CN104961357B - A kind of K9 glass and titanium law temperature joining method - Google Patents
A kind of K9 glass and titanium law temperature joining method Download PDFInfo
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- CN104961357B CN104961357B CN201510392749.XA CN201510392749A CN104961357B CN 104961357 B CN104961357 B CN 104961357B CN 201510392749 A CN201510392749 A CN 201510392749A CN 104961357 B CN104961357 B CN 104961357B
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- 239000010936 titanium Substances 0.000 title claims abstract description 106
- 239000011521 glass Substances 0.000 title claims abstract description 79
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 71
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000005304 joining Methods 0.000 title claims abstract description 23
- 229910000679 solder Inorganic materials 0.000 claims abstract description 47
- 239000002131 composite material Substances 0.000 claims abstract description 40
- 238000002791 soaking Methods 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 230000005684 electric field Effects 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims description 97
- 238000000498 ball milling Methods 0.000 claims description 36
- 230000003647 oxidation Effects 0.000 claims description 25
- 238000007254 oxidation reaction Methods 0.000 claims description 25
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 23
- 229910052797 bismuth Inorganic materials 0.000 claims description 23
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 23
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 23
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 23
- 239000000292 calcium oxide Substances 0.000 claims description 23
- 235000012054 meals Nutrition 0.000 claims description 23
- 239000011701 zinc Substances 0.000 claims description 23
- 229910052725 zinc Inorganic materials 0.000 claims description 23
- 229910052810 boron oxide Inorganic materials 0.000 claims description 21
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 239000000945 filler Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000000087 stabilizing effect Effects 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 description 15
- 238000010304 firing Methods 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 230000035882 stress Effects 0.000 description 5
- 230000008646 thermal stress Effects 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910020658 PbSn Inorganic materials 0.000 description 1
- 101150071746 Pbsn gene Proteins 0.000 description 1
- -1 baroque compound Chemical group 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006023 eutectic alloy Substances 0.000 description 1
- 230000004313 glare Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
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- Joining Of Glass To Other Materials (AREA)
- Glass Compositions (AREA)
Abstract
The present invention relates to the connection of glass and metal, specifically a kind of K9 glass and titanium law temperature joining method, it is characterised in that step is as follows：（One）, prepare the powdered composite solder of bismuthates containing active element Ti,（Two）And then composite solder is placed between titanium and K9 glass,（Three）, sample is taken out after be placed in bonding in vacuum stove, bonding in vacuum stove be provided with voltage be 100 ~ 700V DC electric field, temperature be 300 ~ 600 °C, while apply perpendicular to sample plane pressure be 5 ~ 40Pa, vacuum 10‑3~10‑2Pa；Soaking time is no more than 120min, realizes that K9 glass is effectively connected with titanium, cools to room temperature taking-up with the furnace, completes K9 glass and titanium law temperature joining, has the advantages that simple to operate, environmental protection, high working efficiency, process stabilizing.
Description
Technical field
The present invention relates to the connection of glass and metal, specifically one kind is particularly well-suited to optical window, observation window etc.
K9 glass and titanium law temperature joining method.
Background technology
During the assembling and use of optical window, window is needed in its end and glass stitching portion and metallic matrix reality
Now it is reliably connected, and suppresses to connect the veiling glare of window interior and eliminate flat board junction high-speed flight to be produced with air friction
Thermal gradient the problems such as.At present frequently with metallic matrix be titanium, it has high specific strength, specific stiffness, good antioxygen
The advantages of property changed and excellent high temperature and cryogenic mechanics performance, there is wide application in Aeronautics and Astronautics, military and civilian field
Prospect.
K9 glass exists greatly with titanium in terms of chemical-bond type, microstructure, physical property and mechanical property
Difference, is that high-quality connection therebetween proposes huge challenge.Compared with titanium, the strain point of glass material and softening
Point is relatively low, therefore realizes effective connection of K9 glass and titanium, there is following difficult point：（1）Aerial optical window high is oral
In low temperature environment, mechanical property will at low temperature for conventional soft solder Pb bases, Sn bases solder and PbSn eutectic alloys solder for labour
Produce mutation, therefore may not apply to low temperature environment；（2）Solder is difficult to soak in glass surface, sprawls；（3）To mechanical property
There can be the solders such as requirement very high, Ge bases, Al bases, Cu bases and Ag bases to occur in heating and cooling procedure with thermal coefficient of expansion
Larger stress gradient, so as to produce residual stress, especially for size is larger or the baroque compound structure of glass/metal
The soldering of part, this problem seems especially prominent, and the method frequently with addition stress-buffer layer or intermediate layer connects to alleviate at present
The residual stress of head, but increasing for cushion makes welding process complicated, and brazed seam broadens, and engineer applied adaptability is limited significantly.Cause
How this, solve the study hotspot of the difficult point always Welder author of above-mentioned glass/metal dissimilar material joining.
How to realize that K9 glass is reliably connected with titanium foreign material and prepare shaping as optical window composite construction
Key technology.Current optical window composite construction prepares shaping and mainly uses following two typical process.
（One）One kind heat-sealing pressure technology（Such as Chinese invention patent 93101627.4）, using the technology, can be relatively low
At a temperature of, to carrying out solid-state sealing-in by a kind of Pb bases solder between the glass flange end face and metal end of thermal-collecting tube, i.e., in weldering
Connect material keep solid-state in the state of by appropriate pressurization, seal it.So, not only greatly simplify technique,
The coefficient of expansion between glass tube and the therewith metal material of sealing-in is also solved simultaneously mismatches caused difficulty.But
This technique productions equipment is complicated, glass structure is limited etc., influences quality of connection.
（Two）In order to improve bonding strength, another method is gradually applied, by compound glass and metal using altogether
Anodic field causes the method that diffusion is quickly connected.
First glass and metal are placed in the bonding in vacuum stove of DC electric field to poststack, and are heated to uniform temperature and are protected
After holding a period of time；There is bonding reaction and form bonding in glass, bonding is completed, and connector is cooled down with connection stove,（Such as Chinese patent
Grant number is the open source literature of 1974462B）, combined with ionic bond between such glass and metal, improve bonding strength.However,
If the thermal expansion coefficient difference of glass and metal is big, because glass is high with intermetallic articulamentum residual stress, cause
The phenomenon that glass comes off with metal, influences product quality.
The content of the invention
The present invention in order to after solving existing K9 glass and titanium law temperature joining bond strength it is low, easily come off and use
The problems such as short life, there is provided so that bond strength after a kind of connection is high, new K9 glass difficult for drop-off and titanium law temperature joining
Method.
The present invention can be reached by following measure：
A kind of K9 glass and titanium law temperature joining method, it is characterised in that step is as follows：
（One）, prepare the powdered composite solder of bismuthates containing active element Ti, composite solder is by oxidation bismuth meal, oxidation
Boron powder, oxide powder and zinc, calcium oxide powder and Ti powder are mixed, the percentage by weight of each composition for oxidation bismuth meal 20 ~
98.5%th, boron oxide powder 0.5 ~ 30%, oxide powder and zinc 0.5 ~ 30%, calcium oxide powder 0.5 ~ 30%, Ti powder 0.5 ~ 10%, each composition
Percentage by weight sum be equal to 100%, its granularity be 300-600 μm；
（Two）And then composite solder is placed between titanium and K9 glass, the thickness of composite solder for 0.005 ~
0.50mm, forms sandwich assembling between titanium, composite solder and K9 glass, the sample that will be assembled is placed in resistance furnace and adds
To 200 ~ 600 °C, soaking time is no more than 30min to heat, cools to room temperature with the furnace；
（Three）, sample is taken out after be placed in bonding in vacuum stove, bonding in vacuum stove be provided with voltage be 100 ~ 700V direct current
Electric field, temperature is 300 ~ 600 °C, while it is 5 ~ 40Pa, vacuum 10 to apply perpendicular to the pressure of sample plane-3~10-2Pa；Protect
The warm time be no more than 120min, realize that K9 glass is effectively connected with titanium, cool to the furnace room temperature taking-up, complete K9 glass and
Titanium law temperature joining.
Composite solder of the present invention is prepared by following steps：
（One）Get the raw materials ready：Oxidation bismuth meal, boron oxide powder, oxide powder and zinc, calcium oxide powder and Ti powder are weighed by weight percentage；
（Two）Ball milling：Oxidation bismuth meal, boron oxide powder, oxide powder and zinc, calcium oxide powder and the Ti powder that will be weighed up together load
In ball grinder, ratio of grinding media to material is that 10 ~ 25 ︰ 1, filler ratios are 30% ~ 55%；It is filled with ball milling after argon gas after vacuumizing, Ball-milling Time is 1 ~
8h, rotating ratio are 100 ~ 250r/min；Ball milling ball is taken out and obtains composite solder by ball milling after terminating.
Composite solder between titanium of the present invention and K9 glass puts thickness for 0.05 ~ 0.50mm, titanium, multiple
Close and formed between solder and K9 glass sandwich assembling, the sample that will be assembled is placed in resistance furnace and is heated to 380 ~ 420 °C, protects
Temperature is no more than 18min, cools to room temperature with the furnace.
Bonding in vacuum stove of the present invention is provided with the DC electric field that voltage is 350V, and temperature is 500 °C, while applying to hang down
The straight pressure in sample plane is 35Pa, vacuum 10-3~10-2Pa；Soaking time is 60-80min, realizes K9 glass and titanium
Category effectively connection, cools to room temperature taking-up with the furnace, completes K9 glass and titanium law temperature joining.
The problems such as present invention not only solves K9 glass and titanium jointing low intensity, easily comes off, and utilize
React the TiO of generationxThe characteristics of phase high-modulus, low-thermal-expansion and reduce joint thermal coefficient of expansion, effectively alleviate joint with
Thermal stress between base material metal, can also realize joint in thermal physical characteristic by the content and distribution of effective control joint product
Gradient transition in terms of energy, further relief of thermal stress, so that the fundamentally quality of connection of control glass and metal, the present invention
There is simple to operate, environmental protection, high working efficiency, process stabilizing.
Specific embodiment
The invention will be further described below：
A kind of K9 glass and titanium law temperature joining method, it is characterised in that step is as follows：
（One）, prepare the powdered composite solder of bismuthates containing active element Ti, composite solder is by oxidation bismuth meal, oxidation
Boron powder, oxide powder and zinc, calcium oxide powder and Ti powder are mixed, the percentage by weight of each composition for oxidation bismuth meal 20 ~
98.5%th, boron oxide powder 0.5 ~ 30%, oxide powder and zinc 0.5 ~ 30%, calcium oxide powder 0.5 ~ 30%, Ti powder 0.5 ~ 10%, each composition
Percentage by weight sum be equal to 100%, its granularity be 300-600 μm；(two）And then composite solder is placed in titanium and K9
Between glass, the thickness of composite solder is 0.005 ~ 0.5mm, Sanming City is formed between titanium, composite solder and K9 glass and is purchased things necessary for a long journey
Match somebody with somebody, the sample that will be assembled is placed in resistance furnace and is heated to 200 ~ 600 °C, and soaking time is no more than 30min, cools to room with the furnace
Temperature；（Three）, sample is taken out after be placed in bonding in vacuum stove, bonding in vacuum stove be provided with voltage be 100 ~ 700V DC electric field,
Temperature is 300 ~ 600 °C, while it is 5 ~ 40Pa, vacuum 10 to apply perpendicular to the pressure of sample plane-3~10-2Pa；During insulation
Between be no more than 120min, realize that K9 glass is effectively connected with titanium, cool to the furnace room temperature taking-up, completion K9 glass and titanium
Category law temperature joining.
Described composite solder is prepared by following steps：
（One）Get the raw materials ready：Oxidation bismuth meal, boron oxide powder, oxide powder and zinc, calcium oxide powder and Ti powder are weighed by weight percentage；
（Two）Ball milling：Oxidation bismuth meal, boron oxide powder, oxide powder and zinc, calcium oxide powder and the Ti powder that will be weighed up together are fitted into ball grinder,
Ratio of grinding media to material is that 10 ~ 25 ︰ 1, filler ratios are 30% ~ 55%；Ball milling after argon gas is filled with after vacuumizing, Ball-milling Time is 1 ~ 8h, rotating ratio
It is 100 ~ 250r/min；Ball milling ball is taken out and obtains composite solder by ball milling after terminating；Between described titanium and K9 glass
Composite solder put thickness for 0.05 ~ 0.50mm, sandwich assembling is formed between titanium, composite solder and K9 glass, will fill
The sample for preparing is placed in resistance furnace and is heated to 380 ~ 420 °C, and insulation is no more than 18min, cools to room temperature with the furnace, and described is true
Sky connection stove is provided with the DC electric field that voltage is 350V, and temperature is 500 °C, while applying is perpendicular to the pressure of sample plane
35Pa, vacuum 10-3~10-2Pa；Soaking time is 60-80min, realizes that K9 glass is effectively connected with titanium, furnace cooling
Taken out to room temperature, complete K9 glass and titanium law temperature joining, the present invention not only solves K9 glass and titanium jointing
Low intensity, the problems such as easily come off, and using the TiO of reaction generationxThe characteristics of phase high-modulus, low-thermal-expansion and reduction connect
The thermal coefficient of expansion of head, effectively alleviates the thermal stress between joint and base material metal, by containing for effective control joint product
Amount and distribution can also realize gradient transition of the joint in terms of thermophysical property, further relief of thermal stress, so that fundamentally
The quality of connection of control glass and metal, the present invention has simple to operate, environmental protection, high working efficiency, process stabilizing etc. excellent
Point.
Embodiment 1：The step of present embodiment, is as follows：（One）Get the raw materials ready：Weigh by weight percentage 50% oxidation bismuth meal,
15% boron oxide powder, 15% oxide powder and zinc, 15% calcium oxide powder and 5% Ti powder, wherein Ti powder quality purity is
99.90%, granular size is 400 μm；(two）Ball milling：The oxidation bismuth meal that to weigh up, boron oxide powder, oxide powder and zinc, calcium oxide powder with
And Ti powder is together fitted into ball grinder, ratio of grinding media to material is that 18 ︰ 1, filler ratios are 42%；Argon gas is filled with after vacuumizing, then ball milling is 4
Hour, rotating ratio are 200r/min；Ball milling ball is taken out and has obtained being applied to K9 glass and titanium low temperature by ball milling after terminating
Connection.（Three）Bismuthates composite solder containing Ti is placed between K9 glass and titanium, the bismuthates composite solder containing Ti is thick
It is 0.08mm to spend, and 450 °C are heated under air conditionses, and soaking time is 90min, is taken out after cooling to room temperature with the furnace.（Four）
Sample after taking-up is positioned in the bonding in vacuum stove of the DC electric field that voltage is 500V, connection temperature is 450 °C, connection pressure
Power is 25Pa, vacuum 10-2Pa；Soaking time 90min, realizes that K9 glass is effectively connected with titanium, cools to room temperature with the furnace
Take out；Firing rate：50 °C/min, cooling velocity：20°C/min.
Embodiment 2：The step of present embodiment, is as follows：（One）Get the raw materials ready：Weigh by weight percentage 20% oxidation bismuth meal,
30% boron oxide powder, 30% oxide powder and zinc, 10% calcium oxide powder and 10% Ti powder, wherein Ti powder quality purity is
99.95%, granular size is 100 μm；（Two）Ball milling：The oxidation bismuth meal that to weigh up, boron oxide powder, oxide powder and zinc, calcium oxide powder with
And Ti powder is together fitted into ball grinder, ratio of grinding media to material is that 25 ︰ 1, filler ratios are 55%；Argon gas is filled with after vacuumizing, then ball milling is 8
Hour, rotating ratio are 250r/min；Ball milling ball is taken out and has obtained being applied to K9 glass and titanium low temperature by ball milling after terminating
Connection.（Three）Bismuthates composite solder containing Ti is placed between K9 glass and titanium, the bismuthates composite solder containing Ti is thick
It is 0.005 ~ 0.5mm to spend, and 600 °C are heated under air conditionses, and soaking time is 120min, is taken after cooling to room temperature with the furnace
Go out.（Four）Sample after taking-up is positioned in the bonding in vacuum stove of the DC electric field that voltage is 700V, connection temperature is 600 °
C, connection pressure is 40Pa, vacuum 10-2Pa；Soaking time 120min, realizes that K9 glass is effectively connected with titanium, cold with stove
But taken out to room temperature；Firing rate：50 °C/min, cooling velocity：20°C/min.
Embodiment 3：The step of present embodiment, is as follows：（One）Get the raw materials ready：Weigh by weight percentage 98% oxidation bismuth meal,
0.5% boron oxide powder, 0.5% oxide powder and zinc, 0.5% calcium oxide powder and 0.5% Ti powder, wherein Ti powder quality purity is
90%, granular size is 100 μm；（Two）Ball milling：The oxidation bismuth meal that to weigh up, boron oxide powder, oxide powder and zinc, calcium oxide powder and
Ti powder is together fitted into ball grinder, and ratio of grinding media to material is that 10 ︰ 1, filler ratios are 30%；Argon gas is filled with after vacuumizing, then ball milling is 1.1
Hour, rotating ratio are 250r/min；Ball milling ball is taken out and has obtained being applied to K9 glass and titanium low temperature by ball milling after terminating
Connection.（Three）Bismuthates composite solder containing Ti is placed between K9 glass and titanium, the bismuthates composite solder containing Ti is thick
It is 0.005 ~ 0.5mm to spend, and 500 °C are heated under air conditionses, and soaking time is 120min, is taken after cooling to room temperature with the furnace
Go out.（Four）Sample after taking-up is positioned in the bonding in vacuum stove of the DC electric field that voltage is 600V, connection temperature is 600 °
C, connection pressure is 40Pa, vacuum 10-2Pa；Soaking time 120min, realizes that K9 glass is effectively connected with titanium, cold with stove
But taken out to room temperature；Firing rate：50 °C/min, cooling velocity：20°C/min.
Embodiment 4：The step of present embodiment, is as follows：
（One）Get the raw materials ready：20 ~ 98.5% oxidation bismuth meal, 0.5 ~ 30% boron oxide powder, 0.5 ~ 30% is weighed by weight percentage
Oxide powder and zinc, 0.5 ~ 30% calcium oxide powder and 0.5 ~ 10% Ti powder, wherein Ti powder quality purity is 99 ~ 99.95%,
Grain size is 10 ~ 100 μm；（Two）Ball milling：Oxidation bismuth meal, boron oxide powder, oxide powder and zinc, calcium oxide powder and the Ti powder that will be weighed up
Together it is fitted into ball grinder, ratio of grinding media to material is that 10 ~ 25 ︰ 1, filler ratios are 30% ~ 55%；Argon gas is filled with after vacuumizing, then ball milling is 1
~ 8 hours, rotating ratio be 100 ~ 250r/min；Ball milling ball is taken out and has obtained being applied to K9 glass and titanium by ball milling after terminating
Category law temperature joining.（Three）Bismuthates composite solder containing Ti is placed between K9 glass and titanium, the bismuthates containing Ti is combined
Solder thickness is 0.005 ~ 0.5mm, and 200 ~ 600 °C are heated under air conditionses, and soaking time is 0 ~ 120min, furnace cooling
Taken out after to room temperature.（Four）Sample after taking-up is positioned in the bonding in vacuum stove of the DC electric field that voltage is 100 ~ 700V,
Connection temperature is 300 ~ 600 °C, and connection pressure is 5 ~ 40Pa, vacuum 10-3~10-2Pa；0 ~ 120min of soaking time, realizes K9
Glass is effectively connected with titanium, cools to room temperature taking-up with the furnace；Firing rate：2 °C/min ~ 50 °C/min, cooling velocity：1°
C/min~20°C/min。
Embodiment 4：The step of present embodiment, is as follows：（One）Get the raw materials ready：Weigh by weight percentage 40% oxidation bismuth meal,
15% boron oxide powder, 15% oxide powder and zinc, 15% calcium oxide powder and 15% Ti powder, wherein Ti powder quality purity is
99.85%, granular size is 10 ~ 100 μm；（Two）Ball milling：Oxidation bismuth meal, boron oxide powder, oxide powder and zinc, the calcium oxide that will be weighed up
Powder and Ti powder are together fitted into ball grinder, and ratio of grinding media to material is that 10 ~ 25 ︰ 1, filler ratios are 30% ~ 55%；Argon gas is filled with after vacuumizing,
Then ball milling be 1 ~ 8 hour, rotating ratio be 100 ~ 250r/min；Ball milling ball is taken out and has obtained being applied to K9 by ball milling after terminating
Glass and titanium law temperature joining.（Three）Bismuthates composite solder containing Ti is placed between K9 glass and titanium, containing Ti's
Bismuthates composite solder thickness is 0.005 ~ 0.5mm, is heated to 200 ~ 600 °C under air conditionses, soaking time is 0 ~
120min, takes out after cooling to room temperature with the furnace.（Four）Sample after taking-up is positioned over the DC electric field that voltage is 100 ~ 700V
Bonding in vacuum stove in, connection temperature be 300 ~ 600 °C, connection pressure be 5 ~ 40Pa, vacuum 10-3~10-2Pa；Soaking time
0 ~ 120min, realizes that K9 glass is effectively connected with titanium, cools to room temperature taking-up with the furnace；Firing rate：2°C/min~50°C/
Min, cooling velocity：1°C/min~20°C/min.
Embodiment 5：The present embodiment is with the difference of embodiment 1：Step（One）In containing Ti powder bismuthates Combined Welding
Material by weight percentage by 60% oxidation bismuth meal, 25% boron oxide powder, 5% oxide powder and zinc, 5% calcium oxide powder and 5%
Ti powder is constituted.
Embodiment 6：The present embodiment is with the difference of embodiment 1：Difference be step（Three）In be coated on K9
The composite solder of bismuthates containing Ti powder thickness between glass and titanium is 0.05mm.Embodiment 7：The present embodiment and embodiment
1 difference is：Step（Three）It is middle obtain composite solder intermediate layer process conditions be：Heating-up temperature：450 °C, during insulation
Between：30min, firing rate：5 °C/min ~ 15 °C/min, cooling velocity：5°C/min~18°C/min.
Embodiment 8：The present embodiment is with the difference of embodiment 1：Step（Three）Anodic bonding technology condition is：It is lazy
Property protective gas purity：99 ~ 99.95%, DC voltage be 100 ~ 700V, connection temperature be 300 ~ 600 °C, connection pressure be 5 ~
40Pa, vacuum 10-3~10-2Pa；0 ~ 120min of soaking time.Firing rate：5 °C/min ~ 30 °C/min, cooling velocity：1°
C/min~15°C/min.Other steps are identical with specific embodiment one.
Embodiment 9：The present embodiment is with the difference of embodiment 1：Step（Two）Middle ratio of grinding media to material is for 15 ︰ 1, filler ratios
40%；It is 200r/min to be filled with after argon gas intermittent ball milling 4h, rotating speed.
Embodiment 10：The present embodiment is with the difference of embodiment 1：Step（Four）Middle acquisition solder intermediate layer condition
For：Heating-up temperature：450 °C, soaking time：15min, firing rate：10 °C/min, cooling velocity：8°C/min.
Claims (5)
1. a kind of K9 glass and titanium law temperature joining method, it is characterised in that step is as follows：
（One）, prepare the powdered composite solder of bismuthates containing active element Ti, composite solder is by oxidation bismuth meal, boron oxide
Powder, oxide powder and zinc, calcium oxide powder and Ti powder are mixed, the percentage by weight of each composition is oxidation bismuth meal 20 ~ 98.5%,
Boron oxide powder 0.5 ~ 30%, oxide powder and zinc 0.5 ~ 30%, calcium oxide powder 0.5 ~ 30%, Ti powder 0.5 ~ 10%, the weight of each composition
Percentage sum is equal to 100%, and its granularity is 300-600 μm；
（Two）And then composite solder is placed between titanium and K9 glass, the thickness of composite solder is 0.005 ~ 0.50mm, titanium
Forming sandwich assembling between metal, composite solder and K9 glass, the sample that will be assembled is placed in resistance furnace and is heated to 200 ~
600 °C, soaking time is no more than 30min, cools to room temperature with the furnace；
（Three）, sample is taken out after be placed in bonding in vacuum stove, bonding in vacuum stove be provided with voltage be 100 ~ 700V DC electric field,
Temperature is 300 ~ 600 °C, while it is 5 ~ 40Pa, vacuum 10 to apply perpendicular to the pressure of sample plane-3~10-2Pa；During insulation
Between be no more than 120min, realize that K9 glass is effectively connected with titanium, cool to the furnace room temperature taking-up, completion K9 glass and titanium
Category law temperature joining.
2. a kind of K9 glass according to claim 1 and titanium law temperature joining method, it is characterised in that composite solder leads to
Cross following steps preparation：
（One）Get the raw materials ready：Oxidation bismuth meal, boron oxide powder, oxide powder and zinc, calcium oxide powder and Ti powder are weighed by weight percentage；（Two）
Ball milling：Oxidation bismuth meal, boron oxide powder, oxide powder and zinc, calcium oxide powder and the Ti powder that will be weighed up together are fitted into ball grinder, ball material
Than being 30% ~ 55% for 10 ~ 25 ︰ 1, filler ratios；Ball milling after argon gas is filled with after vacuumizing, Ball-milling Time is 1 ~ 8h, rotating ratio is 100
~250r/min；Ball milling ball is taken out and obtains composite solder by ball milling after terminating.
3. a kind of K9 glass according to claim 1 and titanium law temperature joining method, it is characterised in that titanium and K9
Composite solder between glass puts thickness for 0.05 ~ 0.50mm.
4. a kind of K9 glass according to claim 1 and titanium law temperature joining method, it is characterised in that by what is assembled
Sample is placed in resistance furnace and is heated to 380 ~ 420 °C, and insulation is no more than 18min, cools to room temperature with the furnace.
5. a kind of K9 glass according to claim 1 and titanium law temperature joining method, it is characterised in that bonding in vacuum stove
The DC electric field that voltage is 350V is provided with, temperature is 500 °C, while it is 35Pa, vacuum to apply perpendicular to the pressure of sample plane
Degree 10-3~10-2Pa；Soaking time is 60-80min, realizes that K9 glass is effectively connected with titanium, cools to room temperature with the furnace and takes
Go out, complete K9 glass and titanium law temperature joining.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510392749.XA CN104961357B (en) | 2015-07-07 | 2015-07-07 | A kind of K9 glass and titanium law temperature joining method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510392749.XA CN104961357B (en) | 2015-07-07 | 2015-07-07 | A kind of K9 glass and titanium law temperature joining method |
Publications (2)
| Publication Number | Publication Date |
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| CN104961357A CN104961357A (en) | 2015-10-07 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20200040582A (en) * | 2018-10-10 | 2020-04-20 | 현대자동차주식회사 | Flux composition for brazing aluminium and brazing method of aluminium using the same |
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| CN106007409B (en) * | 2016-07-12 | 2019-01-11 | 牛济泰 | A kind of device to be packaged melts the method and its application of envelope with glass insulation terminal low temperature |
| CN108623192B (en) * | 2017-03-23 | 2021-04-16 | 南京理工大学 | Titanium alloy-K9 glass composite connection equipment and method based on intermediate layer gradient |
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| CN101157519A (en) * | 2007-09-17 | 2008-04-09 | 东华大学 | Barium crown glass powder for electrode superposition and preparation method thereof |
| CN101376561A (en) * | 2008-09-28 | 2009-03-04 | 陈培 | Low-melting point lead-less glasses powder for frit slurry, and preparation and use thereof |
| CN101746964A (en) * | 2008-12-19 | 2010-06-23 | 沈阳兴华航空电器有限责任公司 | Titanium alloy and glass sealing process method |
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| KR102610732B1 (en) * | 2018-10-10 | 2023-12-07 | 현대자동차주식회사 | Flux composition for brazing aluminium and brazing method of aluminium using the same |
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