CN106430989B - A kind of low melting point glass powder, preparation method and application and the method for preparing compound glass column using low melting point glass powder - Google Patents
A kind of low melting point glass powder, preparation method and application and the method for preparing compound glass column using low melting point glass powder Download PDFInfo
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- C03—GLASS; MINERAL OR SLAG WOOL
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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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Abstract
A kind of low melting point glass powder, preparation method and application and the method for preparing compound glass column using low melting point glass powder, the present invention relates to chemical industry, electronic technology field, and in particular to a kind of low melting point glass powder, preparation method and application and the method for preparing compound glass column using low melting point glass powder.The present invention is to solve existing glass powder poor chemical stabilities, at high cost, it cannot be guaranteed that the good problem of electronic packing piece hermetic seal.A kind of low melting point glass powder is made of by mass fraction stannous oxide, phosphorus pentoxide, zinc oxide, sodium oxide molybdena, barium monoxide, potassium oxide, silica, indium oxide, magnesia, di-iron trioxide, aluminium oxide and strontium oxide strontia.Not only chemical stability is good for low melting point glass powder prepared by the present invention, and linear expansion coefficient is appropriate, leadless environment-friendly, and has lower melt temperature, the hermetic seal of the lead terminal especially suitable for phased-array radar T/R module and highly sophisticated device etc..
Description
Technical field
The present invention relates to chemical industry, electronic technology field, and in particular to a kind of low melting point glass powder, preparation method and application
And the method for using low melting point glass powder preparing compound glass column.
Background technique
The sealing-in of glass and metal, purposes is very extensive, especially in electronics, laser, space flight and aviation and automobile manufacture etc.
There is more application in field.With the wide variety of electronic component, complex-shapedization, to the sealing technology of glass and metal
It is required that higher and higher, it is desirable that closure has good mechanical performance and electric conductivity.In Electronic Packaging field, by low temperature seal skill
When art uses transition sealing technology, it is crucial that the preparation process of compound glass column, includes the system of cryogenic glass powder among these
Standby, compound glass column preparation, several key problems such as positioning sintering fixture design.
Although being all distinctly claimed the use of limitation lead in many laws and regulations, commercial low-melting glass is still so far
Old is based on high pbo glass, because the properties of lead base low-melting glass can meet requirement well: work
Temperature is minimum can be down to 400 DEG C, and controllable crystallization property and special " metal bridge " effect ensure that sealing strength and airtight
Property, relatively low manufacturing cost ensure that the workability of client.In recent years, domestic and foreign scholars to Unlead low-smelting point glass into
It has gone a large amount of research, however has also been difficult to successfully be substituted on a large scale from lead base low-melting glass from the point of view of current result, this is
Due to the manufacturing cost of Unlead low-smelting point glass too high (such as Sn0 base and Bi203Base glass), ingredient contains serious harm in the middle
Substance (such as V of human health205Base glass), while corresponding requirement (such as phosphorus is also not achieved in its chemical stability and operating temperature
Silicate glass).
With the continuous development of science and technology, the especially progress of aeronautical technology, electronic technology and energy technology, makes more next
More electronic device applications miniaturizations, simplifies, diversified and precise treatment, this just wants the air-tightness of closure and firmness
Ask higher and higher.Low melting point glass powder is a kind of specific use glass with low operating temperature, is used extensively in the electronics industry
Sealing-in between the materials such as metal, glass, ceramics and composite material and coating, is assigned on the basis of not damaging properties of product
Give the enough bonding strengths of product and sealing-in air-tightness.Low melting point glass powder is widely used in the gas of electronic component, vacuum device
Sealing connects.
Summary of the invention
The present invention is to solve existing glass powder poor chemical stabilities, at high cost, it cannot be guaranteed that electronic packing piece hermetic seal
The good problem connect, and a kind of low melting point glass powder, preparation method and application are provided and prepared using low melting point glass powder
The method of compound glass column.
A kind of low melting point glass powder is by mass fraction by 30~80 parts of stannous oxides, 20~60 parts of phosphorus pentoxides, 1~5
Part zinc oxide, 0.1~1 part of sodium oxide molybdena, 0.5~1 part of barium monoxide, 0.1~1 part of potassium oxide, 0.1~1 part of silica, 0.1~1
Part indium oxide, 0.1~1 part of magnesia, 0.04 part of di-iron trioxide, 0.03 part of aluminium oxide, 0.01 part of strontium oxide strontia and 0.5~1 part
Active carbon is prepared；The melt temperature of the low melting point glass powder be 490 DEG C~550 DEG C, transition temperature be 375 DEG C~
385 DEG C, softening temperature is 425 DEG C~435 DEG C, and the low melting point glass powder is flat under the conditions of temperature is 20 DEG C~300 DEG C
Equal linear expansion coefficient is 73 × 10-7/ DEG C~79 × 10-7/℃。
A kind of preparation method of low melting point glass powder is specifically to follow the steps below:
One, 30~80 parts of stannous oxides, 20~60 parts of phosphorus pentoxides, 1~5 part of zinc oxide, 0.1 are weighed in parts by weight
~1 part of sodium oxide molybdena, 0.5~1 part of barium monoxide, 0.1~1 part of potassium oxide, 0.1~1 part of silica, 0.1~1 part of indium oxide, 0.1
~1 part of magnesia, 0.04 part of di-iron trioxide, 0.03 part of aluminium oxide, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon；
Two, by weighed 30~80 parts of stannous oxides of step 1,20~60 parts of phosphorus pentoxides, 1~5 part of zinc oxide, 0.1
~1 part of sodium oxide molybdena, 0.5~1 part of barium monoxide, 0.1~1 part of potassium oxide, 0.1~1 part of silica, 0.1~1 part of indium oxide, 0.1
After~1 part of magnesia, 0.04 part of di-iron trioxide, 0.03 part of aluminium oxide, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon mixing
It is put into corundum crucible, is subsequently placed in 202-2 type thermostatic drying chamber, with the heating rate of 2 DEG C/min by the temperature of drying box
From room temperature to 220 DEG C, and 1h is kept the temperature under conditions of temperature is 220 DEG C, obtains block mixture；
Three, block mixture is ground into powder, be then placed again into corundum crucible, being subsequently placed in temperature is 800 DEG C
In~850 DEG C of high temperature box type resistance furnace, with the heating rate of 5 DEG C/min by the temperature of high temperature box type resistance furnace from 800 DEG C~
850 DEG C are warming up to 1150 DEG C, and the glass of melting is cast in clean steel after heat preservation 2h under conditions of temperature is 1150 DEG C
On molding jig, cooled to room temperature makes annealing treatment the glass cooled down to be put into Muffle furnace, annealing temperature 320
DEG C, the glass after annealing is fitted into planetary ball mill by annealing time 1h, with the speed ball milling 1h of 500r/min, is obtained
Evengranular oxide powder, i.e., low melting point glass powder.
The low melting point glass powder is for high temp glass column respectively between aluminium alloy, high sial or aluminum matrix composite
Stick to each other, the leak rate after adhesion are lower than 10-8Pa·m3/s。
The low melting point glass powder is used for the sealing-in of electronic vacuum component, and the leak rate after sealing-in is lower than 10-8Pa·m3/s。
Hermetic seal of the low melting point glass powder for phased-array radar T/R module and the lead terminal of highly sophisticated device
It connects, the leak rate after sealing-in is lower than 10-8Pa·m3/s。
It is specifically to follow the steps below using the method that above-mentioned low melting point glass powder prepares compound glass column:
One layer of low melting point glass powder is coated in the outer surface of glass insulation terminal, is subsequently placed in sintering furnace, by sintering furnace
Temperature in 40min from room temperature to 436 DEG C, temperature be 436 DEG C under conditions of heat preservation 30min after, cool to the furnace
300 DEG C of taking-ups, obtain compound glass column.
The beneficial effects of the present invention are:
Not only chemical stability is good for low melting point glass powder prepared by the present invention, and linear expansion coefficient is appropriate, leadless environment-friendly, and
With lower melt temperature, melt temperature is 490~550 DEG C, 20~300 DEG C of average linear coefficients of expansion 76 ± 3 × 10-7/ DEG C, 380 ± 5 DEG C of transition temperature, 430 ± 5 DEG C of softening temperature.Glass powder of the present invention be suitable for high temp glass column and aluminium alloy,
Stick to each other between high sial and aluminum matrix composite, the cold-resistant thermal shock of device after adhesion, matching is good, in formula not
Containing precious metal, cost of material is low, and operating procedure is simple, industrialized production easy to accomplish, no poisonous and harmful element, to environment
Pollution is not constituted.Suitable for the sealing-in of electrovacuum component, especially suitable for phased-array radar T/R module and highly sophisticated device etc.
Lead terminal hermetic seal, provide guarantee for the large-scale production and popularization and application of T/R module.
The present invention is by optimization and adjusts the proportion of low melting point glass powder each component and adds the transition gold of proper specific gravity
Belong to oxide, to significantly reduce its temperature for melting sealing-in；Meanwhile by adjusting the type of low-expansion material and
Content can reasonably adjust its low-expansion coefficient, it is made to be more nearly the coefficient of expansion of basis material to be packaged.Therefore, energy
Enough realize good, the reliable hermetic seal of electronic packing piece.
Specific embodiment
Specific embodiment 1: a kind of low melting point glass powder of present embodiment is sub- by 30~80 parts of oxidations by mass fraction
Tin, 20~60 parts of phosphorus pentoxides, 1~5 part of zinc oxide, 0.1~1 part of sodium oxide molybdena, 0.5~1 part of barium monoxide, 0.1~1 part of oxidation
Potassium, 0.1~1 part of silica, 0.1~1 part of indium oxide, 0.1~1 part of magnesia, 0.04 part of di-iron trioxide, 0.03 part of oxidation
Aluminium, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon are prepared；The melt temperature of the low melting point glass powder be 490 DEG C~
550 DEG C, transition temperature is 375 DEG C~385 DEG C, and softening temperature is 425 DEG C~435 DEG C, and the low melting point glass powder is in temperature
It is 73 × 10 for the average linear expansion coefficient under the conditions of 20 DEG C~300 DEG C-7/ DEG C~79 × 10-7/℃。
Specific embodiment 2: the present embodiment is different from the first embodiment in that: low melting point glass powder presses quality
Number is by 55.96 parts of stannous oxides, 39.86 parts of phosphorus pentoxides, 1.58 parts of zinc oxide, 0.77 part of sodium oxide molybdena, 0.65 part of oxidation
Barium, 0.43 part of potassium oxide, 0.32 part of silica, 0.21 part of indium oxide, 0.14 part of magnesia, 0.04 part of di-iron trioxide,
0.03 part of aluminium oxide, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon are prepared.Other are same as the specific embodiment one.
Specific embodiment 3: the preparation method of the low melting point glass powder of present embodiment is specifically to follow the steps below
:
One, 30~80 parts of stannous oxides, 20~60 parts of phosphorus pentoxides, 1~5 part of zinc oxide, 0.1 are weighed in parts by weight
~1 part of sodium oxide molybdena, 0.5~1 part of barium monoxide, 0.1~1 part of potassium oxide, 0.1~1 part of silica, 0.1~1 part of indium oxide, 0.1
~1 part of magnesia, 0.04 part of di-iron trioxide, 0.03 part of aluminium oxide, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon；
Two, by weighed 30~80 parts of stannous oxides of step 1,20~60 parts of phosphorus pentoxides, 1~5 part of zinc oxide, 0.1
~1 part of sodium oxide molybdena, 0.5~1 part of barium monoxide, 0.1~1 part of potassium oxide, 0.1~1 part of silica, 0.1~1 part of indium oxide, 0.1
After~1 part of magnesia, 0.04 part of di-iron trioxide, 0.03 part of aluminium oxide, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon mixing
It is put into corundum crucible, is subsequently placed in 202-2 type thermostatic drying chamber, with the heating rate of 2 DEG C/min by the temperature of drying box
From room temperature to 220 DEG C, and 1h is kept the temperature under conditions of temperature is 220 DEG C, obtains block mixture；
Three, block mixture is ground into powder, be then placed again into corundum crucible, being subsequently placed in temperature is 800 DEG C
In~850 DEG C of high temperature box type resistance furnace, with the heating rate of 5 DEG C/min by the temperature of high temperature box type resistance furnace from 800 DEG C~
850 DEG C are warming up to 1150 DEG C, and the glass of melting is cast in clean steel after heat preservation 2h under conditions of temperature is 1150 DEG C
On molding jig, cooled to room temperature makes annealing treatment the glass cooled down to be put into Muffle furnace, annealing temperature 320
DEG C, the glass after annealing is fitted into planetary ball mill by annealing time 1h, with the speed ball milling 1h of 500r/min, is obtained
Evengranular oxide powder, i.e., low melting point glass powder.
In the low melting point glass powder of present embodiment preparation, SnO is the auxiliary material of glass.ZnO can reduce the heat of glass
The coefficient of expansion improves the chemical stability of glass, refractive index.SiO2Addition can reduce the tendency towards devitrification of glass, improve glass
Chemical stability, thermal stability, mechanical strength, hardness and refractive index, glass expansion coefficient can be adjusted.K20 is network
Modifier oxides can reduce the glass melting temperature of glass, improve glass expansion coefficient, increase the transparency of glass.Mg0 is in glass
Crystallization tendency and crystallization rate can be reduced, increases high temperature viscosity of glass, improves the chemical stability and mechanical strength of glass.Al2O3
The crystallization tendency that glass can be reduced, improves chemical stability, thermal stability, mechanical strength, hardness, refractive index, mitigates glass pair
The corrosion of refractory material, and facilitate the milkiness of fluoride.
It is in order to ensure certain reducing atmosphere that the purpose of active carbon is added in the present embodiment.
Specific embodiment 4: present embodiment is unlike specific embodiment three: weighing 55.96 parts in step 1
Stannous oxide, 39.86 parts of phosphorus pentoxides, 1.58 parts of zinc oxide, 0.77 part of sodium oxide molybdena, 0.65 part of barium monoxide, 0.43 part of oxidation
Potassium, 0.32 part of silica, 0.21 part of indium oxide, 0.14 part of magnesia, 0.04 part of di-iron trioxide, 0.03 part of aluminium oxide,
0.01 part of strontium oxide strontia and 0.5~1 part of active carbon.Other are the same as the specific implementation mode 3.
Specific embodiment 5: a kind of application of low melting point glass powder of present embodiment is to use the low melting point glass powder
In high temp glass column, the stick to each other between aluminium alloy, high sial or aluminum matrix composite, the leak rate after adhesion are lower than respectively
10-8Pa·m3/s。
The glass powder is suitable for aluminium alloy, high sial and aluminum matrix composite, and the sintered rear surface glossiness of sample is good,
Faying face is good.Through helium mass spectrometer leak, air-tightness is best, is all satisfied service performance requirement, and leak rate is lower than 10-8Pa·m3/s。
Specific embodiment 6: a kind of application of low melting point glass powder of present embodiment is to use the low melting point glass powder
In the sealing-in of electronic vacuum component, the leak rate after sealing-in is lower than 10-8Pa·m3/s。
When the low melting point glass powder is used for the sealing-in of electronic vacuum component, the glass insulator of vacuum component is burnt
Sample is tied after helium mass spectrometer leak, air-tightness is all satisfied service performance requirement, and leak rate is lower than 10-8Pa·m3/s。
Specific embodiment 7: a kind of application of low melting point glass powder of present embodiment is to use the low melting point glass powder
In the hermetic seal of phased-array radar T/R module and the lead terminal of highly sophisticated device, the leak rate after sealing-in is lower than 10-8Pa·
m3/s。
Temperature shock simulation test is carried out to the glass sealing exemplar of high silica/aluminum-based body, actual conditions are as follows: low temperature -55
DEG C (cryogenic box): 250 DEG C of high temperature (is simulated, sample surface observed temperature is 250 DEG C) in thermal station, and high/low temperature conversion time is less than 5
Minute, 10 circulations are carried out altogether.After temperature examination, glass sealing exemplar carries out semitight leak detection, and leak rate is lower than 10-8Pa·m3/
S, air-tightness are qualified.
Specific embodiment 8: present embodiment using low melting point glass powder prepare compound glass column method be specifically by
It is carried out according to following steps:
One layer of low melting point glass powder is coated in the outer surface of glass insulation terminal, is subsequently placed in sintering furnace, by sintering furnace
Temperature in 40min from room temperature to 436 DEG C, temperature be 436 DEG C under conditions of heat preservation 30min after, cool to the furnace
300 DEG C of taking-ups, obtain compound glass column.
The preparation of present embodiment compound glass column, design and sintering process including mold.The design of mold includes examining
The precise positioning of dimensional contraction rate and center line after considering glass sintering.Sintering process includes heating rate, soaking time and burning
The technological parameters such as junction temperature.Mold aperture size needed for sintered combined glass column is generally bigger than high temp glass column radius size
0.3~0.4mm, such as the high temp glass column of Φ 1.9, hole milling size should be 2.5~Φ of Φ 2.7 or so, and left and right value is taken after hole milling
Test, the aperture size for finally taking effect best.Highly (or depth) direction, hole milling depth should be higher than the height of high temp glass column
About 0.05~0.1mm.The thermal expansion coefficient (CTE) of low melting point glass powder matches or close, compound glass with by seal, sealing materials
After column sintering, the low glassy layer that melts of high temp glass column surface sintering has fraction of contraction, generally in 0.06mm or so.
Specific embodiment 9: present embodiment is unlike specific embodiment eight: the low melting point glass powder
With a thickness of 0.3~0.4mm.Other are identical as specific embodiment eight.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one: a kind of preparation method of low melting point glass powder is specifically to follow the steps below:
One, 55.96 parts of stannous oxides, 39.86 parts of phosphorus pentoxides, 1.58 parts of zinc oxide, 0.77 are weighed in parts by weight
Part sodium oxide molybdena, 0.65 part of barium monoxide, 0.43 part of potassium oxide, 0.32 part of silica, 0.21 part of indium oxide, 0.14 part of magnesia,
0.04 part of di-iron trioxide, 0.03 part of aluminium oxide, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon；
Two, by the weighed 55.96 parts of stannous oxides of step 1,39.86 parts of phosphorus pentoxides, 1.58 parts of zinc oxide, 0.77
Part sodium oxide molybdena, 0.65 part of barium monoxide, 0.43 part of potassium oxide, 0.32 part of silica, 0.21 part of indium oxide, 0.14 part of magnesia,
Corundum crucible is put into after 0.04 part of di-iron trioxide, 0.03 part of aluminium oxide, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon mixing
In, be subsequently placed in 202-2 type thermostatic drying chamber, with the heating rate of 2 DEG C/min by the temperature of drying box from room temperature to
220 DEG C, and 1h is kept the temperature under conditions of temperature is 220 DEG C, obtain block mixture；
Three, block mixture is ground into powder, be then placed again into corundum crucible, being subsequently placed in temperature is 800 DEG C
In~850 DEG C of high temperature box type resistance furnace, with the heating rate of 5 DEG C/min by the temperature of high temperature box type resistance furnace from 800 DEG C~
850 DEG C are warming up to 1150 DEG C, and the glass of melting is cast in clean steel after heat preservation 2h under conditions of temperature is 1150 DEG C
On molding jig, cooled to room temperature makes annealing treatment the glass cooled down to be put into Muffle furnace, annealing temperature 320
DEG C, the glass after annealing is fitted into planetary ball mill by annealing time 1h, with the speed ball milling 1h of 500r/min, is obtained
Evengranular oxide powder, i.e., low melting point glass powder.
Not only chemical stability is good for low melting point glass powder manufactured in the present embodiment, and linear expansion coefficient is appropriate, leadless environment-friendly, and
And there is lower melt temperature, melt temperature is 490~550 DEG C, 20~300 DEG C of average linear coefficients of expansion 76 ± 3 ×
10-7/ DEG C, 380 ± 5 DEG C of transition temperature, 430 ± 5 DEG C of softening temperature.Glass powder of the present invention is suitable for high temp glass column and aluminium closes
Stick to each other between golden, high sial and aluminum matrix composite, the cold-resistant thermal shock of device after adhesion, matching is good, formula
In do not contain precious metal, cost of material is low, and operating procedure is simple, industrialized production easy to accomplish, and no poisonous and harmful element is right
Environment does not constitute pollution.Suitable for the sealing-in of electrovacuum component, especially suitable for phased-array radar T/R module and high-accuracy instrument
The hermetic seal of the lead terminal of device etc. provides guarantee for the large-scale production and popularization and application of T/R module.
Embodiment two: being specifically to follow the steps below using the method that low melting point glass powder prepares compound glass column
:
One layer of low melting point glass powder is coated in the outer surface of the glass insulation terminal having a size of Φ 2.4mm × 1.6mm, then
It is placed in sintering furnace, by the temperature of sintering furnace from room temperature to 436 DEG C in 40min, is protected under conditions of temperature is 436 DEG C
After warm 30min, 300 DEG C of taking-ups being cooled to the furnace, obtaining compound glass column, the size of the compound glass column is Φ 2.9mm.
By macroscopic view and microexamination, discovery combined column is coaxial, and surface gloss is good, and faying face is good.
Claims (9)
1. a kind of low melting point glass powder, it is characterised in that low melting point glass powder is by mass fraction by 30~80 parts of stannous oxides, 20
~60 parts of phosphorus pentoxides, 1~5 part of zinc oxide, 0.1~1 part of sodium oxide molybdena, 0.5~1 part of barium monoxide, 0.1~1 part of potassium oxide,
0.1~1 part of silica, 0.1~1 part of indium oxide, 0.1~1 part of magnesia, 0.04 part of di-iron trioxide, 0.03 part of aluminium oxide,
0.01 part of strontium oxide strontia and 0.5~1 part of active carbon are prepared；The melt temperature of the low melting point glass powder is 490 DEG C~550
DEG C, transition temperature is 375 DEG C~385 DEG C, and softening temperature is 425 DEG C~435 DEG C, and the low melting point glass powder is 20 in temperature
DEG C~300 DEG C under the conditions of average linear expansion coefficient be 73 × 10-7/ DEG C~79 × 10-7/℃。
2. a kind of low melting point glass powder according to claim 1, it is characterised in that low melting point glass powder by mass fraction by
55.96 parts of stannous oxides, 39.86 parts of phosphorus pentoxides, 1.58 parts of zinc oxide, 0.77 part of sodium oxide molybdena, 0.65 part of barium monoxide, 0.43
Part potassium oxide, 0.32 part of silica, 0.21 part of indium oxide, 0.14 part of magnesia, 0.04 part of di-iron trioxide, 0.03 part of oxidation
Aluminium, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon are prepared.
3. a kind of preparation method of low melting point glass powder as described in claim 1, it is characterised in that the system of low melting point glass powder
Preparation Method is specifically to follow the steps below:
One, 30~80 parts of stannous oxides, 20~60 parts of phosphorus pentoxides, 1~5 part of zinc oxide, 0.1~1 are weighed by mass fraction
Part sodium oxide molybdena, 0.5~1 part of barium monoxide, 0.1~1 part of potassium oxide, 0.1~1 part of silica, 0.1~1 part of indium oxide, 0.1~1
Part magnesia, 0.04 part of di-iron trioxide, 0.03 part of aluminium oxide, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon；
Two, by weighed 30~80 parts of stannous oxides of step 1,20~60 parts of phosphorus pentoxides, 1~5 part of zinc oxide, 0.1~1
Part sodium oxide molybdena, 0.5~1 part of barium monoxide, 0.1~1 part of potassium oxide, 0.1~1 part of silica, 0.1~1 part of indium oxide, 0.1~1
It is put into after part magnesia, 0.04 part of di-iron trioxide, 0.03 part of aluminium oxide, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon mixing
It in corundum crucible, is subsequently placed in 202-2 type thermostatic drying chamber, with the heating rate of 2 DEG C/min by the temperature of drying box from room
Temperature is warming up to 220 DEG C, and keeps the temperature 1h under conditions of temperature is 220 DEG C, obtains block mixture；
Three, block mixture is ground into powder, be then placed again into corundum crucible, being subsequently placed in temperature is 800 DEG C~850
DEG C high temperature box type resistance furnace in, with the heating rate of 5 DEG C/min by the temperature of high temperature box type resistance furnace from 800 DEG C~850 DEG C
1150 DEG C are warming up to, and the glass of melting is cast in clean steel die after heat preservation 2h under conditions of temperature is 1150 DEG C
On tool, cooled to room temperature makes annealing treatment the glass cooled down to be put into Muffle furnace, and annealing temperature is 320 DEG C, moves back
The fiery time is 1h, and the glass after annealing is fitted into planetary ball mill, with the speed ball milling 1h of 500r/min, it is equal to obtain particle
Even oxide powder, i.e., low melting point glass powder.
4. a kind of preparation method of low melting point glass powder according to claim 3, it is characterised in that weighed in step 1
55.96 parts of stannous oxides, 39.86 parts of phosphorus pentoxides, 1.58 parts of zinc oxide, 0.77 part of sodium oxide molybdena, 0.65 part of barium monoxide, 0.43
Part potassium oxide, 0.32 part of silica, 0.21 part of indium oxide, 0.14 part of magnesia, 0.04 part of di-iron trioxide, 0.03 part of oxidation
Aluminium, 0.01 part of strontium oxide strontia and 0.5~1 part of active carbon.
5. a kind of application of low melting point glass powder as described in claim 1, it is characterised in that be by the low melting point glass powder
For high temp glass column, the stick to each other between aluminium alloy, high sial or aluminum matrix composite, the leak rate after adhesion are low respectively
In 10-8Pa·m3/s。
6. a kind of application of low melting point glass powder as described in claim 1, it is characterised in that be by the low melting point glass powder
For the sealing-in of electronic vacuum component, the leak rate after sealing-in is lower than 10-8Pa·m3/s。
7. a kind of application of low melting point glass powder as described in claim 1, it is characterised in that be by the low melting point glass powder
For the hermetic seal of phased-array radar T/R module and the lead terminal of highly sophisticated device, the leak rate after sealing-in is lower than 10-8Pa·
m3/s。
8. the method for preparing compound glass column using low melting point glass powder described in claim 1, it is characterised in that prepare compound
The method of glass column is specifically to follow the steps below:
One layer of low melting point glass powder is coated in the outer surface of glass insulation terminal, is subsequently placed in sintering furnace, by the temperature of sintering furnace
Degree, from room temperature to 436 DEG C, under conditions of temperature is 436 DEG C after heat preservation 30min, cools to 300 DEG C with the furnace in 40min
It takes out, obtains compound glass column.
9. the method according to claim 8 for preparing compound glass column using low melting point glass powder, it is characterised in that described
Low melting point glass powder with a thickness of 0.3mm~0.4mm.
Priority Applications (1)
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| CN108640519B (en) * | 2018-05-31 | 2022-01-11 | 北京天力创玻璃科技开发有限公司 | Lead-free sealing glass and preparation method thereof |
| CN109052965B (en) * | 2018-09-07 | 2021-12-24 | 苏州融睿电子科技有限公司 | Combination, mixture, sealing glass and manufacturing method thereof |
| CN111039547B (en) * | 2019-12-31 | 2022-05-24 | 河南理工大学 | Preparation and use method of low-temperature glass ring for sealing aluminum-based composite material and glass insulation terminal |
| CN112876073A (en) * | 2021-01-29 | 2021-06-01 | 中国科学院上海光学精密机械研究所 | Luminescent glass and preparation method thereof |
| CN113003940A (en) * | 2021-04-23 | 2021-06-22 | 贵州国锐鑫节能科技有限公司 | Low-melting-point low-expansion-coefficient glass powder and preparation method thereof |
| CN115925439B (en) * | 2022-12-06 | 2024-01-23 | 凯龙蓝烽新材料科技有限公司 | Silicon carbide particle catcher and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003146691A (en) * | 2001-11-15 | 2003-05-21 | Asahi Techno Glass Corp | Low melting point glass, and production method therefor |
| CN102471137A (en) * | 2009-07-31 | 2012-05-23 | 旭硝子株式会社 | Sealing glass, sealing material and sealing material paste for semiconductor devices, and semiconductor device and process for production thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003146691A (en) * | 2001-11-15 | 2003-05-21 | Asahi Techno Glass Corp | Low melting point glass, and production method therefor |
| CN102471137A (en) * | 2009-07-31 | 2012-05-23 | 旭硝子株式会社 | Sealing glass, sealing material and sealing material paste for semiconductor devices, and semiconductor device and process for production thereof |
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| CN106430989A (en) | 2017-02-22 |
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