CN100404452C - Process for super low temp, anode bonding of microcrystal glass and stainless steel and apparatus thereof - Google Patents
Process for super low temp, anode bonding of microcrystal glass and stainless steel and apparatus thereof Download PDFInfo
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- CN100404452C CN100404452C CNB2005100200009A CN200510020000A CN100404452C CN 100404452 C CN100404452 C CN 100404452C CN B2005100200009 A CNB2005100200009 A CN B2005100200009A CN 200510020000 A CN200510020000 A CN 200510020000A CN 100404452 C CN100404452 C CN 100404452C
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- glass
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- stainless steel
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
Abstract
The present invention relates to an anode bonding method of nucleated glass and stainless steel materials at ultralow temperature, and a device. The method comprises the following steps that firstly, the sample glass is smelted and processed by a heat treatment technology; then, the obtained nucleated glass substrate and the stainless steel substrate are polished, cleaned, dried, and rapidly put in an anode bonding device so as to achieve effective anode bonding at 100 to 180 DEG C at bonding voltage of 600 to 1000V, and thus, novel bonding materials are obtained. The device is provided with a vacuum pump (1), a temperature controller (2), a vacuum chamber (3) and a high-temperature camera device (7), wherein the inner cavity of the vacuum chamber is orderly provided with a cathode (4), a nucleated glass substrate (5), a stainless steel substrate (6), an anode (8), a heating plate (9) and a cooling water pipe (10) from top to bottom. The present invention can realize the effective anode bonding of the materials at low bonding temperature and bonding voltage, and thereby, novel materials with low residual stress, high bond strength and favorable sealability are obtained.
Description
Technical field
The present invention relates to special glass manufacturing technology field and micro-electromechanical system field, the very low temperature anode linkage method of particularly a kind of devitrified glass and stainless material.
Background technology
The thermal bonding technology comprises anode linkage, Direct Bonding, fusion bonding and eutectic bonding etc. at present, though the thermal bonding technology has more advantage, but its critical defect is to need pyroprocessing, to obtain enough bonded energies (as silicon-silicon anode linkage: 350～450 ℃; Silicon-Si direct bonding:＞800 ℃; Fusion bonding:＞1000 ℃; Eutectic bonding: 363 ℃).High bonding temperature not only can cause big unrelieved stress, thereby bond strength is reduced, and this strain also can cause having existed the structure of parts and performance to change, as the resistance to fatigue to device very big influence is just arranged, and can make it to produce distortion.Obviously the height of temperature or the distribution of heat are the important factors that influences bonding quality in the thermal bonding process.Therefore reduce bonding temperature, improve bonding quality, significant.
As everyone knows, glass is of paramount importance substrate material or packaged material in the present micro-system field.Glass has stronger rigidity, good stopping property, has good insulation performance performance and heat-insulating property under the normal temperature.In micro mechanical sensor, during as the substrate of silicon device, the distributed capacity of device is little, thermonoise is little with glass; , not only have transparent characteristic, and have good air-tightness during with glass as the packaged material of device.Therefore, its purposes in micro mechanical sensor is increasingly extensive.Though glass is ideal bonding seal, sealing materials, the glass bonding of only under high bonding temperature, just realizing ideal, and cause big bonding stress thus, and sheet glass under high pressure easily punctures in addition, and rate of etch is also lower.Therefore, cooperate research fast, low temperature, high-quality anode linkage technology, seek satisfactory novel material and just have important and practical meanings.
A kind of metal that patent CN1541802A introduces and the anode welding process between glass and the pottery are used for being connected between under comparatively high temps various glass, ceramic and metal, the alloy.
In addition, do not retrieve other relevant patent or paper.
Summary of the invention
Technical problem to be solved by this invention is: the very low temperature anode linkage method of a kind of devitrified glass and stainless material is provided, so that under the state more much lower than conventional bonding temperature, and preparation devitrified glass and stainless bonding novel material.
The technical scheme that the present invention solves its technical problem employing is: be Li with mother glass at first
2O-ZnO-SiO
2The raw material of system glass is founded and is handled by thermal treatment process, obtains glass-ceramic substrate.Adopt then glossing with glass-ceramic substrate and stainless steel substrate polish, clean, drying, put in the anode linking device rapidly again, the very low temperature and the bonding voltage that make it at 100～180 ℃ are to realize effective anode linkage of devitrified glass and stainless material under 600～1000V state, thereby obtain new bonding material.Wherein, mother glass is made of the composition of following mass percent: SiO
255～70, ZnO 1～20, Li
2O 10～30, Al
2O
31～10, K
2O 2～6, Na
2O 2～6, P
2O
31～5.
The very low temperature anode linking device of devitrified glass provided by the invention and stainless material, its structure is: the vacuum pump that is provided with vacuum chamber and is attached thereto, inner chamber at vacuum chamber is equipped with negative electrode, glass-ceramic substrate, stainless steel substrate, anode, hot-plate and water-cooled tube from top to bottom successively, and temperature regulator and high temperature camera head are housed in the side of vacuum chamber.Wherein, negative electrode links to each other with a contact of digital signal converter by lead, and connects altogether through another contact of variable resistor and digital signal converter and the negative pole of direct supply controller, and anode is linked to each other by the positive pole of lead with the direct supply controller; The adjustable power of hot-plate, its temperature controlling range are 100～200 ℃; Digital signal converter links to each other with computer.
Advantage of the present invention is: owing to designed advanced technology and device, particularly adopted and glass, ceramic phase ratio, the microcrystal glass material that performance is more superior, its thermal expansivity can be adjusted to and the stainless steel approximate match, can be (under 600～1000V) states at lower bonding temperature (100～180 ℃) and bonding voltage, realize effective anode linkage of devitrified glass and stainless material, thereby the acquisition unrelieved stress is little, bond strength is high, the high quality bonding novel material of good airproof performance.
Description of drawings
Accompanying drawing is the structural representation of very low temperature anode linking device of the present invention.
Embodiment
The invention will be further described below in conjunction with embodiment.
One, the very low temperature anode linkage method of devitrified glass and stainless material
Adopt Li earlier
2O-ZnO-SiO
2(LZS) system glass, form and corresponding heat treating regime by selecting suitable glass, acquisition is suitable for the devitrified glass of very low temperature anode linkage and forms and best heat treating regime, control its principal crystalline phase, crystalline content and grain-size size, obtaining principal crystalline phase is the devitrified glass of two lithium silicates and/or cristobalite etc., prepares the glass-ceramic substrate with stainless material thermal expansivity approximate match in the bonding temperature scope.Again glass-ceramic substrate and stainless steel substrate polished, clean, drying.Then, put them into realize devitrified glass and metal stainless material in the anode linking device effective anode linkage immediately, thereby obtain high-quality bonding novel material.Specific as follows:
Be Li at first with mother glass
2O-ZnO-SiO
2The raw material of system glass is founded and is handled by thermal treatment process, obtains glass-ceramic substrate, and the principal crystalline phase of this substrate is two lithium silicates and/or cristobalite.
Adopt then glossing with glass-ceramic substrate and stainless steel substrate polish, clean, drying, put in the anode linking device rapidly again, the very low temperature and the bonding voltage that make it at 100～180 ℃ are effective anode linkage of realizing devitrified glass and stainless material under 600～1000V state, thus the bonding novel material that acquisition conforms to quality requirements.
Above-mentioned mother glass can be made of the composition of following mass percent: SiO
255～70, ZnO 1～20, Li
2O 10～30, Al
2O
31～10, K
2O 2～6, Na
2O 2～6, P
2O
31～5.
Above-mentioned melting technology parameter recommendation is: 1350～1450 ℃ of glass melting temperatures, soaking time 2～5 hours.
Above-mentioned heat treatment process parameter suggestion is: 500～600 ℃ of nucleation temperatures, 700～900 ℃ of crystallization temperatures.
In constant temperature, clean working environment glass-ceramic substrate and stainless steel substrate are polished, the suggestion of its glossing is: selecting fusing point for use is that 1710 ℃, Morse hardness are 7, granularity is nano level SiO
2Colloidal solution is as polishing fluid, and its mass concentration is 50～70%; The speed range of lower main axis is 30～100rpm on the polishing machine; Glass-ceramic substrate and stainless steel substrate polishing time are respectively 10～30,3～10min.
Above-mentioned cleaning suggestion is: dividing two sections to clean to glass-ceramic substrate in class 100 clean room, is earlier 80～90% dense HNO in mass concentration
3In clean 10min, use deionized water rinsing again, change mass concentration then over to and be 60～70% HNO
3The middle 15min that cleans uses deionized water rinsing again; Stainless steel cleans 5min with acetone, uses alcohol wash 5min, gets final product with deionized water rinsing 10min again.
Glass-ceramic substrate after the cleaning and stainless steel substrate can adopt the high speed rotating method to carry out drying.High speed rotating method exsiccant principle is: utilize centrifuging make on-chip fluid or moisture under action of centrifugal force with substrate separation, thereby reach the exsiccant purpose.Its speed range is 150～200rpm.
Below, enumerate several examples of having done according to the method described above:
Example 1; Adopt Li
2O-ZnO-SiO
2(LZS) system glass, its glass ingredient are SiO
256%, ZnO 12%, Li
2O 23%, Al
2O
36%, K
2O 2%, P
2O
31%.The melting technology parameter is: 1350 ℃ of glass melting temperatures, soaking time 2hr; Heat treatment process parameter is: 540 ℃ of nucleation temperatures, soaking time 2hr; 750 ℃ of crystallization temperatures, soaking time 2hr.Obtaining principal crystalline phase is the glass-ceramic substrate of two lithium silicates.
Selecting fusing point then for use is that 1710 ℃, Morse hardness are 7, granularity is nano level SiO
2Colloidal solution is as polishing fluid, and its mass concentration is 50%; The speed range of lower main axis is 50rpm on the polishing machine; Polishing time: glass-ceramic substrate 10min, stainless steel substrate 5min; In constant temperature, clean working environment, glass-ceramic substrate and stainless steel substrate are polished.
Dividing two sections to clean to devitrified glass in class 100 clean room, is earlier 80% dense HNO in mass concentration
3In clean 10min, use deionized water rinsing again, change concentration then over to and be 60% HNO
3The middle 15min that cleans uses deionized water rinsing again; Stainless steel cleans 5min with acetone, uses alcohol wash 5min, gets final product with deionized water rinsing 10min again.Make glass-ceramic substrate and stainless steel substrate drying by the high speed rotating method at last.
Immediately print being put in the special anode linking device, is that 100 ℃ and bonding voltage are under the 1000V state at bonding temperature, realizes effective anode linkage of devitrified glass and stainless material, thus acquisition bonding novel material.
Example 2: adopt Li
2O-ZnO-SiO
2(LZS) system glass, its glass ingredient are SiO
260%, ZnO 15%, Li
2O 20%, Al
2O
32%, Na
2O 2%, P
2O
31%.The melting technology parameter is: 1400 ℃ of glass melting temperatures, soaking time 2hr; Heat treatment process parameter is: 560 ℃ of nucleation temperatures, soaking time 2hr; 800 ℃ of crystallization temperatures, soaking time 2hr.Obtaining principal crystalline phase is the glass-ceramic substrate of two lithium silicates, cristobalite etc.
Selecting fusing point then for use is that 1710 ℃, Morse hardness are 7, granularity is nano level SiO
2Colloidal solution is as polishing fluid, and its mass concentration is 60%; The speed range of lower main axis is 60rpm on the polishing machine; Polishing time: glass-ceramic substrate 20min, stainless steel substrate 7min; In constant temperature, clean working environment, glass-ceramic substrate and stainless steel substrate are polished.
Dividing two sections to clean to glass-ceramic substrate in class 100 clean room, is earlier 80% dense HNO in mass concentration
3In clean 10min, use deionized water rinsing again, change mass concentration then over to and be 60% HNO
3The middle 15min that cleans uses deionized water rinsing again; Stainless steel substrate cleans 5min with acetone, uses alcohol wash 5min, gets final product with deionized water rinsing 10min again.Make glass-ceramic substrate and stainless steel substrate drying by the high speed rotating method at last.
Immediately print being put in the special anode linking device, is that 140 ℃ and bonding voltage are under the 800V state at bonding temperature, realizes effective anode linkage of devitrified glass and stainless material, thus acquisition bonding novel material.
Example 3: adopt Li
2O-ZnO-SiO
2(LZS) system glass, its glass ingredient are SiO
264%, ZnO 17%, Li
2O 15%, Al
2O
32%, K
2O 1%, P
2O
31%.The melting technology parameter is: 1450 ℃ of glass melting temperatures, soaking time 2hr; Heat treatment process parameter is: 580 ℃ of nucleation temperatures, soaking time 2hr; 850 ℃ of crystallization temperatures, soaking time 2hr.Obtaining principal crystalline phase is the glass-ceramic substrate of cristobalite.
Selecting fusing point then for use is that 1710 ℃, Morse hardness are 7, granularity is nano level SiO
2Colloidal solution is as polishing fluid, and its mass concentration is 70%; The speed range of lower main axis is 70rpm on the polishing machine; Polishing time: glass-ceramic substrate 30min, stainless steel substrate 9min; In constant temperature, clean working environment, glass-ceramic substrate and stainless steel substrate are polished.
Dividing two sections to clean to glass-ceramic substrate in class 100 clean room, is earlier 80% dense HNO in mass concentration
3In clean 10min, use deionized water rinsing again, change mass concentration then over to and be 60% HNO
3The middle 15min that cleans uses deionized water rinsing again; Stainless steel substrate cleans 5min with acetone, uses alcohol wash 5min, gets final product with deionized water rinsing 10min again.Make glass-ceramic substrate and stainless steel substrate drying by the high speed rotating method at last.
Immediately print being put in the special anode linking device, is that 180 ℃ and bonding voltage are under the 600V state at bonding temperature, realizes effective anode linkage of devitrified glass and stainless material, thus acquisition bonding novel material.
Two. the very low temperature anode linking device of devitrified glass and stainless material
This device is for realizing the special very low temperature anode linking device of technical solution of the present invention, its structure is as shown in the figure: the vacuum pump 1 that is provided with vacuum chamber 3 and is attached thereto, inner chamber at vacuum chamber is equipped with negative electrode 4, glass-ceramic substrate 5, stainless steel substrate 6, anode 8, hot-plate 9 and water-cooled tube 10 from top to bottom successively, and temperature regulator 2 and high temperature camera head 7 are housed in the side of vacuum chamber.Wherein, negative electrode links to each other with a contact of digital signal converter by lead, and connects altogether through variable resistor 11 and another contact of digital signal converter and the negative pole of direct supply controller, and anode is linked to each other by the positive pole of lead with the direct supply controller; The adjustable power of hot-plate, by temperature regulator control, the temperature controlling range that makes hot-plate is 100～200 ℃.Water-cooled tube carries out controlled chilling to Heating element.The high temperature camera head is monitored in real time to the bonding process of material.Digital signal converter links to each other with computer.
Above-mentioned vacuum chamber 3 can be made by No. 340 stainless materials, and it is shaped as rectangular parallelepiped, and indoor size suggestion is 500mm * 400mm * 300mm, stainless steel thickness of slab 10～15mm.Hot-plate 6 can adopt the resistance wire heating, and silicon carbide is as the heating panel, and its thickness is 15～18mm.
Claims (4)
1. the anode linkage method of devitrified glass and stainless material is Li with mother glass at first
2O-ZnO-SiO
2The raw material of system glass is founded and is handled by thermal treatment process, obtain glass-ceramic substrate, adopt then glossing with glass-ceramic substrate and stainless steel substrate polish, clean, drying, put in the anode linking device rapidly again, the very low temperature and the bonding voltage that make it at 100～180 ℃ are effective anode linkage of realizing devitrified glass and stainless material under 600～1000V state, thereby obtain new bonding material, it is characterized in that mother glass is made of the composition of following mass percent: SiO
255～70, ZnO1～20, Li
2O10～30, Al
2O
31～10, K
2O2～6, Na
2O2～6, P
2O
31～5.
2. the anode linkage method of devitrified glass according to claim 1 and stainless material is characterized in that the composition that described mother glass replaces with by following mass percent is constituted: SiO
256%, ZnO12%, Li
2O23%, Al
2O
36%, K
2O2%, P
2O
31%.
3. the anode linkage method of devitrified glass according to claim 1 and stainless material is characterized in that the composition that described mother glass replaces with by following mass percent is constituted: SiO
260%, ZnO15%, Li
2O20%, Al
2O
32%, Na
2O2%, P
2O
31%.
4. the anode linkage method of devitrified glass according to claim 1 and stainless material is characterized in that the composition that described mother glass replaces with by following mass percent is constituted: SiO
264%, ZnO17%, Li
2O15%, Al
2O
32%, K
2O1%, P
2O
31%.
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|---|---|---|---|---|
| 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 |
| CN103130180B (en) * | 2011-12-02 | 2015-10-28 | 中国科学院微电子研究所 | A kind of wafer scale anode linkage method |
| CN103626121A (en) * | 2013-04-27 | 2014-03-12 | 苏州迪纳精密设备有限公司 | Anodic automatic bonding equipment |
| CN104760927B (en) * | 2014-01-06 | 2016-08-31 | 无锡华润上华半导体有限公司 | The method of bonding |
| CN106277800B (en) * | 2016-08-26 | 2019-10-11 | 湖北戈碧迦光电科技股份有限公司 | Li2O-Al2O3-SiO2The preparation method and application of system glass ceramics |
| CN108529885B (en) * | 2017-03-06 | 2019-10-15 | 中国科学院上海硅酸盐研究所 | One kind can anode linkage LTCC material and its preparation method and application |
| CN108328912B (en) * | 2018-04-08 | 2020-01-31 | 武汉理工大学 | anodic bonding method and device for vacuum glass sealing |
| CN113072309A (en) * | 2021-03-11 | 2021-07-06 | 卓外（上海）医疗电子科技有限公司 | Method suitable for jointing lens material and metal material |
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