 part two are weighed
Silica, 2~3 parts of antimony oxides, 1~2 part of bismuth oxide, 1.5~1.7 parts of aluminium oxide, 5~7 parts of boric acid and 6~8 parts
Water puts into grinding in corundum crucible and uniformly, corundum crucible is placed in Elema resistance furnace, increases in-furnace temperature to 950~1000
DEG C, 50~60min is preheated, 1200~1300 DEG C are warming up to after preheating, 60~80min of calcining at constant temperature obtains molten product,
Molten product is poured into mold, cooled to room temperature is up to high insulated heat seal glass.
Example 1
The Adlerika 1:5 in mass ratio that poplar sawdust and mass fraction are 14% is weighed to put into reaction kettle, it will be in reaction kettle
Temperature is increased to 220 DEG C, is filled with nitrogen and increases in kettle that air pressure is to 2.2MPa, closed reactor, constant temperature and pressure reacts 30min, system
Obtain mixed serum；The fine copper powder of mixed serum quality 5% is added into reaction kettle, it is mixed with the revolving speed of 500r/min with blender
It closes stirring 40min and mixed liquor is made, the sodium carbonate liquor that mass fraction is 15% is added dropwise into reaction kettle in whipping process, adjusts
PH value is saved to 9, heats temperature in the kettle to 280 DEG C, filter residue is obtained by filtration after reaction in isothermal reaction 50min；Above-mentioned filter residue is steamed
Distilled water is cleaned 3 times and is placed in Muffle furnace, is increased temperature in Muffle furnace and is put into row after calcining to 600 DEG C, high-temperature calcination 40min
Calcined product is made with the revolving speed mixed grinding 150min of 400r/min in celestial body grinding machine；According to parts by weight, weigh 8 parts it is above-mentioned
In calcined product, 1.0 parts of (dioctyl phosphito acyloxy) titanate esters of tetra isopropyl two and 15 parts of acetone investment beakers, by beaker
It is placed in sonic oscillation instrument, 3h is vibrated with the frequency ultrasound of 32kHz, mix products are made；Above-mentioned mix products are placed in tubular type
In furnace, it is passed through argon gas into tube furnace, is warming up to 300 DEG C with the rate of 8 DEG C/min, reaction is made after isothermal reaction 60min and produces
Object weighs 8 parts of reaction products, 2 parts of starch, 4 portions of soybean and 16 parts of water and puts into fermenter, by fermentor according to parts by weight
It is placed in the greenhouse that temperature is 38 DEG C, ferment at constant temperature 7 days, modified filter cake is obtained by filtration after fermentation；According to parts by weight, 9 are weighed
Part above-mentioned modified filter cake, 16 parts of silica, 2 parts of antimony oxides, 1 part of bismuth oxide, 1.5 parts of aluminium oxide, 5 parts of boric acid and
Uniformly, corundum crucible is placed in Elema resistance furnace for grinding in 6 parts of water investment corundum crucibles, increases in-furnace temperature to 950 DEG C,
50min is preheated, 1200 DEG C are warming up to after preheating, calcining at constant temperature 60min obtains molten product, and molten product is poured into mold
In, cooled to room temperature is up to high insulated heat seal glass.
Example 2
The Adlerika 1:5 in mass ratio that poplar sawdust and mass fraction are 15% is weighed to put into reaction kettle, it will be in reaction kettle
Temperature is increased to 230 DEG C, is filled with nitrogen and increases in kettle that air pressure is to 2.3MPa, closed reactor, constant temperature and pressure reacts 35min, system
Obtain mixed serum；The fine copper powder of mixed serum quality 7% is added into reaction kettle, it is mixed with the revolving speed of 525r/min with blender
It closes stirring 45min and mixed liquor is made, the sodium carbonate liquor that mass fraction is 16% is added dropwise into reaction kettle in whipping process, adjusts
PH value is saved to 9, heats temperature in the kettle to 290 DEG C, filter residue is obtained by filtration after reaction in isothermal reaction 55min；Above-mentioned filter residue is steamed
Distilled water is cleaned 4 times and is placed in Muffle furnace, is increased temperature in Muffle furnace and is put into row after calcining to 625 DEG C, high-temperature calcination 45min
Calcined product is made with the revolving speed mixed grinding 155min of 425r/min in celestial body grinding machine；According to parts by weight, weigh 9 parts it is above-mentioned
In calcined product, 1.1 parts of (dioctyl phosphito acyloxy) titanate esters of tetra isopropyl two and 16 parts of acetone investment beakers, by beaker
It is placed in sonic oscillation instrument, 3h is vibrated with the frequency ultrasound of 33kHz, mix products are made；Above-mentioned mix products are placed in tubular type
In furnace, it is passed through argon gas into tube furnace, is warming up to 325 DEG C with the rate of 9 DEG C/min, reaction is made after isothermal reaction 70min and produces
Object weighs 9 parts of reaction products, 2 parts of starch, 5 portions of soybean and 17 parts of water and puts into fermenter, by fermentor according to parts by weight
It is placed in the greenhouse that temperature is 40 DEG C, ferment at constant temperature 8 days, modified filter cake is obtained by filtration after fermentation；According to parts by weight, 10 are weighed
Part above-mentioned modified filter cake, 17 parts of silica, 2 parts of antimony oxides, 1 part of bismuth oxide, 1.6 parts of aluminium oxide, 6 parts of boric acid and
Uniformly, corundum crucible is placed in Elema resistance furnace for grinding in 7 parts of water investment corundum crucibles, increases in-furnace temperature to 975 DEG C,
55min is preheated, 1250 DEG C are warming up to after preheating, calcining at constant temperature 70min obtains molten product, and molten product is poured into mold
In, cooled to room temperature is up to high insulated heat seal glass.
Example 3
The Adlerika 1:5 in mass ratio that poplar sawdust and mass fraction are 16% is weighed to put into reaction kettle, it will be in reaction kettle
Temperature is increased to 240 DEG C, is filled with nitrogen and increases in kettle that air pressure is to 2.4MPa, closed reactor, constant temperature and pressure reacts 40min, system
Obtain mixed serum；The fine copper powder of mixed serum quality 8% is added into reaction kettle, it is mixed with the revolving speed of 550r/min with blender
It closes stirring 50min and mixed liquor is made, the sodium carbonate liquor that mass fraction is 17% is added dropwise into reaction kettle in whipping process, adjusts
PH value is saved to 10, heats temperature in the kettle to 300 DEG C, filter residue is obtained by filtration after reaction in isothermal reaction 60min；Above-mentioned filter residue is used
Distilled water is cleaned 5 times and is placed in Muffle furnace, is increased temperature to 650 DEG C, high-temperature calcination 50min in Muffle furnace and is put into after calcining
Calcined product is made with the revolving speed mixed grinding 160min of 450r/min in planetary ball mill；According to parts by weight, 10 parts are weighed
It, will in above-mentioned calcined product, 1.2 parts of (dioctyl phosphito acyloxy) titanate esters of tetra isopropyl two and 17 parts of acetone investment beakers
Beaker is placed in sonic oscillation instrument, vibrates 4h with the frequency ultrasound of 34kHz, mix products are made；Above-mentioned mix products are placed in
In tube furnace, it is passed through argon gas into tube furnace, is warming up to 350 DEG C with the rate of 10 DEG C/min, is made anti-after isothermal reaction 80min
Product is answered, according to parts by weight, 10 parts of reaction products, 3 parts of starch, 6 portions of soybean and 18 parts of water is weighed and puts into fermenter, will send out
Fermentation tank is placed in the greenhouse that temperature is 42 DEG C, and ferment at constant temperature 9 days, modified filter cake is obtained by filtration after fermentation；According to parts by weight, claim
Take 11 parts of above-mentioned modified filter cakes, 18 parts of silica, 3 parts of antimony oxides, 2 parts of bismuth oxides, 1.7 parts of aluminium oxide, 7 parts of boron
Grinding uniformly, corundum crucible is placed in Elema resistance furnace, increases in-furnace temperature extremely in acid and 8 parts of water investment corundum crucibles
1000 DEG C, 60min is preheated, 1300 DEG C are warming up to after preheating, calcining at constant temperature 80min obtains molten product, by molten product
It pours into mold, cooled to room temperature is up to high insulated heat seal glass.
Comparative example
With the seal glass of company of Fuzhou City production as a comparison case to high insulated heat seal glass produced by the present invention and
Seal glass in comparative example is detected, and testing result is as shown in table 1:
Tensile strength test method is tested referring to ASTMD638-2014 standard.
Bending strength test method is tested referring to ASTMD790-2003 standard.
Glass transition temperature and sealing temperature are tested
It is measured using synthesis thermal analyzer, heating rate is 10~30 DEG C/min, and test scope is 25 DEG C~1000 DEG C.
Thermal expansion coefficient test
It is tested using thermomechanical analyzer, by the sealing-in in high insulated heat seal glass produced by the present invention and comparative example
Glass is as sample, after being made into the bar-shaped sample of 100mm or so, rises to 300 DEG C by room temperature, heating rate is 3~5 DEG C/min.
1 performance measurement result of table
According to data in table 1 it is found that high insulated heat seal glass produced by the present invention, has intensity height, conductive, thermal insulation
It is good, sealing-in excellent effect, and the feature of environmental protection is good, thermal expansion coefficient good without poisonous and harmful substances, chemical stabilities such as lead, cadmium, thalliums
It is adjustable in a certain range, suitable for the sealing-in of electronic component, there is wide prospect of the application.
Claims (7)
1. a kind of preparation method of high insulated heat seal glass, it is characterised in that specific preparation step are as follows:
(1) it weighs in poplar sawdust and Adlerika 1:5 in mass ratio investment reaction kettle, reactor temperature is increased to,
It is filled with nitrogen and increases air pressure in kettle, closed reactor, constant temperature and pressure, which reacts, is made mixed serum；
(2) the fine copper powder of mixed serum quality 5~8% is added into reaction kettle, is mixed with blender and mixed liquor is made,
It is added dropwise sodium carbonate liquor into reaction kettle in whipping process, adjusts pH value to 9~10, thermostatic reaction in heating kettle, instead
Should after filter residue is obtained by filtration；
(3) above-mentioned filter residue is placed in Muffle furnace for 3~5 times wash with distilled water, increases temperature progress high temperature in Muffle furnace and forges
It burns, mixed grinding in planetary ball mill is put into after calcining, calcined product is made；
(4) according to parts by weight, 8~10 parts of above-mentioned calcined products, 1.0~1.2 parts of two (dioctyl phosphitos of tetra isopropyl are weighed
Acyloxy) in titanate esters and 15~17 parts of acetone investment beakers, sonic oscillation in sonic oscillation instrument is placed the beaker, mixing is made
Product；
(5) above-mentioned mix products are placed in tube furnace, argon gas is passed through into tube furnace, increased thermostatic reaction in managing and be made
Reaction product weighs 8~10 parts of reaction products, 2~3 parts of starch, 4~6 portions of soybean and 16~18 parts of water and throws according to parts by weight
Enter in fermentor, fermentor is placed in a greenhouse ferment at constant temperature, modified filter cake is obtained by filtration after fermentation；
(6) according to parts by weight, 9~11 parts of above-mentioned modified filter cakes, 16~18 parts of silica, 2~3 part of three oxidation two are weighed
Grinding is equal in antimony, 1~2 part of bismuth oxide, 1.5~1.7 parts of aluminium oxide, 5~7 parts of boric acid and 6~8 parts of water investment corundum crucibles
It is even, corundum crucible is placed in Elema resistance furnace, in-furnace temperature preheating is increased, heating progress calcining at constant temperature obtains after preheating
To molten product, molten product is poured into mold, cooled to room temperature is up to high insulated heat seal glass.
2. a kind of preparation method of high insulated heat seal glass according to claim 1, it is characterised in that: step (1)
Described in the mass fraction of Adlerika be 14~16%, the temperature in reaction kettle is increased to 220~240 DEG C, air pressure in kettle
It is increased to 2.2~2.4MPa, constant temperature and pressure reacts 30~40min.
3. a kind of preparation method of high insulated heat seal glass according to claim 1, it is characterised in that: step (2)
Described in the revolving speed of blender be 500~550r/mi, mixing time is 40~50min, the quality of sodium carbonate liquor point
Number is 15~17%, and reactor temperature is increased to 280~300 DEG C, and the isothermal reaction time is 50~60min.
4. a kind of preparation method of high insulated heat seal glass according to claim 1, it is characterised in that: step (3)
Described in Muffle furnace in temperature be increased to 600~650 DEG C, the high-temperature calcination time is 40~50min, is turned in planetary ball mill
Speed is 400~450r/min, and the mixed grinding time is 150~160min.
5. a kind of preparation method of high insulated heat seal glass according to claim 1, it is characterised in that: step (4)
Described in sonic oscillation instrument in frequency be 32~34kHz, the sonic oscillation time be 3~4h.
6. a kind of preparation method of high insulated heat seal glass according to claim 1, it is characterised in that: step (5)
Described in tube furnace in be passed through the rate of argon gas be 8~10 DEG C/min, be warming up to 300~350 DEG C in tube furnace, isothermal reaction
Time is 60~80min, and the temperature in greenhouse is 38~42 DEG C, and the ferment at constant temperature time is 7~9 days.
7. a kind of preparation method of high insulated heat seal glass according to claim 1, it is characterised in that: step (6)
Described in Elema resistance furnace in temperature be increased to 950~1000 DEG C, preheating time is 50~60min, again warming temperature
To 1200~1300 DEG C, the calcining at constant temperature time is 60~80min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110713346A (en) * | 2019-10-30 | 2020-01-21 | 陕西航空电气有限责任公司 | Inorganic sealing material and application method thereof on ignition nozzle |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110713346A (en) * | 2019-10-30 | 2020-01-21 | 陕西航空电气有限责任公司 | Inorganic sealing material and application method thereof on ignition nozzle |
| CN110713346B (en) * | 2019-10-30 | 2022-06-07 | 陕西航空电气有限责任公司 | Inorganic sealing material and application method thereof on ignition nozzle |
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