CN1267242C - Anode welding process for metal-glass and metal-ceram - Google Patents
Anode welding process for metal-glass and metal-ceram Download PDFInfo
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- CN1267242C CN1267242C CN 200310105894 CN200310105894A CN1267242C CN 1267242 C CN1267242 C CN 1267242C CN 200310105894 CN200310105894 CN 200310105894 CN 200310105894 A CN200310105894 A CN 200310105894A CN 1267242 C CN1267242 C CN 1267242C
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Abstract
The present invention discloses an anode welding method for metal, glass and ceramic, which belongs to the technical field of the connection of dissimilar materials. The welding of the present invention is carried out in the atmosphere, and the welding temperature of the present invention is low. The present invention can directly carry out the connection in a solid state under the condition of no addition of materials, the deformation of workpieces is small, and the technological processes are simple; the present invention can realize precision welding in vacuum or shielding gas atmosphere, and realize the precision welding in the air. The present invention can be used for the matched sealing and the unmatched sealing of various nonmetal medium materials (such as pyrex glass, sodium-calcium silicate glass, oxidation alumino-silicate glass, fiber-optic glass, quartz, sapphire, nucleated glass, beta-Al2O3 ceramic, etc.), alloys of kovar (Kovar), Fe-Ni, Al, Cu, Ti, etc., metal and simiconductor materials (such as Si, Ga, As, etc.) The technology of the present invention has high requirements for the surface process precision; the present invention is mainly used for manufacturing micromachines and microsensors, and used for electrovacuum field and aerospace field.
Description
Technical field
The invention belongs to the interconnection technique field of dissimilar materials.Be particularly related to the anode welding method between a kind of metal and the aluminium oxide ceramics.
Background technology
Along with the development of science and technology and new material, metal is also constantly advancing with (sealing-in) technology that is connected of glass and pottery (insulating materials) always, and the application in industry is more and more, and importance grows with each passing day.
The method of attachment of metal and pottery and glass mainly contains: vacuum brazing, splicing, steaming.There is following defective usually in said method:
Pottery is connected higher temperature of needs and vacuum equipment with the vacuum brazing of metal, and energy consumption is bigger.
The method of steaming is that pottery or glass are placed vacuum, makes the metal gasification, thereby with pottery or metal surface metallization, energy consuming ratio is bigger.
Metal and pottery and glass bonding, though method is simple, serviceability temperature is not high, bond strength is lower, long service, bonding agent can wear out, and makes adhesive failure.
Anode is welded in late 1960s and is found and applied for a patent by Daniel.I.Pomerantz.Development is the time of existing three more than ten years so far.During this, people such as Wallis, Pomerantz, Anthony, Albaugh, Denee, Arata have made a few thing, and the research of being carried out focuses mostly on the structure of glass and silicon, glass and metal.The emphasis of its research is in vacuum or the welding under inert gas shielding, and the scope of its welding is subjected to the restriction of vacuum equipment.
Summary of the invention
The objective of the invention is to, the welding method of the anode between a kind of metal and the aluminium oxide ceramics is provided.
The technical solution that realizes above-mentioned purpose is that the anode welding method between a kind of metal and the aluminium oxide ceramics is characterized in that, carries out according to the following steps:
1) divides other single face to carry out the machine glazed finish processing on soldered metal and aluminium oxide ceramics joint material, after then in acetone and alcohol, cleaning, dry respectively, press between the burnishing surface in conjunction with assembling;
2) sample that assembles is put on the stove anchor clamps fixed, wherein aluminium oxide ceramics connects negative electrode, and metal material connects anode;
3) anchor clamps are placed on are warmed up to 300 ℃～500 ℃ in the stove, apply the DC voltage of 400V～600V, pressure 5Pa～10Pa, after holding temperature, the voltage 30～50min, DC voltage is stopped, cool to room temperature with the furnace, above-mentioned joint can be welded together, the strength of joint that obtains is 18MPa～25Mpa;
When 4) powering up intensification, start recorder, record current in loop situation of change, antianode weldering process is carried out monitoring.
Some other characteristics of the present invention are to need not to add the intermediate layer between the joint faying face.
The roughness of described machine glazed finish is 0.5 μ m～1.0 μ m.
The stove of heating usefulness need not to vacuumize, the atmospheric environment of welding atmosphere for not circulating.
Adopt method of the present invention, need not pressurization or apply light pressure, under the DC electric field effect, solder side fits together, after temperature raises, under electric field action, make nonmetallic materials generation polarization and electronics and ion are moved to the interface, physical-chemical reaction is taking place at the interface, form oxide and spinelle, realize integrated connection.
Description of drawings
Fig. 1 is an anode welder schematic diagram of the present invention;
Fig. 2 is that the heating furnace intensification powers up the mode curve map;
Fig. 3 is embodiments of the invention K
4Glass and Kovar alloy interface power spectrum line sweep be collection of illustrative plates as a result;
Fig. 4 is K
4The stereoscan photograph (Mag=4000X) of glass and silicon weldering.
For a more clear understanding of the present invention, the present invention is described in further detail below in conjunction with drawings and Examples.
The specific embodiment
According to technical scheme of the present invention, the anode welding method between metal and the aluminium oxide ceramics, the welding process that this method is carried out is all carried out under atmospheric conditions, mainly examines or check the influence to welding process of temperature, voltage, conduction time.Experimental rig principle such as Fig. 1 show.This device comprises heating furnace and electrical power control cabinet, between heating furnace and the electrical power control cabinet tape deck is arranged.
To be carried out machine glazed finish processing (0.5 μ m-1 μ m) by weldering sample single face before the experiment, and then clean in acetone and alcohol respectively, and after the oven dry sample that assembles be put on the stove anchor clamps and fix, wherein aluminium oxide ceramics connects negative electrode, and metal connects anode.Begin the energising that heats up, intensification, energising, insulation, outage, cooling method are as shown in Figure 2.When powering up, start recorder, record current in loop situation of change.After stopping to power up, the sample cooling is taken out during to room temperature.
Method of the present invention is also applicable to metal and nonmetal, and dissimilar materials such as semiconductor and glass carry out anodic bonding welding, different material anode welding condition temperature, voltage, the corresponding change of temperature retention time.
Below be the embodiment that the inventor provides, but the invention is not restricted to these embodiment.
Embodiment 1: aluminium-K
4The anodic bonding of glass
The material constituent:
This experiment material is K
4Glass and fine aluminium, glass and aluminium flake are 12mm * 12mm, and machine glazed finish all need be carried out in the surface, and clean in acetone and alcohol respectively.Welding process is carried out the welding in the atmosphere in experimental facilities shown in Figure 1, postwelding cools to room temperature with the furnace.
In optimal processing parameter (250 ℃～400 ℃ of temperature, voltage 600V～800V), the seam rate reaches more than 90%, and test shows that the seam rate increases with the increase of temperature and voltage.The effect of the temperature that raises is to make the more weak ion of connection in the glass break away from constraint, and directed moving taken place under electric field action.The raising of temperature helps the carrying out of ions diffusion.But the raising of temperature, make the aggravation of two kinds of material coefficient of thermal expansion coefficient mismatch problems, simultaneous temperature bring up to a threshold value (〉=400 ℃, 800V) after, will be easy to puncture, so temperature should not be too high.In addition, the effect of voltage is to form electric field, produces powerful electric field force, makes the workpiece driving fit.Equally, after voltage is added to certain value (〉=800V, 400 ℃), also be easy to puncture, so the selection of voltage also need be decided on selected materials and temperature.In a word, temperature and voltage have the problem of an optimum Match.
The postwelding cooling velocity is excessive, is easy to generate bigger residual stress, thereby causes the welding failure, therefore needs the control cooling velocity.Cooling rate is controlled at 4K/s～5K/s can reaches best welding effect.The shape of time, pressure, programming rate, electrode etc. all has the effect that can not be ignored to welding process.
The anodic bonding of glass and aluminium is by the alkaline kation Na+ in the glass, O2-, and the transmission of H+ is carried out, and the Na+ in the glass is main conducting ion.
Embodiment 2: kovar alloy-K
4The anodic bonding of glass
Can cut down (Kovar) alloy and have linear expansion coefficient close and good low-temperature stability with Pyrex at 20 ℃～450 ℃, with the metal solder process in, can reduce the thermal stress that produce owing to the foreign material thermal coefficient of expansion is different.The weldment of this alloy and glass is mainly used in the electrovacuum components and parts, locates as transmitting tube, oscillator, sealing plug, magnetron etc.
K
4Glass specimen is of a size of 10mm * 10mm * 2mm, and the Kovar alloy sample is of a size of 10mm * 10mm * 15mm.
Process of the test is with K
4Glass and Kovar alloy carry out surperficial single-sided polishing to be handled, and surface roughness reaches 0.5 μ m～1.0 μ m, uses acetone and alcohol wash again, and two burnishing surfaces are fitted relatively, puts into anchor clamps and assembles, and wherein, the Kovar alloy links to each other with anode, K
4Glass links to each other with negative electrode, as shown in Figure 1.After weldment assembled, putting into stove heats, when temperature rises to assigned temperature, add certain DC voltage (U) again, after keeping 15～50min, deenergization, weldment cools off with stove, when welding temperature between 350 ℃～450 ℃, weldingvoltage is between 800V～900V the time, the tensile strength of the welding point of acquisition is 10MPa～20MPa.
In the anodic bonding process, since the effect of extra electric field, K
4Na in the glass
+Move to negative electrode, make that the one side near anode produces poor Na in the glass
+The district.The ion migration that produces under the highfield effect, cation active in glass comprise that also the cation that connects in the anode metal moves in glass to negative electrode moves, and sluggish relatively anion anode migration in the glass.In stripping section, because Na
+To cathodic migration, cause that negative electrical charge increases, therefore produce the negative electrical charge accumulation regions near vitreum one side at stripping section, form powerful electric field between this district and the anode, two kinds of materials are closely contacted.In the non-negative electrical charge accumulation regions of stripping section, the anode metal cation spreads in glass, and the anion anode in the glass moves, and finally the chemical metallurgy reaction is taking place at the interface, and the complex chemical compound that is generated links together welded part securely.
At welding Kovar alloy and K
4During glass, cracking phenomena does not take place almost, this makes the Kovar alloy become a kind of desirable glass welding material.
Kovar alloy and K
4Glass has formed with FeSiO in the anodic bonding process
3And Fe
7SiO
10And some amorphous substances are main transition zone, and with the materials to be welded seam together.K
4Glass and Kovar alloy interface power spectrum line sweep result are as shown in Figure 3.
Embodiment 3:K
4The anodic bonding of glass and monocrystalline silicon piece
K
4The specimen size of glass is 10mm * 10mm * 2mm.The specimen size of single crystalline Si sheet is 10mm * 10mm * 0.3mm.
Soldering test device and process sample carry out surface finish (roughness 0.5～1.0 μ m) and surface clean (with acetone and alcohol wash surface) before assembling, put into stove after two samples are assembled, and wherein silicon chip links to each other with anode, and glass is connected with negative electrode.After treating that sample is heated to 350 ℃～400 ℃ temperature, give by the weldering sample to add 710V～840V DC voltage, behind maintenance 15～50min, deenergization, test specimen cools off with stove.
In welding process,, after discovery welding current dullness rises to a maximum, slowly descend with the variation of test macro record current.In welding process, produce faint electric current in the circuit, this phenomenon shows that the glass intermediate ion moves under electric field action, thereby produces electric current in the loop, and along with the prolongation of time, ion moves and is tending towards saturated, and electric current reduces gradually.At a certain temperature, with reducing of electric-field intensity, welding process ion migration amount reduces, and welding current reduces.When voltage was constant, temperature reduced, and the ions diffusion ability weakens, and the welding process electric current reduces.
The seam rate increases with the rising of temperature under certain voltage, because temperature is high more, help ions diffusion migration more, but temperature can not surpass certain value, otherwise can cause the excessive and puncture test specimen of electric current.Equally, within the specific limits, the seam rate increases with the rising of voltage.
As seen, K
4There is an optimal processing parameter scope when glass and silicon chip welding, in this scope, welds, all can obtain desirable welding point.Evidence K
4Optimal processing parameter when glass and silicon chip welding is voltage: 710V～840V, temperature: 350 ℃～400 ℃.
K
4Glass belongs to SiO
2B
2O
3More alkali metal oxide is contained in NaO glass system, the oxide of sodium especially, and in welding process, electric current is mainly by the alkali metal ion conduction, and contains Al in glass
2O
3The time, can impel the active increase of alkali metal ion.Sodium ion is assembled to negative electrode under effect of electric field, makes glass be produced the poor Na of one deck by the face of weld
+The district, and at the another side of glass with Na
+Or the NaOH form is separated out.Simultaneously, Si forms joint closely with the oxonium ion generation electrochemical reaction of assembling to weld seam.Temperature raises or field intensity increases, and the ion mobility strengthens, and impels silicon and oxygen diffusivity to strengthen, and adhesion increases at the faying face place, and the stereoscan photograph of welding point as shown in Figure 4.
In welding process,, can eliminate, in this welding procedure, obtain satisfied effect by postheating owing to the different stress that produces of two material thermal expansion coefficients.
Mechanical test proof K
4The anodic bonding of glass and silicon chip can obtain the high quality welding joint, and the tensile strength of joint is greater than mother metal.
Embodiment 4:Y-ZrO2 is connected with the anodic bonding of aluminium foil
ZrO2 is an oxonium ion type conductivity ceramics, has high temperature resistant and the high advantage of conductance, is the excellent material of fuel cell and chemical sensor.Improved the shortcoming of the low and thermal shock resistance difference of ceramic original toughness with the toughness reinforcing ZrO2 of Y2O3.Wherein aluminium foil links to each other with anode, and Y-ZrO2 is connected with negative electrode.300 ℃～500 ℃ of welding temperatures, voltage 800V～1000V, pressure 5Pa～10Pa, time 30min～50min; The strength of joint that obtains is greater than 25MPa.
Embodiment 5: aluminum matrix composite is connected with pottery
Aluminum matrix composite most widely used general and the most ripe successfully is applied to Aeronautics and Astronautics, vehicle and electron trade.Metal-base composites is except high strength, high elastic modulus and low-expansion coefficient, also have good toughness, shock resistance and thermal shock resistance, the hear resistance height, the transverse mechanical performance is good, does not burn, and is nonhygroscopic, conduction and thermal conductivity are good, radiation hardness, and series of advantages such as high vacuum environment is stable have become the preferred material of microelectronic component substrate.
The aluminum matrix composite that adopts the SiC particle to strengthen is connected with β-Al2O3 with Pyrex respectively.Wherein aluminum matrix composite connects anode, and Pyrex and β-Al2O3 connect negative electrode.300 ℃～500 ℃ of welding temperatures, voltage 400V～600V, pressure 5Pa～10Pa, time 15min～30min; The strength of joint that obtains is 18MPa～25Mpa.
Claims (4)
1. the anode welding method between metal and the aluminium oxide ceramics is characterized in that, carries out according to the following steps:
1) divides other single face to carry out the machine glazed finish processing on soldered metal and aluminium oxide ceramics joint material, after then in acetone and alcohol, cleaning, dry respectively, press between the burnishing surface in conjunction with assembling;
2) sample that assembles is put on the stove anchor clamps fixed, wherein aluminium oxide ceramics connects negative electrode, and metal material connects anode;
3) anchor clamps are placed on are warmed up to 300 ℃～500 ℃ in the stove, apply the DC voltage of 400V～600V, pressure 5Pa～10Pa, after holding temperature, the voltage 30～50min, DC voltage is stopped, cool to room temperature with the furnace, above-mentioned joint can be welded together, the strength of joint that obtains is 18MPa～25Mpa;
When 4) powering up intensification, start recorder, record current in loop situation of change, antianode weldering process is carried out monitoring.
2. method according to claim 1 is characterized in that, need not to add the intermediate layer between the joint faying face.
3. method according to claim 1 and 2 is characterized in that, the roughness of described machine glazed finish is 0.5 μ m～1.0 μ m.
4. method according to claim 1 is characterized in that, the stove of heating usefulness need not to vacuumize, the atmospheric environment of welding atmosphere for not circulating.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310105894 CN1267242C (en) | 2003-11-07 | 2003-11-07 | Anode welding process for metal-glass and metal-ceram |
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|---|---|---|---|
| CN 200310105894 CN1267242C (en) | 2003-11-07 | 2003-11-07 | Anode welding process for metal-glass and metal-ceram |
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| CN1267242C true CN1267242C (en) | 2006-08-02 |
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| CN100404452C (en) * | 2005-12-13 | 2008-07-23 | 武汉理工大学 | Process for super low temp, anode bonding of microcrystal glass and stainless steel and apparatus thereof |
| CN100364707C (en) * | 2006-03-24 | 2008-01-30 | 中国科学院上海技术物理研究所 | Vacuum seal welding method for window and optic window of low temperature metal Dewar |
| CN1974462B (en) * | 2006-12-14 | 2010-05-12 | 太原理工大学 | Common-anode electrostatic field connection process of multilayer glass and metal |
| JP5268002B2 (en) * | 2007-07-25 | 2013-08-21 | 国立大学法人 熊本大学 | Welding method of metallic glass and crystalline metal by high energy beam |
| CN103011625B (en) * | 2012-12-27 | 2014-12-24 | 中天科技精密材料有限公司 | Method for connecting high-purity glass tube and metal tube in manufacturing of ultralow-water-peak optical fiber preform |
| CN103949742B (en) * | 2014-04-25 | 2016-02-10 | 甘肃虹光电子有限责任公司 | A kind of sapphire sheet and metal active method for sealing |
| CN104692676B (en) * | 2015-02-15 | 2017-01-18 | 太原理工大学 | Electric-field-assisted diffusion bonding device and method for glass tubes and metal plates |
| CN106392388B (en) * | 2016-10-14 | 2018-06-01 | 深圳市品川新能源技术有限公司 | Ceramics and conductor welding procedure |
| CN109926748B (en) * | 2019-03-22 | 2021-06-01 | 中国科学院上海光学精密机械研究所 | Vacuum observation window sealed by metal solder and manufacturing method thereof |
| CN113843468A (en) * | 2021-09-22 | 2021-12-28 | 长江师范学院 | Method for connecting metal and ceramic in industrial atmosphere |
| CN116352233B (en) * | 2023-05-30 | 2023-08-22 | 中镱新材料智能制造研究院(山西)有限公司 | Manufacturing method for fused accumulation additive of ejection type ceramic particle reinforced composite material |
| CN118084359B (en) * | 2024-04-22 | 2024-07-09 | 太原理工大学 | Vacuum diffusion connection method for sodium-calcium-silicon glass and metal |
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