CN108439814A - A kind of plasma-activated Direct Bonding method using vapor pretreating surface - Google Patents

A kind of plasma-activated Direct Bonding method using vapor pretreating surface Download PDF

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Publication number
CN108439814A
CN108439814A CN201810380619.8A CN201810380619A CN108439814A CN 108439814 A CN108439814 A CN 108439814A CN 201810380619 A CN201810380619 A CN 201810380619A CN 108439814 A CN108439814 A CN 108439814A
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China
Prior art keywords
plasma
vapor
quartz glass
activated
bonding method
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CN201810380619.8A
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CN108439814B (en
Inventor
王晨曦
许继开
康秋实
聂啸
卢达洲
吴斌
戚晓芸
田艳红
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Harbin Institute of Technology
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Harbin Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C15/00Surface treatment of glass, not in the form of fibres or filaments, by etching
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00Annealing glass products
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0005Other surface treatment of glass not in the form of fibres or filaments by irradiation
    • C03C23/006Other surface treatment of glass not in the form of fibres or filaments by irradiation by plasma or corona discharge
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C27/00Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06Joining glass to glass by processes other than fusing

Abstract

The invention discloses a kind of plasma-activated Direct Bonding method using vapor pretreating surface, the method specific implementation step is as follows:One, quartz glass to be bonded is placed on the sample stage of vapor treatment and carries out steam treatment;Two, using plasma activates the quartz glass after steam treatment;Three, the quartz glass after will be plasma-activated is bonded, and is stood under atmosphere at room temperature environment;Four, the quartz glass after fitting is kept the temperature.The present invention it is plasma-activated it is preceding quartz glass is handled using vapor, it is plasma-activated compared to single, under identical annealing temperature and annealing time, the bond strength between quartz glass and quartz glass can be significantly increased.

Description

A kind of plasma-activated Direct Bonding method using vapor pretreating surface
Technical field
The invention belongs to wafer bond techniques fields, are related to a kind of plasma-activated bonding method of glass, and in particular to A kind of low-temperature direct bonding method plasma-activated using vapor pretreated glass.
Background technology
Glass is the amorphous material for the single component being made of silica, and close structure has fabulous light saturating The property crossed, coefficient of thermal expansion are extremely low(5.6×10-7/K), heat resisting temperature is up to 1000 DEG C or more.In addition to hydrofluoric acid, glass at room temperature Glass is hardly reacted with other acid or alkali, has good chemical stability.Based on above-mentioned advantage possessed by glass, usually It is applied to imaging sensor, solar cell and fiber waveguide device etc..Wafer bonding refer to by clean surface be bonded after, Under the action of external energy so that interface, which is formed, to be covalently attached, the process to be combined as a whole.Key between glass and glass It closes, since the transmission of the light to different-waveband is bigger, high mechanical strength is widely used in the preparation of microfluidic device.
Currently, the bonding method between glass mainly has melting bonding method and plasma-activated bonding method.But melting key It is legal to usually require to realize higher bond strength under 800 ~ 1000 DEG C of high annealing, easily damage the sensitive member of temperature The function of device.And plasma-activated bonding method when annealing temperature be less than 250 DEG C when, bond strength is extremely low, or even can not hold Generated mechanical stress in by subsequent mechanical process.Therefore, the low temperature between glass(≤ 200℃)Bonding is for temperature The exploitation of sensitive microfluidic device has important research significance with application.
Invention content
Based on the high problem of above-mentioned bonding temperature, the present invention provides a kind of using vapor pretreating surface Plasma-activated Direct Bonding method.This method can realize glass and glass under the annealing temperature not higher than 200 DEG C High intensity is bonded.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of plasma-activated Direct Bonding method using vapor pretreating surface realizes that low temperature is high according to the following steps Intensity is bonded:Glass pre-process using vapor treatment → using plasma to the glass of steam treatment into It anneals under the plasma-activated glass surface → low temperature of row activation → fitting, specific implementation step is as follows:
One, glass to be bonded is placed on the sample stage of vapor treatment and carries out steam treatment, at the vapor The temperature of reason is 150 ~ 500 DEG C, and the time is 0.5 ~ 30min;
Two, using plasma activates the glass after steam treatment, and the gaseous species of the plasma are O2With N2, the power of activation process is 50 ~ 300W, and the time is 0.5 ~ 10min;
Three, the glass after will be plasma-activated is bonded, and is stood under atmosphere at room temperature environment, and the time of the standing is 12~72h;
Four, the glass after fitting being kept the temperature, the temperature of the heat preservation is 100 ~ 200 DEG C, the time is 2 ~ for 24 hours.
The bonding principle of the present invention is as follows:
Stress corrosion and the H of water can occur in water vapor atmosphere for glass2O can occur anti-with the Si-O-Si structures of glass surface It answers:Si-O-Si + H2O → Si-OH+HO-Si, on the one hand so that the Si-OH density of glass surface increases, more It is hydrophilic;On the other hand, a degree of softening can occur for glass surface, be conducive to the interatomic phase counterdiffusion in interface.Through it is equal from After daughter processing, the Si-OH density of glass surface can further increase, and surface can become more smooth so that quartz glass is easy In bonding, and higher bond strength is obtained under process annealing.
Compared with the prior art, the present invention has the following advantages:
The present invention it is plasma-activated it is preceding glass is handled using vapor, it is plasma-activated compared to single, Under identical annealing temperature and annealing time, the bond strength between glass and glass can be significantly increased.
Description of the drawings
Fig. 1 is the bonding method process flow chart of the present invention;
Fig. 2 is that oxygen plasma activates after pre-processing 10min using oxygen plasma activation and 170 DEG C of vapor in embodiment 1 The pre- bond strength bar chart of glass/glass;
In figure:1 is quartz glass, and 2 be vapor treatment sample stage, and 3 be deionized water, and 4 be culture dish, and 5 be warm table, 6 be plasma-activated device(Manufacturer is Germany Plasmatechnology GmbH, model PlasmaFlecto 10), 6-1 is activated gas air inlet, and 6-2 is air inlet, and 6-3 is plasma-activated device sample stage, and 6-4 is vacuum Bleeding point, 6-5 are power supply adaptor, and 7 be heating and thermal insulation stove.
Specific implementation mode
Technical scheme of the present invention is further described with reference to embodiment, however, it is not limited to this, every right Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit of the technical scheme of the invention and range, should all be contained It covers in protection scope of the present invention.
Embodiment 1:
A kind of plasma-activated Direct Bonding method using vapor pretreating surface is present embodiments provided, such as Fig. 1 institutes Show, specific implementation step is as follows:
(1)Quartz glass is pre-processed using vapor treatment:
Quartz glass to be bonded is placed on the sample stage of vapor treatment, 10min is handled at a temperature of 170 DEG C.
As shown in Figure 1, vapor treatment used in the present embodiment is by warm table, the first culture dish, the second culture dish, sample Four parts of sample platform form, wherein:The first culture dish and the second culture dish are provided on the warm table, and the first culture dish is set In in the second culture dish, sample stage is placed in the first culture dish;The manufacturer of the warm table is CHEMAT Co., Ltds, type Number it is MODEL KW-4AH, heating temperature is controllable at 50 ~ 500 DEG C;First culture dish and the second culture dish be it is cylindric, first A diameter of 60 ~ 80mm of culture dish is highly 10 ~ 15mm, and wall thickness is 1 ~ 3mm, the diameter of the second culture dish is 100 ~ 120mm is highly 20 ~ 25mm, and wall thickness is 1 ~ 3mm;The sample stage be cuboid, length be 30 ~ 50mm, width be 30 ~ 50mm is highly 15 ~ 18mm.
(2)Using plasma activates the quartz glass of steam treatment:
Using O2Plasma activates 1 min to the quartz glass after steam treatment under the power of 150W.
(3)It is bonded plasma-activated Quartz glass surfaces:
By O2Quartz glass fitting after plasma-activated, and 24 h are stood under atmosphere at room temperature environment.It can from Fig. 2 Go out, after steam treatment, pre- bond strength is substantially improved.
(4)It anneals under low temperature:
Fitting quartz glass/quartz glass is annealed at a temperature of 150 DEG C, and keeps the temperature 12 h.
Embodiment 2:
A kind of plasma-activated Direct Bonding method using vapor pretreating surface is present embodiments provided, such as Fig. 1 institutes Show, specific implementation step is as follows:
(1)Quartz glass is pre-processed using vapor treatment:
Quartz glass to be bonded is placed on the sample stage of vapor treatment, 10min is handled at a temperature of 200 DEG C.
(2)Using plasma activates the quartz glass of steam treatment:
Using O2Plasma activates 1 min to the quartz glass after steam treatment under the power of 100 W.
(3)It is bonded plasma-activated Quartz glass surfaces:
By O2Quartz glass fitting after plasma-activated, and stood for 24 hours under atmosphere at room temperature environment.
(4)It anneals under low temperature:
Fitting quartz glass/quartz glass is annealed at a temperature of 150 DEG C, and keeps the temperature 12h.
Embodiment 3:
A kind of plasma-activated Direct Bonding method using vapor pretreating surface is present embodiments provided, such as Fig. 1 institutes Show, specific implementation step is as follows:
(1)Quartz glass is pre-processed using vapor treatment:
Quartz glass to be bonded is placed on the sample stage of vapor treatment, 15min is handled at a temperature of 150 DEG C.
(2)Using plasma activates the quartz glass of steam treatment:
Using N2Plasma activates 1.5min to the quartz glass after steam treatment under the power of 150W.
(3)It is bonded plasma-activated Quartz glass surfaces:
By N2Quartz glass fitting after plasma-activated, and stand 36h under atmosphere at room temperature environment.
(4)It anneals under low temperature:
Fitting quartz glass/quartz glass is annealed at a temperature of 150 DEG C, and keeps the temperature 12h.

Claims (6)

1. a kind of plasma-activated Direct Bonding method using vapor pretreating surface, it is characterised in that the method has Body implementation steps are as follows:
One, quartz glass to be bonded is placed on the sample stage of vapor treatment and carries out steam treatment;
Two, using plasma activates the quartz glass after steam treatment;
Three, the quartz glass after will be plasma-activated is bonded, and is stood under atmosphere at room temperature environment;
Four, the quartz glass after fitting is kept the temperature.
2. the plasma-activated Direct Bonding method according to claim 1 using vapor pretreating surface, special Sign is that the temperature of the steam treatment is 150 ~ 500 DEG C, and the time is 0.5 ~ 30min.
3. the plasma-activated Direct Bonding method according to claim 1 using vapor pretreating surface, special Sign is that the gaseous species of the plasma are O2And N2
4. the plasma-activated Direct Bonding method according to claim 1 using vapor pretreating surface, special Sign is that the power of the activation process is 50 ~ 300W, and the time is 0.5 ~ 10min.
5. the plasma-activated Direct Bonding method according to claim 1 using vapor pretreating surface, special Sign is that the time of the standing is 12 ~ 72h.
6. the plasma-activated Direct Bonding method according to claim 1 using vapor pretreating surface, special Sign be the heat preservation temperature be 100 ~ 200 DEG C, the time be 2 ~ for 24 hours.
CN201810380619.8A 2018-04-25 2018-04-25 Plasma activation direct bonding method for surface pretreatment by using water vapor Active CN108439814B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109081595A (en) * 2018-09-30 2018-12-25 江苏耀兴安全玻璃有限公司 A kind of preparation method of devitrified glass
CN110473778A (en) * 2019-08-17 2019-11-19 哈尔滨工业大学 A method of utilizing plasma-activated Direct Bonding zirconium oxide and aluminum oxide

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101990697A (en) * 2008-04-10 2011-03-23 信越化学工业株式会社 Method for manufacturing bonded substrate
US20110290320A1 (en) * 2006-10-30 2011-12-01 Shin-Etsu Chemical Co., Ltd. Method for producing single crystal silicon solar cell and single crystal silicon solar cell
CN105016632A (en) * 2015-06-12 2015-11-04 哈尔滨工业大学深圳研究生院 Method of cryogenic surface activation direct bonding for preparation of quartz glass capillary tube
CN105161437A (en) * 2015-09-18 2015-12-16 北京工业大学 Plasma-assisted glass or quartz chip microstructure alignment and pre-bonding method
CN105197880A (en) * 2014-06-24 2015-12-30 中芯国际集成电路制造(上海)有限公司 Bonding method of wafers with cavities

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110290320A1 (en) * 2006-10-30 2011-12-01 Shin-Etsu Chemical Co., Ltd. Method for producing single crystal silicon solar cell and single crystal silicon solar cell
CN101990697A (en) * 2008-04-10 2011-03-23 信越化学工业株式会社 Method for manufacturing bonded substrate
CN105197880A (en) * 2014-06-24 2015-12-30 中芯国际集成电路制造(上海)有限公司 Bonding method of wafers with cavities
CN105016632A (en) * 2015-06-12 2015-11-04 哈尔滨工业大学深圳研究生院 Method of cryogenic surface activation direct bonding for preparation of quartz glass capillary tube
CN105161437A (en) * 2015-09-18 2015-12-16 北京工业大学 Plasma-assisted glass or quartz chip microstructure alignment and pre-bonding method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109081595A (en) * 2018-09-30 2018-12-25 江苏耀兴安全玻璃有限公司 A kind of preparation method of devitrified glass
CN110473778A (en) * 2019-08-17 2019-11-19 哈尔滨工业大学 A method of utilizing plasma-activated Direct Bonding zirconium oxide and aluminum oxide
CN110473778B (en) * 2019-08-17 2021-10-15 哈尔滨工业大学 Method for directly bonding zirconium oxide and aluminum oxide by using plasma activation

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