CN114920469A - Bonding method of borosilicate glass - Google Patents
Bonding method of borosilicate glass Download PDFInfo
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- CN114920469A CN114920469A CN202210618131.0A CN202210618131A CN114920469A CN 114920469 A CN114920469 A CN 114920469A CN 202210618131 A CN202210618131 A CN 202210618131A CN 114920469 A CN114920469 A CN 114920469A
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- substrate
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- bonding method
- glass substrate
- borosilicate glass
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000005388 borosilicate glass Substances 0.000 title claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000003213 activating effect Effects 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 239000011521 glass Substances 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 11
- 230000003287 optical effect Effects 0.000 claims description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000003517 fume Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 2
- 229910008051 Si-OH Inorganic materials 0.000 claims 1
- 229910006358 Si—OH Inorganic materials 0.000 claims 1
- 239000002390 adhesive tape Substances 0.000 claims 1
- 239000003344 environmental pollutant Substances 0.000 claims 1
- 231100000719 pollutant Toxicity 0.000 claims 1
- 238000002525 ultrasonication Methods 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 6
- 241000252506 Characiformes Species 0.000 abstract description 3
- 229910021529 ammonia Inorganic materials 0.000 abstract description 3
- 238000000861 blow drying Methods 0.000 abstract 1
- 238000001994 activation Methods 0.000 description 12
- 230000004913 activation Effects 0.000 description 11
- 239000000126 substance Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910002656 O–Si–O Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000000678 plasma activation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- 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
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The invention provides a bonding method of borosilicate glass, which comprises the following steps: (1) cleaning the polished borosilicate glass substrate with a smooth surface by using pure water and ethanol respectively, removing dirt (2), ultrasonically cleaning the borosilicate glass substrate in piranha solution, cleaning the borosilicate glass substrate again by using the pure water and the ethanol, blow-drying the borosilicate glass substrate by using a nitrogen gun (3), dropwise adding ammonia activating solution on a bonding surface, bonding the borosilicate glass substrate, standing the bonded substrate in an environment with the humidity of 70-90% for 2 hours, separating the bonded substrate, dropwise adding the ammonia activating solution again, and bonding the bonded substrate again for later use. (4) And (3) putting the substrate after being attached and standing into a vacuum drying box, firstly preserving heat for 1h at 100 ℃, and then continuously preserving heat for 4h at 200 ℃. (5) And naturally cooling to room temperature along with the furnace, and finishing bonding. The bonding method does not need to be carried out in a high-cleanness environment, has low requirements on equipment and environment, and is low in cost and convenient to operate.
Description
Technical Field
The invention relates to a bonding method of borosilicate glass, belonging to the technical field of device bonding.
Background
Borosilicate glass is defined by SiO 2 ,B 2 O 3 ，Al 2 O 3 ,Na 2 O is a glass which substantially constitutes the component. Borosilicate glass has an extremely low coefficient of thermal expansion (one third of that of ordinary glass), is not easy to crack and deform at high temperature, and is widely applied to devices such as cinema projectors, inspection window covers of chemical reactors, high-efficiency lamps and the like which need to work under high-temperature conditions or in environments with severe temperature changes. In addition, borosilicate glass also has the advantages of small shape deviation, high visible light transmittance, low dispersion, relatively low refractive index and the like, and is widely applied to optical devices such as telescopes, reflectors and the like.
The key and the technology have wide application, and can be used for manufacturing chip structures in electronic products, various semiconductor materials and structural devices, and even more complex three-dimensional structure chips. The bonding technique is also widely used in the field of optical device manufacturing, and the quality of glass bonding directly affects the final performance of an optical component, and is very important in the whole process flow.
At present, the bonding methods of the glass mainly comprise the following steps:
(1) conventional thermal bonding: the bonding is carried out by heating at high temperature (typically greater than 800 ℃), and the most important drawback of this bonding method is that the higher temperature causes some deformation of the glass substrate during bonding. For optical devices with higher precision, the deformation of the substrate can cause the optical precision to be seriously reduced, and the performance of the device is influenced;
(2) intermediate medium bonding: and placing the low-melting-point glass frit on a bonding interface, heating to the softening temperature of the glass frit, and bonding the glass frit through the glass frit. This method generally has the problem that the bonding frit used is not consistent with the refractive index and thermal expansion coefficient of the glass to be bonded, resulting in a reduction in the optical accuracy of the assembly;
(3) anodic bonding: and applying pressure and voltage to two ends of the bonding glass to enable Na ions in the glass to drift towards the negative electrode direction to form a depletion layer to form an O-Si-O bond so as to realize bonding. This method has a disadvantage of limited diffusion ability of Na ions, and when the glass substrate to be bonded is too thick, Na ions are not sufficiently diffused, resulting in poor bonding effect.
The bonding method mostly needs to be activated through plasma surface modification, and the temperature required by bonding is high, so that the preparation process is complicated to operate, the technology is not easy to master, and the large-scale industrial production of the material is influenced to a certain extent. The bonding technology generally comprises four steps of substrate cleaning, surface modification and activation, pre-bonding and bonding. The activation method can be broadly classified into plasma activation, ultraviolet light activation, and chemical solution activation. In this case, the chemical solution activation does not require any special instrument or equipment, and only requires the use of a chemical solution, so that the method has the advantages of low cost and simple operation compared with other activation methods. The traditional chemical solution activation method needs heating and boiling activation liquid to activate the substrate when activating the substrate, so that the reaction is severe and the risk is high. There is still room for further improvement and simplification of chemical solution activated bonding processes.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and provide a borosilicate glass bonding method which can be completed in a common laboratory. The bonding method adopts a chemical solution ultrasonic cleaning method to carry out the activation treatment of the substrate, does not need special treatment equipment, has lower cost, does not need to boil the activation solution in the activation process, is safe and reliable, and is easy to operate. The bonding technology has high bonding success rate, the strength can meet the preparation requirement of a common optical component, and the performance of the optical component obtained by bonding is excellent.
The borosilicate glass bonding method comprises the following specific steps:
1. the glass surface was polished using an optical polishing instrument and then ultrasonically cleaned in pure water, ethanol and acetone for 5 min.
2. Placing the glass substrate in a fume hood, placing the glass substrate in a washing liquid of a mixed solution of 98% concentrated sulfuric acid and 30% hydrogen peroxide in a volume ratio of 7:3, ultrasonically cleaning for 5min, then ultrasonically cleaning for 3min by sequentially using pure water and ethanol, taking out, and drying by using a nitrogen gun for later use.
3. Suction with syringe (NH) 4 )OH:H 2 O 2 :H 2 And (3) dropwise adding ammonia water activating solution with the volume ratio of 0: 2:2 on the surface to be bonded of one substrate, then attaching the surface to be bonded of the other substrate, and standing for 2 hours in an environment with the humidity of 70% -90%. Then the substrates are separated, ammonia activating solution is repeatedly dripped to attach again, and then standing is carried out for standby.
4. And (3) putting the attached substrate into a vacuum drying box, vacuumizing to 100Mbar-200Mbar, heating to 100 ℃ at the speed of 2-3 ℃/min, and preserving heat for 2 hours, and then heating to 200 ℃ at the same heating speed, and preserving heat for 4 hours. And then naturally cooling to room temperature along with the furnace, and finishing bonding.
The mechanism and the beneficial effects of the invention are as follows:
the invention has the advantages of simple equipment, low cost, no need of surface modification by plasma or ultraviolet light, and no need of high cleanliness environment. The method has the advantages that the activating solution does not need to be boiled during the substrate activating treatment, and compared with the traditional chemical activation, the method is safer and is more convenient to operate. The bonded glass substrate is not easy to generate bubbles, the glass substrate is not deformed in the bonding process, and the bonded glass assembly has good light transmission. The formation of Si-O-Si bonding after annealing enables the glass substrate to have larger bonding force under the condition that the surface micro-nano structure is not damaged. The whole bonding process is simple to operate, the technology is easy to master, and the method is suitable for large-batch industrial production. ,
drawings
FIG. 1 is a flow chart of the bonding of borosilicate glass according to the present invention.
Detailed Description
The present invention provides a method for bonding borosilicate glass, and in order to make the objects and advantages of the present invention more clear, the present invention will be further described with reference to examples.
Example 1
And (3) putting the two polished borosilicate glasses into a beaker filled with pure water, ultrasonically cleaning for 5min, pouring absolute ethyl alcohol after pouring out the pure water, ultrasonically cleaning for 5min again, adding acetone after pouring out the ethyl alcohol, ultrasonically cleaning for 5min, and taking out the two polished borosilicate glasses.
And putting the cleaned glass substrate into a mixed solution (piranha solution, commonly called piranha solution) of 98% concentrated sulfuric acid and 30% hydrogen peroxide in a volume ratio of 7:3, and ultrasonically cleaning for 5min under the power of 50W. And then pouring out the mixed solution, adding a large amount of pure water for ultrasonic cleaning for 3min, pouring out the pure water, adding a large amount of ethanol for ultrasonic cleaning for 3min, taking out, and drying by using a nitrogen gun.
Placing a substrate to be bonded with the bonding surface facing upwards, sucking 10mL of activating solution of 25-28% concentrated ammonia water, 30% hydrogen peroxide and pure water in a volume ratio of 6:2:2 by using a needle cylinder, and slowly and uniformly dripping the activating solution on the whole bonding surface. And (3) placing the surface to be bonded of the other substrate into a constant humidity box with the humidity set to be 75% for standing for 2 hours after the surface to be bonded of the other substrate is attached. And then taking out the substrate, separating the substrate, dripping the activating solution again, laminating again and putting the substrate back into the constant humidity box.
Taking the substrate out of the constant humidity box, putting the substrate into a vacuum drying box, vacuumizing to 1500Mbar, starting heating after setting the heating rate to be 2 ℃/min, keeping the temperature for 2h after heating to 100 ℃, then continuing to heat to 200 ℃ at the rate of 2 ℃/min, and keeping the temperature for 4 h. And naturally cooling to room temperature, and taking out the bonded substrate. The bonded substrate has good light transmittance and high bonding strength.
Claims (7)
1. A bonding method of borosilicate glass is characterized by comprising the following steps:
step 1, polishing a glass sample by using an optical polishing instrument, and respectively cleaning by using pure water, ethanol and acetone to obtain a cleaned glass substrate;
2, putting the glass substrate into a mixed solution of 98% concentrated sulfuric acid and 30% hydrogen peroxide in a volume ratio of 7:3 in a fume hood for ultrasonic cleaning, putting the substrate cleaned in the step 1 into a middle ultrasonic processing unit for a period of time, further removing pollutants on the surface of the glass substrate, simultaneously generating Si-OH bonds to make the surface hydrophilic, ultrasonically cleaning the glass substrate again by using pure water and ethanol for a period of time, and then drying the glass substrate by using a nitrogen gun for standby;
step 3, according to the volume ratio of NH 4 OH:H 2 O 2 :H 2 Preparing ammonia water activating solution according to the proportion of O6: 2:2, dropwise adding the ammonia water activating solution on the surface of one substrate to be bonded by using a needle cylinder, attaching the other substrate to the ammonia water activating solution, standing for a period of time in a wet environment with the humidity of 70-90%, repeating the step, and continuously standing for later use;
step 4, separating the substrates after standing, repeating the step 3, dropwise adding the ammonia water activating solution, and continuing standing for 2 hours;
step 5, putting the substrate into a vacuum drying box, heating to 100 ℃ for heat preservation for a period of time, and then continuously heating to 200 ℃ for heat preservation for a period of time;
and 6, cooling to room temperature along with the furnace, and finishing bonding.
2. The bonding method according to claim 1, characterized in that:
in the step 1, the ultrasonic power of the ultrasonic cleaning is 40-60W, and the cleaning time is 5 min.
3. The bonding method according to claim 1, characterized in that:
in step 2, the ultrasonication is carried out for more than 5 min.
4. The bonding method according to claim 1, wherein:
in step 2, the ultrasonic cleaning is carried out for more than 3min by using pure water and ethanol again.
5. The bonding method according to claim 1, characterized in that:
in step 2, the other piece is attached to the adhesive tape and then is kept stand for more than 2 hours in a humid environment with the humidity of 70% -90%.
6. The bonding method according to any one of claims 1 to 5, wherein:
in step 5, the substrate is put into a vacuum oven with the vacuum degree of 100Mbar-200Mbar, the temperature is raised to 100 ℃ at the speed of 2-3 ℃/min, and then the temperature is preserved for more than 2 h.
7. The bonding method according to claim 6, wherein the temperature is further raised to 200 ℃ at the same rate and then maintained for 4 hours or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210618131.0A CN114920469B (en) | 2022-06-01 | Bonding method of borosilicate glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210618131.0A CN114920469B (en) | 2022-06-01 | Bonding method of borosilicate glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114920469A true CN114920469A (en) | 2022-08-19 |
| CN114920469B CN114920469B (en) | 2024-04-30 |
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Citations (7)
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|---|---|---|---|---|
| US20030079823A1 (en) * | 2001-10-26 | 2003-05-01 | Robert Sabia | Direct bonding of articles containing silicon |
| US20030211705A1 (en) * | 2000-02-16 | 2003-11-13 | Ziptronix, Inc. | Method for low temperature bonding and bonded structure |
| CN101050066A (en) * | 2007-05-11 | 2007-10-10 | 华中科技大学 | Method for local bonding silicon / glass by laser |
| US20140170378A1 (en) * | 2012-12-13 | 2014-06-19 | Corning Incorporated | Glass articles and methods for controlled bonding of glass sheets with carriers |
| CN109721257A (en) * | 2018-08-02 | 2019-05-07 | 比亚迪股份有限公司 | Glass composite, shell, display device and terminal device |
| CN112851145A (en) * | 2019-11-28 | 2021-05-28 | 中国科学院大连化学物理研究所 | Chemical activation based low-temperature direct bonding method for quartz glass |
| CN112897899A (en) * | 2021-01-21 | 2021-06-04 | 中国科学院电工研究所 | Glass assembly bonding method |
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030211705A1 (en) * | 2000-02-16 | 2003-11-13 | Ziptronix, Inc. | Method for low temperature bonding and bonded structure |
| US20030079823A1 (en) * | 2001-10-26 | 2003-05-01 | Robert Sabia | Direct bonding of articles containing silicon |
| CN101050066A (en) * | 2007-05-11 | 2007-10-10 | 华中科技大学 | Method for local bonding silicon / glass by laser |
| US20140170378A1 (en) * | 2012-12-13 | 2014-06-19 | Corning Incorporated | Glass articles and methods for controlled bonding of glass sheets with carriers |
| CN109721257A (en) * | 2018-08-02 | 2019-05-07 | 比亚迪股份有限公司 | Glass composite, shell, display device and terminal device |
| CN112851145A (en) * | 2019-11-28 | 2021-05-28 | 中国科学院大连化学物理研究所 | Chemical activation based low-temperature direct bonding method for quartz glass |
| CN112897899A (en) * | 2021-01-21 | 2021-06-04 | 中国科学院电工研究所 | Glass assembly bonding method |
Non-Patent Citations (1)
| Title |
|---|
| 张克立等: "无机合成化学 第2版", 武汉大学出版社, pages: 49 * |
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