CN103056553B - A kind of solder and preparation method thereof and the method utilizing solder to be connected sapphire and niobium or niobium alloy - Google Patents
A kind of solder and preparation method thereof and the method utilizing solder to be connected sapphire and niobium or niobium alloy Download PDFInfo
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Abstract
Solder and preparation method thereof and the method utilizing solder to be connected sapphire and niobium or niobium alloy, relate to the field of solder and preparation and method of attachment.The present invention will solve existing method for brazing to connect sapphire and metal and there is joint and have larger residual stress and non-refractory, technique comparatively complexity and the not high problem of strength of joint.A kind of solder: be by Ag powder, CuO powder, TiH
2powder, Si
3n
4nano-ceramic particle and binding agent are prepared from.Preparation method: one, Ag-CuO-TiH
2the preparation of powder; Two, the preparation of solder mixed-powder; Three, solder mixed-powder and binding agent Homogeneous phase mixing.Solder is utilized to connect the method for sapphire and niobium or niobium alloy: one, to prepare sapphire sample to be welded and niobium to be welded or niobium alloy sample; Two, solder is coated in welding surface; Three, by Segmented heating form, connection is completed.The present invention is applicable to welding field.
Description
Technical field
The present invention relates to the field of solder and preparation and method of attachment.
Background technology
Sapphire is α-Al
2o
3monocrystalline, is a kind ofly have the combined excellent crystalline material of excellent physical characteristic, mechanical property and the chemical characteristics such as high strength, high thermal shock drag, high-corrosion resistance and high wave transmission rate, is considered to the ideal material of satellite optical window.But because it is the monocrystal material of aluminium oxide, price is more expensive, its application needs inevitably to be connected with metal, as niobium, kovar alloy and carbon steel etc.At present, the method for attachment of sapphire and metal mainly contains: soldering, diffusion welding (DW), glass solder method, splicing and mechanical connection.Diffusion Welding strength of joint is higher, but the connect hours is long, and cost is high, and gas pore in weld metal can have a strong impact on the air-tightness of seal.Larger residual stress can be produced in glass welding method weld seam, and easily form the defects such as crackle, pore, cavity, glassy layer also corrosion-vulnerable itself, the poor high temperature stability of joint.Gluded joint intensity is low, can not bear high temperature, easily aging, has had a strong impact on service life and the reliability of connector.The air-tightness of mechanical connecting element is not enough, sapphire screw processing difficulties, and easily generation stress is concentrated and ftractures.Method for brazing connects sapphire and metal is mainly active soldering and indirect soldering.Active soldering method joint has larger residual stress and non-refractory, and indirect method for brazing technique is comparatively complicated and strength of joint is not high.
CN102699572A discloses a kind of solder by Ag powder, Cu powder, Ti powder and Si
3n
4nano-ceramic particle is prepared from.
Summary of the invention
The present invention will solve existing method for brazing to connect sapphire and metal and there is joint and have larger residual stress and non-refractory, technique comparatively complexity and the not high problem of strength of joint, and provides a kind of solder and preparation method thereof and the method utilizing solder to be connected sapphire and niobium or niobium alloy.
A kind of solder is by Ag powder, CuO powder, TiH
2powder, Si
3n
4nano-ceramic particle and binding agent are prepared from; Wherein, described Ag powder and the mass ratio of CuO powder are 1:(0.06 ~ 0.17), described Ag powder and TiH
2the mass ratio of powder is 1:(0.01 ~ 0.11), described Ag powder and Si
3n
4the mass ratio of nano-ceramic particle is 1:(0.012 ~ 0.12), described Ag powder and the mass ratio of binding agent are 1:(0.05 ~ 0.07).
Described binding agent is mixed by glycerine, hydroxyethylcellulose and water; Wherein, described glycerine and the mass ratio of hydroxyethylcellulose are 1:(3 ~ 7), described glycerine and the mass ratio of water are 1:(90 ~ 92).
A preparation method for solder, specifically completes according to the following steps:
One, by Ag powder, CuO powder and TiH
2powder mixes, and adds acetone wherein, then, under argon shield, with the speed ball milling 1h ~ 3h of 200r/min ~ 300r/min, obtains Ag-CuO-TiH
2powder; Wherein, described Ag powder and the mass ratio of CuO powder are 1:(0.06 ~ 0.17), described Ag powder and TiH
2the mass ratio of powder is 1:(0.01 ~ 0.11), abrading-ball is (4 ~ 6) with the mass ratio of the mixed powder added: 1, Ag powder, CuO powder and TiH
2the quality summation of powder is 1g:(0.45mL ~ 0.72mL with the ratio of the volume of acetone);
Two, to the Ag-CuO-TiH that step one obtains
2in powder, add Si
3n
4nano-ceramic particle and acetone, mix, and be then less than the condition of 5Pa in vacuum under, with the ball milling speed of 200r/min ~ 300r/min, ball milling 2h ~ 5h, obtains solder mixed-powder; Wherein, Ag-CuO-TiH
2in powder Ag with enter Si
3n
4the mass ratio of nano-ceramic particle is 1:(0.012 ~ 0.12), abrading-ball is (15 ~ 25) with the mass ratio of the summation of the powder added: 1, Ag-CuO-TiH
2powder and Si
3n
4the summation of the quality of nano-ceramic particle is 1g:(0.5mL ~ 0.8mL with the ratio of the volume of acetone);
Three, solder mixed-powder step 2 obtained mixes with binding agent, obtains paste solder, namely completes the preparation of solder; Wherein, the Ag in described solder mixed-powder and the mass ratio of binding agent are 1:(0.05 ~ 0.07).
Utilize solder to connect the method for sapphire and niobium or niobium alloy, specifically complete according to the following steps:
One, prepare sapphire sample, sapphire surface to be welded to surface roughness of polishing is 0.1 μm ~ 0.3 μm, prepares niobium or niobium alloy sample, and the surface roughness of polishing to surface to be welded is 0.1 μm ~ 0.2 μm; Sapphire sample after clean polishing and the surface of niobium or niobium alloy sample, obtain sapphire sample to be welded and niobium to be welded or niobium alloy sample;
Two, solder of the present invention being evenly coated in step one obtains on the surface to be welded of sapphire sample to be welded and the surface to be welded of niobium to be welded or niobium alloy sample, the coated side of sapphire sample to be welded with niobium to be welded or niobium alloy sample is docked and compacting, obtains pretreatment sample; Wherein, the pressure between the surface to be welded of sapphire sample to be welded and the surface to be welded of niobium to be welded or niobium alloy sample is 9.8 × 10
3pa ~ 10 × 10
3pa;
Three, be 0.6 × 10 in vacuum
-3pa ~ 1.5 × 10
-3under the condition of Pa, the pretreatment sample that step 2 is obtained, 410 DEG C ~ 480 DEG C are heated to from room temperature with the heating rate of 15 DEG C/min ~ 20 DEG C/min, insulation 10min ~ 20min, then, 700 DEG C ~ 750 DEG C are heated to the heating rate of 5 DEG C/min ~ 15 DEG C/min, insulation 15min ~ 25min, 1050 DEG C ~ 1150 DEG C are heated to again with the heating rate of 7 DEG C/min ~ 15 DEG C/min, insulation 20min ~ 30min, finally, 350 DEG C ~ 450 DEG C are cooled to the rate of temperature fall of 5 DEG C/min ~ 10 DEG C/min, afterwards, naturally cool to room temperature, namely the method utilizing solder to connect sapphire and niobium or niobium alloy is completed.
Advantage of the present invention: when solder provided by the invention is for connecting sapphire and niobium or niobium alloy, owing to adding nano ceramics phase particle in solder, greatly alleviate the residual stress produced because the coefficient of expansion does not mate, X ray test joint interface residual stress is only 5MPa, and adopt conventional Ag-Cu-Ti solder soldering under same process parameter, in postwelding joint, residual stress is then up to 65Mpa, and the weld interface obtained does not exist the defect of crackle or pore; Meanwhile, adopt solder of the present invention to connect the technique of sapphire and niobium or niobium alloy simply, the average shear strength of joint is up to 200MPa, and joint member can bear the high temperature of more than 1000 DEG C.
Accompanying drawing explanation
Fig. 1 is that the step 2 in test one obtains solder mixed-powder scanning electron microscope diagram.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of solder, it is by Ag powder, CuO powder, TiH
2powder, Si
3n
4nano-ceramic particle and binding agent are prepared from; Wherein, described Ag powder and the mass ratio of CuO powder are 1:(0.06 ~ 0.17), described Ag powder and TiH
2the mass ratio of powder is 1:(0.01 ~ 0.11), described Ag powder and Si
3n
4the mass ratio of nano-ceramic particle is 1:(0.012 ~ 0.12), described Ag powder and the mass ratio of binding agent are 1:(0.05 ~ 0.07).
TiH is selected in present embodiment
2as the interpolation form of active Ti, TiH
2can decompose by heating in vacuum dehydrogenation the Ti obtaining activating completely, effectively prevent active Ti oxidized.
Present embodiment has the following advantages: when the solder that present embodiment provides is for connecting sapphire and niobium or niobium alloy, owing to adding nano ceramics phase particle in solder, greatly alleviate the residual stress produced because the coefficient of expansion does not mate, X ray test joint interface residual stress is only 5MPa, and adopt conventional Ag-Cu-Ti solder soldering under same process parameter, in postwelding joint, residual stress is then up to 65Mpa, and the weld interface obtained does not exist the defect of crackle or pore; Meanwhile, adopt the solder of present embodiment to connect the technique of sapphire and niobium or niobium alloy simply, the average shear strength of joint is up to 200MPa, and joint member can bear the high temperature of more than 1000 DEG C.
Detailed description of the invention two: the difference of present embodiment and detailed description of the invention one is: described binding agent is mixed by glycerine, hydroxyethylcellulose and water; Wherein, described glycerine and the mass ratio of hydroxyethylcellulose are 1:(3 ~ 7), described glycerine and the mass ratio of water are 1:(90 ~ 92).Other is identical with detailed description of the invention one.
Detailed description of the invention three: the difference of present embodiment and detailed description of the invention one or two is: described Ag powder and the mass ratio of binding agent are 1:0.06.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: the preparation method that present embodiments provide for a kind of solder, specifically completes according to the following steps:
One, by Ag powder, CuO powder and TiH
2powder mixes, and adds acetone wherein, then, under argon shield, with the speed ball milling 1h ~ 3h of 200r/min ~ 300r/min, obtains Ag-CuO-TiH
2powder; Wherein, described Ag powder and the mass ratio of CuO powder are 1:(0.06 ~ 0.17), described Ag powder and TiH
2the mass ratio of powder is 1:(0.01 ~ 0.11), abrading-ball is (4 ~ 6) with the mass ratio of the mixed powder added: 1, Ag powder, CuO powder and TiH
2the quality summation of powder is 1g:(0.45mL ~ 0.72mL with the ratio of the volume of acetone)
Two, to the Ag-CuO-TiH that step one obtains
2in powder, add Si
3n
4nano-ceramic particle and acetone, mix, and be then less than the condition of 5Pa in vacuum under, with the ball milling speed of 200r/min ~ 300r/min, ball milling 2h ~ 5h, obtains solder mixed-powder; Wherein, Ag-CuO-TiH
2in powder Ag with enter Si
3n
4the mass ratio of nano-ceramic particle is 1:(0.012 ~ 0.12), abrading-ball is (15 ~ 25) with the mass ratio of the powder summation added: 1, Ag-CuO-TiH
2powder and Si
3n
4the summation of the quality of nano-ceramic particle is 1g:(0.5mL ~ 0.8mL with the ratio of the volume of acetone);
Three, solder mixed-powder step 2 obtained mixes with binding agent, obtains paste solder, namely completes the preparation of solder; Wherein, the Ag in described solder mixed-powder and the mass ratio of binding agent are 1:(0.05 ~ 0.07).
Use acetone abrasive media to play in present embodiment and accelerate ball milling process, reduce the surface energy of powder, stop powder aggegation, alleviate cold welding effect, improve flour extraction.
TiH is selected in present embodiment
2as the interpolation form of active Ti, TiH
2can decompose by heating in vacuum dehydrogenation the Ti obtaining activating completely, effectively prevent active Ti oxidized.
Present embodiment has the following advantages: when the solder that present embodiment provides is for connecting sapphire and niobium or niobium alloy, owing to adding nano ceramics phase particle in solder, greatly alleviate the residual stress X ray test joint interface residual stress produced because the coefficient of expansion does not mate and be only 5MPa, and adopting conventional Ag-Cu-Ti solder soldering under same process parameter, in postwelding joint, residual stress is then up to 65Mpa., there is not the defect of crackle or pore in the weld interface obtained; Meanwhile, adopt the solder of present embodiment to connect the technique of sapphire and niobium or niobium alloy simply, the average shear strength of joint is up to 200MPa, and joint member can bear the high temperature of more than 1000 DEG C.
Detailed description of the invention five: the difference of present embodiment and detailed description of the invention four is: the binding agent in described step 3 is mixed by glycerine, hydroxyethylcellulose and water; Wherein, described glycerine and the mass ratio of hydroxyethylcellulose are 1:(3 ~ 7), described glycerine and the mass ratio of water are 1:(90 ~ 92).Other is identical with detailed description of the invention four.
Detailed description of the invention six: the difference of present embodiment and detailed description of the invention four or five is: the Ag in the solder mixed-powder in described step 3 and the mass ratio of binding agent are 1:0.06.Other is identical with detailed description of the invention four or five.
Detailed description of the invention seven: present embodiments provide for the method utilizing solder to connect sapphire and niobium or niobium alloy, specifically complete according to the following steps:
One, prepare sapphire sample, sapphire surface to be welded to surface roughness of polishing is 0.1 μm ~ 0.3 μm, prepares niobium or niobium alloy sample, and the surface roughness of polishing to surface to be welded is 0.1 μm ~ 0.2 μm; Sapphire sample after clean polishing and the surface of niobium or niobium alloy sample, obtain sapphire sample to be welded and niobium to be welded or niobium alloy sample;
Two, the solder described in detailed description of the invention one being evenly coated in step one obtains on the surface to be welded of sapphire sample to be welded and the surface to be welded of niobium to be welded or niobium alloy sample, the coated side of sapphire sample to be welded with niobium to be welded or niobium alloy sample is docked and compacting, obtains pretreatment sample; Wherein, the pressure between the surface to be welded of sapphire sample to be welded and the surface to be welded of niobium to be welded or niobium alloy sample is 9.8 × 10
3pa ~ 10 × 10
3pa;
Three, be 0.6 × 10 in vacuum
-3pa ~ 1.5 × 10
-3under the condition of Pa, the pretreatment sample that step 2 is obtained, 410 DEG C ~ 480 DEG C are heated to from room temperature with the heating rate of 15 DEG C/min ~ 20 DEG C/min, insulation 10min ~ 20min, then, 700 DEG C ~ 750 DEG C are heated to the heating rate of 5 DEG C/min ~ 15 DEG C/min, insulation 15min ~ 25min, 1050 DEG C ~ 1150 DEG C are heated to again with the heating rate of 7 DEG C/min ~ 15 DEG C/min, insulation 20min ~ 30min, finally, 350 DEG C ~ 450 DEG C are cooled to the rate of temperature fall of 5 DEG C/min ~ 10 DEG C/min, afterwards, naturally cool to room temperature, namely the method utilizing solder to connect sapphire and niobium or niobium alloy is completed.
Pressure in present embodiment step 2 between sapphire sample to be welded and niobium to be welded or niobium alloy sample is 9.8 × 10
3pa ~ 10 × 10
3pa is the close contact in order to ensure sapphire and niobium or niobium alloy in welding process.
Adopt Segmented heating form in present embodiment step 3, ensure that binding agent fully can decompose volatilization at 410 DEG C ~ 480 DEG C temperature, then make TiH
2active Ti can be resolved into completely at 700 DEG C ~ 750 DEG C, finally with slower ramp to 1050 DEG C ~ 1150 DEG C, ensure that composite soldering sufficient wetting and spreading on mother metal, by the insulation of 20min ~ 30min, make solder and mother metal produce suitable metallurgical reaction and make brazing seam structure's homogenising, improve strength of joint, the cooldown rate of postwelding cooling employing 5 DEG C/min ~ 10 DEG C/min is the residual stress in order to reduce postwelding joint to the full extent, ensures the reliability of joint.
Present embodiment has the following advantages: when the solder that present embodiment provides is for connecting sapphire and niobium or niobium alloy, owing to adding nano ceramics phase particle in solder, greatly alleviate the residual stress X ray test joint interface residual stress produced because the coefficient of expansion does not mate and be only 5MPa, and adopting conventional Ag-Cu-Ti solder soldering under same process parameter, in postwelding joint, residual stress is then up to 65MPa., there is not the defect of crackle or pore in the weld interface obtained; Meanwhile, adopt the solder of present embodiment to connect the technique of sapphire and niobium or niobium alloy simply, the average shear strength of joint is up to 200MPa, and joint member can bear the high temperature of more than 1000 DEG C.
Detailed description of the invention eight: the difference of present embodiment and detailed description of the invention seven is: the polishing mode in described step one is: sapphire sample grinding machine is roughly ground, then grind with the waterproof abrasive paper of #240, #360, #600, #800, #1000, #1200 successively, then be that the diamond spraying polishing agent of 0.5 μm ~ 1.5 μm is by sapphire polishing 0.3h ~ 0.7h by granularity; Niobium or niobium alloy grind with the waterproof abrasive paper of #240, #360, #600, #800, #1000, #1200 successively.Other is identical with detailed description of the invention seven.
Detailed description of the invention nine: the difference of present embodiment and detailed description of the invention seven or eight is: the clean method in described step one is: the sapphire sample after polishing and niobium or niobium alloy sample acetone are soaked, ultrasonic cleaning 20min ~ 30min, cleaning temperature is 30 DEG C ~ 40 DEG C, then absolute ethyl alcohol wiping is used, specimen surface to be welded is cleaned, final drying again with the distilled water of flowing.Other is identical with detailed description of the invention seven or eight.
It is because ultrasonic wave is best 30 DEG C ~ 40 DEG C cavitation effects that present embodiment selects 30 DEG C ~ 40 DEG C to heat ultrasonic cleaning mode, can very fully remove specimen surface dirt, be the specimen surface in order to prevent the contaminating impurity in running water from having cleaned out with the distilled water replacement running water cleaning of flowing.
Detailed description of the invention ten: the difference of one of present embodiment and detailed description of the invention seven to nine is: it is 0.5mm ~ 0.8mm that the solder in described step 2 is evenly coated in the thickness that step one obtains the surface to be welded of sapphire sample to be welded, it is 0.5mm ~ 0.8mm that solder is evenly coated in the thickness that step one obtains the surface to be welded of niobium to be welded or niobium alloy sample.Other is identical with one of detailed description of the invention seven to nine.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of preparation method of solder, specifically completes according to the following steps:
One, by Ag powder, CuO powder and TiH
2powder mixes, and adds acetone wherein, then, under argon shield, with the speed ball milling 2h of 220r/min, obtains Ag-CuO-TiH
2powder; Wherein, described Ag powder and the mass ratio of CuO powder are 1:0.1, described Ag powder and TiH
2the mass ratio of powder is 1:0.05, and abrading-ball is 5:1, Ag powder, CuO powder and TiH with the mass ratio of the mixed powder added
2the quality summation of powder is 1g:0.5mL with the ratio of the volume of acetone;
Two, to the Ag-CuO-TiH that step one obtains
2in powder, add Si
3n
4nano-ceramic particle and acetone, mix, and then, be less than the condition of 5Pa in vacuum under, with the ball milling speed of 250r/min, ball milling 5h, obtains solder mixed-powder; Wherein, Ag-CuO-TiH
2in powder Ag with enter Si
3n
4the mass ratio of nano-ceramic particle is 1:0.1, and abrading-ball is 20:1, Ag-CuO-TiH with the mass ratio of the summation of the powder added
2powder and Si
3n
4the summation of the quality of nano-ceramic particle is 1g:0.7mL with the ratio of the volume of acetone;
Three, solder mixed-powder step 2 obtained mixes with binding agent, obtains paste solder, namely completes the preparation of solder; Wherein, described binding agent is mixed by glycerine, hydroxyethylcellulose and water; Described glycerine and the mass ratio of hydroxyethylcellulose are 1:4, and described glycerine and the mass ratio of water are 1:91, and the Ag in described solder mixed-powder and the mass ratio of binding agent are 1:0.06.
Solder mixed-powder is obtained to the step 2 in test one and carries out scanning electron microscope test, can Fig. 1 be obtained.From Fig. 1, nano level Si can be observed
3n
4be adsorbed on original Ag-CuO-Ti powder surface.
Test two: utilize solder to connect the method for sapphire and niobium or niobium alloy, specifically complete according to the following steps:
One, sapphire sample is prepared, sapphire sample grinding machine is roughly ground, then grind with the waterproof abrasive paper of #240, #360, #600, #800, #1000, #1200 successively, spray polishing agent by sapphire polishing 0.5h with the diamond that granularity is 1 μm again, and the surface roughness obtaining surface to be welded is the polishing sapphire of 0.2 μm; Preparing niobium sample, is 0.1 μm by the surface roughness that the waterproof abrasive paper of #240, #360, #600, #800, #1000, #1200 is ground to surface to be welded successively; Sapphire sample and niobium after polishing or niobium alloy sample acetone are soaked, ultrasonic cleaning 30min, cleaning temperature is 35 DEG C, then uses absolute ethyl alcohol wiping, then cleans specimen surface to be welded, final drying with the distilled water flowed;
Two, the solder of test one being evenly coated in step one obtains on the surface to be welded of sapphire sample to be welded and the surface to be welded of niobium to be welded or niobium alloy sample, the coated side of sapphire sample to be welded with niobium to be welded or niobium alloy sample is docked and compacting, obtains pretreatment sample; Wherein, the solder thickness of sapphire sample surface to be welded to be welded is 0.5mm, and the solder thickness of niobium to be welded or niobium alloy sample surface to be welded is 0.5mm, and the pressure between the surface to be welded of sapphire sample to be welded and the surface to be welded of niobium to be welded or niobium alloy sample is 10 × 10
3pa;
Three, be 1 × 10 in vacuum
-3under the condition of Pa, pretreatment sample step 2 obtained, is heated to 450 DEG C with the heating rate of 15 DEG C/min from room temperature, insulation 15min, then, is heated to 730 DEG C with the heating rate of 10 DEG C/min, insulation 20min, 1100 DEG C are heated to again, insulation 25min, finally with the heating rate of 8 DEG C/min, 400 DEG C are cooled to the rate of temperature fall of 9 DEG C/minn, afterwards, naturally cool to room temperature, namely complete the method utilizing solder to connect sapphire and niobium or niobium alloy.
X-ray is adopted to survey the residual stress at detection tabs interface to the joint of the connecting elements that test two obtains, obtaining residual stress is 5MPa, to Ag-Cu-Ti solder soldering under technological parameter identical with test two of existing employing conventional method, in postwelding joint, residual stress is then up to 65MPa, compare down, the residual stress of the joint of the connection member that test two obtains reduces greatly.
Carry out shear strength test to the joint of the connecting elements that test two obtains, the average shear strength that can obtain joint is 200MPa.
Carry out high temperature resistant test to the connecting elements that test two obtains, the serviceability temperature that can obtain joint can reach more than 1000 DEG C.
Claims (5)
1. a solder, it is by Ag powder, CuO powder, TiH
2powder, Si
3n
4nano-ceramic particle and binding agent are prepared from; Wherein, described Ag powder and the mass ratio of CuO powder are 1:(0.06 ~ 0.17), described Ag powder and TiH
2the mass ratio of powder is 1:(0.01 ~ 0.11), described Ag powder and Si
3n
4the mass ratio of nano-ceramic particle is 1:(0.012 ~ 0.12), described Ag powder and the mass ratio of binding agent are 1:(0.05 ~ 0.07);
Described binding agent is mixed by glycerine, hydroxyethylcellulose and water; Wherein, described glycerine and the mass ratio of hydroxyethylcellulose are 1:(3 ~ 7), described glycerine and the mass ratio of water are 1:(90 ~ 92);
The preparation method of described a kind of solder, specifically completes according to the following steps:
One, by Ag powder, CuO powder and TiH
2powder mixes, and adds acetone wherein, then, under argon shield, with the speed ball milling 1h ~ 3h of 200r/min ~ 300r/min, obtains Ag-CuO-TiH
2powder; Wherein, described Ag powder and the mass ratio of CuO powder are 1:(0.06 ~ 0.17), described Ag powder and TiH
2the mass ratio of powder is 1:(0.01 ~ 0.11), abrading-ball is (4 ~ 6) with the mass ratio of the mixed powder added: 1, Ag powder, CuO powder and TiH
2the quality summation of powder is 1g:(0.45mL ~ 0.72mL with the ratio of the volume of acetone);
Two, to the Ag-CuO-TiH that step one obtains
2in powder, add Si
3n
4nano-ceramic particle and acetone, mix, and be then less than the condition of 5Pa in vacuum under, with the ball milling speed of 200r/min ~ 300r/min, ball milling 2h ~ 5h, obtains solder mixed-powder; Wherein, Ag-CuO-TiH
2ag and Si in powder
3n
4the mass ratio of nano-ceramic particle is 1:(0.012 ~ 0.12), abrading-ball is (15 ~ 25) with the mass ratio of the summation of the powder added: 1, Ag-CuO-TiH
2powder and Si
3n
4the summation of the quality of nano-ceramic particle is 1g:(0.5mL ~ 0.8mL with the ratio of the volume of acetone);
Three, solder mixed-powder step 2 obtained mixes with binding agent, obtains paste solder, namely completes the preparation of solder; Wherein, the Ag in described solder mixed-powder and the mass ratio of binding agent are 1:(0.05 ~ 0.07).
2. utilize the solder described in claim 1 to connect the method for sapphire and niobium or niobium alloy, it is characterized in that: method specifically completes according to the following steps:
One, prepare sapphire sample, sapphire surface to be welded to surface roughness of polishing is 0.1 μm ~ 0.3 μm, prepares niobium or niobium alloy sample, and the surface roughness of polishing to surface to be welded is 0.1 μm ~ 0.2 μm; Sapphire sample after clean polishing and the surface of niobium or niobium alloy sample, obtain sapphire sample to be welded and niobium to be welded or niobium alloy sample;
Two, solder according to claim 1 being evenly coated in step one obtains on the surface to be welded of sapphire sample to be welded and the surface to be welded of niobium to be welded or niobium alloy sample, the coated side of sapphire sample to be welded with niobium to be welded or niobium alloy sample is docked and compacting, obtains pretreatment sample; Wherein, the pressure between the surface to be welded of sapphire sample to be welded and the surface to be welded of niobium to be welded or niobium alloy sample is 9.8 × 10
3pa ~ 10 × 10
3pa;
Three, be 0.6 × 10 in vacuum
-3pa ~ 1.5 × 10
-3under the condition of Pa, the pretreatment sample that step 2 is obtained, 410 DEG C ~ 480 DEG C are heated to from room temperature with the heating rate of 15 DEG C/min ~ 20 DEG C/min, insulation 10min ~ 20min, then, 700 DEG C ~ 750 DEG C are heated to the heating rate of 5 DEG C/min ~ 15 DEG C/min, insulation 15min ~ 25min, 1050 DEG C ~ 1150 DEG C are heated to again with the heating rate of 7 DEG C/min ~ 15 DEG C/min, insulation 20min ~ 30min, finally, 350 DEG C ~ 450 DEG C are cooled to the rate of temperature fall of 5 DEG C/min ~ 10 DEG C/min, afterwards, naturally cool to room temperature, namely the method utilizing solder to connect sapphire and niobium or niobium alloy is completed.
3. solder according to claim 2 connects the method for sapphire and niobium or niobium alloy, it is characterized in that: the polishing mode in described step one is: sapphire sample grinding machine is roughly ground, then grind with the waterproof abrasive paper of #240, #360, #600, #800, #1000, #1200 successively, then be that the diamond spraying polishing agent of 0.5 μm ~ 1.5 μm is by sapphire polishing 0.3h ~ 0.7h by granularity; Niobium or niobium alloy grind with the waterproof abrasive paper of #240, #360, #600, #800, #1000, #1200 successively.
4. the solder according to Claims 2 or 3 connects the method for sapphire and niobium or niobium alloy, it is characterized in that: the clean method in described step one is: the sapphire sample after polishing and niobium or niobium alloy sample acetone are soaked, ultrasonic cleaning 20min ~ 30min, cleaning temperature is 30 DEG C ~ 40 DEG C, then absolute ethyl alcohol wiping is used, specimen surface to be welded is cleaned, final drying again with the distilled water of flowing.
5. the solder according to Claims 2 or 3 connects the method for sapphire and niobium or niobium alloy, it is characterized in that: it is 0.5mm ~ 0.8mm that the solder in described step 2 is evenly coated in the thickness that step one obtains the surface to be welded of sapphire sample to be welded, it is 0.5mm ~ 0.8mm that solder is evenly coated in the thickness that step one obtains the surface to be welded of niobium to be welded or niobium alloy sample.
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Cited By (1)
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| CN107414228A (en) * | 2017-08-01 | 2017-12-01 | 合肥利裕泰玻璃制品有限公司 | A kind of processing technology of sapphire glass component |
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| CN103993359B (en) * | 2014-04-30 | 2017-01-04 | 洛阳金诺机械工程有限公司 | A kind of welding process of sapphire wafer |
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| CN105364245B (en) * | 2015-12-17 | 2017-11-03 | 哈尔滨工业大学 | A kind of sapphire low-temperature welding method |
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| CN110405379B (en) * | 2018-04-27 | 2020-11-13 | 哈尔滨工业大学 | Ag-CuO-B2O3Brazing filler metal, preparation method thereof and method for connecting sapphire by using brazing filler metal |
| CN114939753B (en) * | 2022-05-18 | 2023-11-24 | 上海工程技术大学 | Composite brazing filler metal for brazing sapphire and kovar alloy and brazing process thereof |
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