CN101428979B - Vacuum diffusion welding process for glass and metal - Google Patents
Vacuum diffusion welding process for glass and metal Download PDFInfo
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- CN101428979B CN101428979B CN2008102430687A CN200810243068A CN101428979B CN 101428979 B CN101428979 B CN 101428979B CN 2008102430687 A CN2008102430687 A CN 2008102430687A CN 200810243068 A CN200810243068 A CN 200810243068A CN 101428979 B CN101428979 B CN 101428979B
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Abstract
The invention relates to a glass and metal vacuum diffusion welding technology, which comprises the following steps: 1) glass and metal weldments are subjected to surface treatment; and 2) the treated weldments are arranged in a high vacuum solid-state pressure diffusion welding furnace, and the vacuum is pumped for vacuum diffusion welding, wherein the step 1) comprises: step 1.1) the metal weldment is subjected to cleaning and surface finish treatment, and the surface of the glass weldment is cleaned; and step 1.2) the surface of the metal weldment is subjected to pre-oxidization treatment. The technology has the advantages that the technology improves the tensile strength, service life and vacuum tightness of glass and metal sealing joints, and has low cost and good economic effect.
Description
Technical field
What the present invention relates to is a kind of technique manufacturing method that utilizes the vacuum diffusion welding connection technology to carry out glass-to-metal seal, and this processing method can be used in the middle of the solar energy thermal-power-generating technology.
Background technology
It is that two kinds of foreign materials are placed in the vacuum chamber that vacuum diffusion welding connects, and under certain vacuum ranges, and is being heated to below the fusing point of welding material under certain pressure, allows atom spread mutually to realize a kind of solid welding method of welding.Existing metal and nonmetallic vacuum pressure diffusion technology for welding comprise following processing step: (1) carries out surface treatment with weldment, and when metal welding fitting thickness during greater than 2 millimeters, is offering a circle stress groove near the outside of diffusion welding face; Then the weldment of handling well is installed in the solid-state pressure of the high vacuum diffusion brazier and vacuumizes; (2) in stove vacuum in (2-4) * 10
-4Begin during Pa stove heating, in furnace temperature during less than 400 ℃, but in every 4-6 minute heat temperature raising 20-50 ℃; When temperature during greater than 400 ℃, but every 40-80 in second heat temperature raising 8-12 ℃; When temperature during greater than 550 ℃, be incubated 13-17 minute, need heat temperature raising then badly to 600-640 ℃, be incubated and begin cooling after 50-70 minute; (3) be between 640-380 ℃ the time in furnace temperature, should in every 4-6 minute, lower the temperature 8-12 ℃; In furnace temperature is between 380-280 ℃ the time, should lower the temperature 8-12 ℃ in every 10-15 minute; When temperature during, can move back temperature naturally less than 280 ℃; When temperature during less than 16 ℃, can stop to vacuumize, stop plus-pressure until shutdown; (4) in the furnace temperature temperature-rise period, also answer plus-pressure; When furnace temperature rose to 420-480 ℃, the beginning plus-pressure was to 0.2-0.3kg/mm
2, pressurization in every then 4-6 minute once adds up 2.5kg/mm
2, the stagnation pressure pressurization finishes; Pressurize is to shutting down then.
Along with the modern science technology develops rapidly, glass and metal diffusing sealing technology can will apply in the generating of paraboloid trough type solar heat, promptly obtain high-quality solar energy evacuated absorption tube, can improve the efficient of solar thermal power generation greatly, have higher requirement but so simultaneously also glass and metal are got sealing technology.Sealing-in at the glass and the metal of routine, only be being connected of glass and metal alloy, metal is the alloy of main iron content, cobalt, nickel, with high-boron-silicon glass the comparatively approaching coefficient of expansion is arranged, the coefficient of expansion of the two material differs in ± 10%, and the intensity of sealing-in joint is not very high.But in the environment for use of paraboloid trough type solar heat generating, the glass-to-metal seal joint is required can be higher, particularly the requirement aspect mechanical property for example also should have anti-fatigue performance except requiring the glass-to-metal seal joint to possess higher anti-static load stretch capability far above the application performance requirement at electronics.Because under the Circulation of thermal fatigue load, the often generation of glass-to-metal seal joint damage failure phenomenon.Adopt not only technological operation step of above-mentioned prior art complexity, and can not solve the generation damage failure phenomenon of glass-to-metal seal joint.
Summary of the invention
The objective of the invention is at the problems referred to above, improve with the metal sealing manufacturing process nonmetal, the manufacturing process of a kind of glass and metal vacuum diffusion welding is proposed, this technique manufacturing method has improved the tensile strength of glass-to-metal seal joint and work-ing life, vacuum-tightness, and cost is low, has good economical effectiveness.This technology can be applied in the middle of the solar thermal power generation.
Glass and metal vacuum diffusion technology for welding, this technology may further comprise the steps: 1) glass and metal welding fitting are carried out surface treatment; 2) weldment of handling well is installed in the solid-state pressure diffusion of the high vacuum brazier, vacuumizes, carry out vacuum diffusion welding and connect; Above-mentioned steps 1) comprise in:
Step 1.1) the metal welding fitting is cleaned and the surface smoothness processing, clean is carried out on glass weldment surface;
Step 1.2) metal welding fitting surface carries out pre-oxidation treatment.
Above-mentioned steps 1.1) cleaning and the surface treatment of material are in order to satisfy the requirement of diffusion technology for welding before the butt welding.Glass and metal also require both to have good binding ability, i.e. wettability except both coefficients of expansion are consistent.In order to reach this target, metal is carried out clean.
Above-mentioned steps 1.2) be glass and metal diffusing the welding in important step.Because the difference of chemical bond, metal itself can not with glass sealing.The sealing-in of metal and glass is actually carries out pre-oxidation treatment with metal, at high temperature the oxide film of metal and glass soak into fusion then, be that metal and high silicon boron glass are that oxide compound by the metallic surface and glass dissolve each other and is closely linked, so the preoxidation of metal is very important process procedure in glass and the metal diffusing welding, is an important factor that directly influences hermetic seal.
Above-mentioned steps 1.1) further comprises in: the metal welding fitting is placed on earlier uses ultrasonic cleaning in the ethanolic soln, polish after with sand paper and abrasive paper for metallograph metal welding fitting end face being polished then, obtain bright and clean end face, use acetone, ethanol, clear water clean surface more respectively; The glass weldment is used acetone, ethanol, clear water clean surface respectively, and last metal and glass weldment are dried in baking oven.
Susceptibility to Superficial Foreign Body in diffusion welding is very high, and carbon-containing impurities such as micro-grease not only can influence the diffusion welding quality.Therefore, test sample is needing before the diffusion welding through cleaning so that remove foreign matter and the grease that adheres on all surfaces completely.
Above-mentioned steps 1.2) further comprise in: metal under 1000 ℃, with N
2+ H
2O+H
2Be incubated 25min in the atmosphere, carry out oxidation and obtain with Fe
3O
4Oxide film for main component.In the atmosphere of mixed gas, also be to reach good wetting effect in order to form oxide skin in the metallic surface to metal heat treatmet.Oxide thickness is relevant with the intensity and the ventilation property of diffusion welding.The lepthymenia meeting of oxidation causes metal and the direct sealing-in of glass, influences intensity; Oxide film is blocked up then at the residual more oxide film of metallic surface meeting, thereby causes gas leakage.General oxide thickness is 2.5-6g/m
2
As a further improvement on the present invention: the weldment installation steps above-mentioned steps 2) further comprise: metal and glass face of weld are contacted the resistant to elevated temperatures anchor clamps of upper and lower end face single raise.In order to prevent from crushed breakage of glass and the welding process to keep the release of enough pressure and welding residual stress, described anchor clamps inboard adds expanded graphite, and in addition bolting is good in the anchor clamps both sides.When weldment was pipe fitting, described anchor clamps adopted symmetric semicircle, and symmetric semicircle expanded graphite is set in the anchor clamps inboard.In order to produce enough pressure, in metal tube or Glass tubing, add expanded graphite.
As a further improvement on the present invention, above-mentioned steps 2) in vacuum diffusion welding connect and further comprise following technical process:
The weldment that fixes is positioned in the middle of the diffusion brazier vacuum chamber, and closes fire door;
The vacuum system of brazier is spread in startup, will spread in the brazier to vacuumize 1.3 * 10
-3Below the Pa, making welding pressure is 5-10MPa;
Start heating system, weldment is with stove heat temperature raising to 400～450 ℃, and insulation 20-30 minute, makes the temperature at each position of weldment even, and the diffusion brazier continues to heat up 720～750 ℃, and vacuum tightness remains on 1.3 * 10
-2～1.3 * 10
-3Pa, insulation is slowly cooled off with stove more than 10～15 minutes then, and tapping temperature is below 50 ℃.
Glass and metal diffusing weldprocedure significant parameter have the control of maximum heating temperature, soaking time, welding pressure.In the vacuum diffusion welding termination process, these three parameters are to determine whether glass combines with the metal solder interfacial diffusion abundant, thus the key of decision quality of weld joint quality.Adopt vacuum diffusion welding of the present invention to connect step, technical process is simple, and the tensile strength of welding joint reaches 30Mpa, and is good with the heat-collecting pipe vacuum resistance to air loss of this technology welding, its leak rate can≤5 * 10
-11Pam
3/ s (helium mass spectrum leak detection), greatly improve than prior art work-ing life.
Beneficial effect of the present invention is, the use of before vacuum diffusion welding connects, carrying out cleaning and metal pre-oxidation treatment and having the special fixtures of graphite, the welding joint resistance to air loss is improved, employing is than the simple weldprocedure of prior art, by to maximum heating temperature, soaking time, welding pressure parameter control, avoid in the welding process reaching better welding effect because of the different stress damages that cause of the coefficient of expansion of glass and metal, destruction.
Description of drawings
Fig. 1 is the embodiment of the invention 1 glass and metal diffusing welded and installed synoptic diagram.
Fig. 2 is the embodiment of the invention 2 glass and metal diffusing welded and installed synoptic diagram.
Fig. 3 is the A-A sectional view of Fig. 2.
Fig. 4 is the embodiment of the invention 1 and embodiment 2 glass and metal diffusing welding process process flow sheet.
Embodiment
Below in conjunction with accompanying drawing invention is described further.
A kind of glass and metal vacuum diffusion technology for welding, metal are the alloys of main iron content, cobalt, nickel, and this technology may further comprise the steps:
1) glass and metal welding fitting are carried out surface treatment:
I. the metal welding fitting is placed on earlier and uses ultrasonic cleaning in the ethanolic soln, polish after with 800# sand paper and abrasive paper for metallograph metal welding fitting end face being polished then, obtain bright and clean end face, use acetone, ethanol, clear water clean surface more respectively; The glass weldment is used acetone, ethanol, clear water clean surface respectively, and last metal and glass weldment are dried in stoving oven.
Ii. the metal welding fitting under 1000 ℃, and N
2+ H
2O+H
2Be incubated 25min in the atmosphere, carry out oxidation and obtain with Fe
3O
4Oxide film for main component.
2) weldment of handling well is installed in the solid-state pressure diffusion of the high vacuum brazier, vacuumizes, carry out vacuum diffusion welding and connect:
I. metal 1 and glass 2 face of weld are contacted the resistant to elevated temperatures plate anchor clamps 3 of upper and lower end face single raise.In order to prevent to keep in crushed breakage of glass and the welding process release of unrelieved stress in enough pressure and the welding process, the anchor clamps inboard adds expanded graphite 4, and in the anchor clamps both sides in addition bolting is good, glass 2 installs and fixes mode as shown in Figure 1 with metal 1 diffusion welding.
Ii. carrying out vacuum diffusion welding connects:
The sample to be welded that fixes is positioned in the middle of the diffusion brazier vacuum chamber, and closes fire door;
Before the diffusion welding, the vacuum system of brazier is spread in startup, will spread in the brazier to vacuumize 1.3 * 10
-3Below the Pa, welding pressure is 5～10MPa;
Start heating system, to-be-welded pieces is with stove heat temperature raising to 400～450 ℃, and insulation 20-30 minute, makes the temperature at each position of weldment even, and the diffusion brazier continues to heat up 720～750 ℃, and vacuum tightness remains on 1.3 * 10
-2～1.3 * 10
-3Pa, this temperature is the diffusion welding temperature of glass and metal, and the nickel element under this temperature in the metal is in best flow state, considers body material thickness and unit construction, and insulation is slowly cooled off with stove more than 10～15 minutes then, and tapping temperature is below 50 ℃.Glass and the technical process of metal diffusing welding process are as shown in Figure 4.
The present embodiment difference from Example 1 is step 2) in the i step be:
The present invention can be widely used in the middle of the solar thermal power generation, will improve the efficient of sun power paraboloid trough type solar heat generating greatly, thereby alleviating energy crisis reduces Greenhouse effect.
Claims (6)
1. glass and metal vacuum diffusion technology for welding, this technology may further comprise the steps: 1) glass and metal welding fitting are carried out surface treatment; 2) weldment of handling well is installed in the solid-state pressure diffusion of the high vacuum brazier, vacuumizes, carry out vacuum diffusion welding and connect; It is characterized in that above-mentioned steps 1) in comprise:
Step 1.1) the metal welding fitting is cleaned and the surface smoothness processing, glass surface is carried out clean;
Step 1.2) metal welding fitting surface carry out pre-oxidation treatment: the metal welding fitting under 1000 ℃, and N
2+ H
2O+H
2Be incubated 15min in the environment, carry out oxidation and obtain with Fe
3O
4Oxide film for main component;
Above-mentioned steps 2) comprises in: the weldment that fixes is positioned in the middle of the diffusion brazier vacuum chamber, and closes fire door;
The vacuum system of brazier is spread in startup, will spread in the brazier to vacuumize 1.3 * 10
-3Below the Pa, making welding pressure is 5-10MPa;
Start heating system, weldment be incubated 20-30 minute with stove heat temperature raising to 400～450 ℃, makes the temperature at each position of weldment even, and the diffusion brazier continues 720～750 ℃ of intensifications, and vacuum tightness remains on 1.3 * 10
-2～1.3 * 10
-3Pa is incubated 10～15 minutes, slowly cools off with stove then, and tapping temperature is below 50 ℃.
2. weldprocedure according to claim 1, it is characterized in that, above-mentioned steps 1.1) further comprises in: the metal welding fitting is placed on earlier uses ultrasonic cleaning in the ethanolic soln, polish after with sand paper and abrasive paper for metallograph metal welding fitting end face being polished then, obtain bright and clean end face, use acetone, ethanol, clear water clean surface more respectively; The glass weldment is used acetone, ethanol, clear water clean surface respectively, and last metal and glass weldment are dried in stoving oven.
3. weldprocedure according to claim 1 is characterized in that, above-mentioned steps 2) in the weldment installation steps further comprise: metal and glass face of weld are contacted the resistant to elevated temperatures anchor clamps of upper and lower end face single raise.
4. weldprocedure according to claim 3 is characterized in that, adds expanded graphite in described anchor clamps inboard.
5. weldprocedure according to claim 3 is characterized in that described anchor clamps adopt symmetric semicircle, and symmetric semicircle expanded graphite is set in the anchor clamps inboard.
6. weldprocedure according to claim 5 is characterized in that, adds expanded graphite in the inboard of described metal or glass.
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|---|---|---|---|
| CN2008102430687A CN101428979B (en) | 2008-11-28 | 2008-11-28 | Vacuum diffusion welding process for glass and metal |
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|---|---|---|---|
| CN2008102430687A CN101428979B (en) | 2008-11-28 | 2008-11-28 | Vacuum diffusion welding process for glass and metal |
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| CN101428979B true CN101428979B (en) | 2011-11-09 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101708964B (en) * | 2009-11-26 | 2011-08-17 | 南京工业大学 | Glass and metal vacuum brazing technique |
| CN103172277A (en) * | 2011-12-23 | 2013-06-26 | 北京有色金属研究总院 | Hermetic seal method of optical glass and Kovar alloy |
| CN102976635B (en) * | 2012-12-14 | 2015-03-11 | 哈尔滨工业大学 | Method for connecting glass with copper or copper alloy |
| CN107096994A (en) * | 2017-04-25 | 2017-08-29 | 南京云启金锐新材料有限公司 | The diffusion welding (DW) fitting and its production method of a kind of high-purity zirconia composite ceramics and red copper |
| CN107285649B (en) * | 2017-08-17 | 2021-04-23 | 合肥晶鼎光电科技有限公司 | Low-melting-point glass sealing method |
| CN111348842B (en) * | 2018-12-24 | 2022-12-02 | 有研工程技术研究院有限公司 | Automatic glass-metal sealing equipment and method for solar heat collecting tube |
| CN110668709A (en) * | 2019-10-10 | 2020-01-10 | 杭州航天电子技术有限公司 | Airtight sealing method for kovar alloy and glass |
| CN112091536A (en) * | 2020-08-14 | 2020-12-18 | 陕西千山航空电子有限责任公司 | Aluminum frame type part and vacuum connection method and application thereof |
| CN114349321B (en) * | 2022-01-08 | 2022-10-18 | 江苏博联硕焊接技术有限公司 | Vacuum diffusion welding equipment for high-light-transmittance borosilicate glass and using method thereof |
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