CN113072037A - Method for improving BCB bonding of glass substrate through surface plasma activation - Google Patents
Method for improving BCB bonding of glass substrate through surface plasma activation Download PDFInfo
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- CN113072037A CN113072037A CN202110324614.5A CN202110324614A CN113072037A CN 113072037 A CN113072037 A CN 113072037A CN 202110324614 A CN202110324614 A CN 202110324614A CN 113072037 A CN113072037 A CN 113072037A
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000000758 substrate Substances 0.000 title claims abstract description 44
- 239000011521 glass Substances 0.000 title claims abstract description 42
- 238000000678 plasma activation Methods 0.000 title claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000003292 glue Substances 0.000 claims description 14
- 238000004528 spin coating Methods 0.000 claims description 14
- 238000001994 activation Methods 0.000 claims description 13
- 230000004913 activation Effects 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000009987 spinning Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 10
- 239000000853 adhesive Substances 0.000 abstract description 7
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- 238000004806 packaging method and process Methods 0.000 abstract description 5
- 238000009832 plasma treatment Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000003749 cleanliness Effects 0.000 abstract description 3
- UMIVXZPTRXBADB-UHFFFAOYSA-N benzocyclobutene Chemical compound C1=CC=C2CCC2=C1 UMIVXZPTRXBADB-UHFFFAOYSA-N 0.000 description 35
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 238000012876 topography Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000005098 blood-cerebrospinal fluid barrier Anatomy 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 210000003934 vacuole Anatomy 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C3/00—Assembling of devices or systems from individually processed components
- B81C3/001—Bonding of two components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2203/00—Forming microstructural systems
- B81C2203/03—Bonding two components
- B81C2203/033—Thermal bonding
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Joining Of Glass To Other Materials (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
Abstract
The invention provides a method for improving BCB bonding of a glass substrate based on surface plasma activation, and belongs to the technical field of three-dimensional integrated packaging preparation. The method increases the surface activity of the dried BCB adhesive by performing low-temperature argon plasma activation treatment on the surface of the dried BCB adhesive, widens the upper limit of the conventional drying time, improves the activity and the surface cleanliness of the surface BCB, greatly improves the bonding effective area compared with the bonding effective area before surface plasma treatment, and reduces the probability of failure after bonding.
Description
Technical Field
The invention belongs to the technical field of three-dimensional integrated packaging preparation, and particularly relates to a method for improving BCB bonding of a glass substrate based on surface plasma activation.
Background
Three-dimensional integration technology is one of the most promising ways to continue moore's law, in which bonding technology plays an important role in the performance of the final product in a three-dimensional integration scheme as an indispensable means for three-dimensional substrate connection. The bonding medium can be made of metal conductive materials, and electric interconnection is realized through interlayer lead bonding; insulating materials such as organic polymers can also be used to realize the independence of signals between layers, and complete system functions can be formed between the substrates by means of coupling capacitance.
The glass has excellent insulating property, extremely low loss of microwave and millimeter wave frequency bands and thermal expansion coefficient close to that of silicon. With the improvement of glass processing technology, silicon is gradually being replaced as an ideal material for three-dimensional integrated packaging schemes in the field of microwave applications. Benzocyclobutene (BCB) is widely used in MEMS device packaging as a common organic bonding agent, and the BCB glue bonding has the following advantages: the bonding can be realized at a lower curing temperature (200-300 ℃), and compared with other bonding modes, the bonding method has low requirements on surface flatness and has fluidity before curing. The photosensitive BCB paste, which is introduced by the related commercial companies, makes it very suitable for wafer bonding with surface patterning.
However, in the process of using the BCB glue as a bonding medium, the BCB glue causes excessive volatilization of an organic solvent on a surface layer of the medium due to excessively thin thickness, excessively long drying time and the like after spin coating in the preparation process, and the surface fluidity is insufficient and the surface activity is reduced in the subsequent heating and curing step, so that the BCB bonding interface is not tight, and bonding failure occurs at the bonding interface if a small amount of aqueous pollutants is immersed after bonding; however, if the drying time is too short, a large amount of organic solvent is not discharged before heating and curing, and a large amount of bubbles are formed during curing, which also reduces the bonding strength.
Therefore, on the premise of not introducing other factors influencing the bonding effect, how to enhance the reactivity of the BCB at the bonding interface and reduce the influence (low fluidity and fine particle impurities) on the bonding interface, which is unfavorable for forming effective bonding, caused by the narrow parameter range of the drying process, becomes a research focus.
Disclosure of Invention
In view of the problems of the background art, the present invention is directed to a method for improving BCB bonding of a glass substrate based on surface plasma activation. According to the method, the surface activity of the dried BCB adhesive is increased by performing low-temperature plasma activation treatment on the surface of the dried BCB adhesive, and fine impurities on the surface, which influence BCB bonding, are removed, so that the bonding failure probability is reduced.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for improving BCB bonding of a glass substrate based on surface plasma activation comprises the following steps:
step 1, sequentially washing a glass substrate to be bonded by using deionized water, acetone and absolute ethyl alcohol;
step 2, preparing BCB glue on the surface of the glass substrate cleaned in the step 1 by adopting a spin coating method;
step 3, drying the glass substrate coated with the BCB glue in a spinning mode for 90-180 s at the temperature of 90-120 ℃;
and 4, carrying out gas plasma activation treatment on the glass substrate dried in the step 3, wherein the specific treatment process parameters are as follows: the gas flow is 30-50 sccm, the vacuum degree is 10-30 Pa, the radio frequency power is 50-180W, and the activation time is 120-200 s;
and 5, aligning the activated substrate, fixing and pressurizing by using a clamp, and then carrying out heating curing bonding in a nitrogen atmosphere.
Further, the acetone cleaning process in step 1 is as follows: placing the glass substrate in acetone, and carrying out hot bath for 10-20 min in a water bath heating mode; the process of washing with absolute ethanol is as follows: and (3) placing the glass substrate in absolute ethyl alcohol for ultrasonic treatment for 3-5 min.
Further, the technological parameters for preparing the BCB adhesive by spin coating in the step 2 are as follows: spin-coating at 1000rad/min for 10s, then spin-coating at 2000-5000 rad/min for 30s, and finally spin-coating at 1000rad/min for 10 s.
Further, the gas of the gas plasma in step 4 is preferably argon or nitrogen.
Further, the total time from the completion of the plasma activation to the transfer of the nitrogen atmosphere in the step 5 should not exceed 30min, the probability of the contact between the surface BCB molecules and air and the energy exchange is easily increased due to too long time in the transfer process, so that the activation effect is weakened, the BCB subjected to the surface plasma treatment has local static electricity, and the transfer process should be performed in a dust-free environment to avoid electrostatic adsorption of impurities in the air.
Further, in the step 5, applying pressure of 0.2-0.6 Mpa on the glass substrate to be bonded, then heating the glass substrate to 100-150 ℃ from room temperature within 30min, and preserving heat for 10-15 min; and then heating to the curing temperature of 200-275 ℃, preserving the heat for 30-60 min, reducing the curing temperature retention time along with the increase of the temperature, and then naturally cooling to the room temperature.
Furthermore, in the step 5, the purity of the nitrogen is more than 99.9 percent, and the gas flow rate is 5000 sccm-6000 sccm.
The mechanism of the invention is as follows: during the plasma activation treatment process, the ions in the plasma transmit energy to BCB molecules through collision, so that the BCB molecules on the surface are in a high energy state, the wettability and the reactivity of a contact surface are increased, good contact and reaction can be formed between the BCBs excessively dried in the conventional process, the parameter range of the drying step can be widened, part of the BCB molecules can be gasified, surface stains can be treated, the surface roughness is increased, the contact area in the bonding process is increased, and the bonding strength and the reliability are improved
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the method can improve the influence of the difference of the drying degree of the BCB glue on bonding, the internal organic solvent overflows to form vacuoles when the insufficiently dried BCB glue is heated, the organic solvent in the BCB glue with overlong drying time is excessively volatilized, the fluidity is poor, the glue interface is insufficiently fused, and bonding is easy to lose efficacy from the original interface.
2. The drying time of the BCB adhesive in the conventional technology is generally limited to 60-90 s, adverse factors can be introduced when the drying time is lower than or higher than the limited time, insufficient drying or over-drying of the BCB adhesive can be caused due to the difference of the thermal conductivity of the bonding material, the upper limit of the drying time is widened after the method is adopted, so that the organic solvent is removed for a long time during the preparation process as far as possible without causing the problem of activity reduction, the activity and the surface cleanliness of the surface BCB are improved, the bonding effective area is greatly increased compared with that before surface plasma treatment, and the probability of failure after bonding is reduced.
Drawings
Fig. 1 is a schematic diagram of a bonding product obtained by activating BCB bonding paste according to example 1 of the present invention.
Fig. 2 is a schematic diagram of a bonding product of comparative example 1 in which BCB bonding paste is activated.
FIG. 3 is a SEM cross-sectional view of a bonding product after activation of BCB bonding glue in example 1 of the present invention.
FIG. 4 is a graph of AFM surface topography prior to bonding of comparative example 1 to a BCB film of the present invention.
FIG. 5 is a graph of AFM surface topography before bonding to a BCB film in accordance with example 2 of the present invention.
FIG. 6 is a graph of AFM surface topography prior to bonding of comparative example 2 to a BCB film in accordance with the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following embodiments and accompanying drawings.
Example 1
A method for improving BCB bonding of a glass substrate based on surface plasma activation comprises the following steps:
step 1, washing a glass substrate with deionized water, then placing the glass substrate in an acetone solution, carrying out hot bath for 10min in a water bath heating mode, then taking out the glass substrate, washing residual acetone on the surface with the deionized water, carrying out ultrasonic treatment for 5min with absolute ethyl alcohol, and drying the absolute ethyl alcohol on the surface with high-pressure nitrogen;
and 2, fixing the glass substrate cleaned in the step 1 on a spin coater, dripping BCB solution on the surface of the glass by using a glass dropper, uniformly covering the surface of the whole glass substrate, and performing spin coating treatment, wherein the spin coating process parameters are as follows: spin-coating at 1000rad/min for 10s, then at 3000rad/min for 30s, and finally at 1000rad/min for 10 s;
step 3, placing the glass substrate coated with the BCB glue on a drying table, and drying at the temperature of 110 ℃ for 120 s;
and 4, putting the glass substrate dried in the step 3 into a plasma cleaning machine for plasma activation treatment, wherein the specific treatment process parameters are as follows: argon plasma is adopted, the gas flow is 50sccm, the vacuum degree is 30Pa, the radio frequency power is 150W, and the activation time is 120 s;
In the embodiment, when argon is used as plasma to activate the BCB surface, the argon does not participate in reaction to damage the structure, and meanwhile, no obvious residue exists; if the BCB surface is etched by using the mixed plasma of oxygen and argon, the method has long etching time and high power, other products are easily generated in the sputtering process, and the method is not suitable for surface activation.
The bonded product prepared in this example is shown in fig. 1, and the SEM cross-sectional view is shown in fig. 3.
Example 2
Bonding was performed according to the method of example 1, and only the rf power in the plasma activation treatment in step 4 was adjusted to 100W and the time was adjusted to 180s, while the other steps were unchanged.
The AFM surface observation before bonding of the BCB film prepared in this example is shown in fig. 5.
Comparative example 1
The bonding was carried out according to the method of example 1, except that the plasma activation treatment of step 4 was not carried out, and the remaining steps were not changed.
The bonding product prepared by the comparative example is shown in FIG. 2, and the AFM surface topography is shown in FIG. 4.
Comparative example 2
Bonding was performed according to the method of example 1, and only the rf power in the plasma activation treatment in step 4 was adjusted to 50W and the time to 60s, and the other steps were not changed.
The AFM surface observation before bonding of the BCB thin film prepared in this comparative example is shown in fig. 6.
In FIG. 1, the microscope has no obvious air bubbles at the focusing position and almost no black impurity particles; in fig. 2, bubbles of various sizes are formed due to delamination after curing of the BCB interface which is not in good contact and reacts during curing, and some black dots are impurities introduced before alignment. Comparing the two graphs, it can be seen that the surface bonding interface is uniform and complete, the surface cleanliness is higher and the bonding quality is high after the plasma treatment compared with the untreated sample.
FIG. 3 is a SEM cross-sectional view of a bonding product after activation of BCB bonding glue in example 1 of the present invention. As can be seen from the figure, the bonding interface after the activation treatment by the method of the invention is uniform and complete, no obvious boundary or bubble exists, the bonding quality is high, and the bonding result can well meet the bonding requirement of the three-dimensional integrated packaging glass substrate.
FIG. 5 is a photograph of the surface topography of the AFM taken after activation of the BCB bond paste and before bonding in example 2 of the present invention. As can be seen from the figure, the surface of the product has obvious hemispherical protrusions after being activated by the method of the invention, the surface appearance is obviously changed, and the surface activity is obviously improved compared with that in FIG. 6 of comparative example 2.
FIG. 6 is a photograph of the surface topography of the AFM taken after the BCB bond paste was activated and before bonding in this comparative example 2. FIG. 4 is an AFM surface topography of BCB glue without activation treatment of comparative example 1. As can be seen from a comparison of fig. 4 and 6, the improvement of the surface properties by plasma activation is not significant in the case of activation times not meeting the requirements of the method of the present invention. Thus, fig. 4, 5 and 6 comparatively illustrate that the selection of specific parameters for activation is important to ultimately achieve the desired BCB gum surface activity.
While the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.
Claims (7)
1. A method for improving BCB bonding of a glass substrate by surface plasma activation is characterized by comprising the following steps:
step 1, sequentially washing a glass substrate to be bonded by using deionized water, acetone and absolute ethyl alcohol;
step 2, preparing BCB glue on the surface of the glass substrate cleaned in the step 1 by adopting a spin coating method;
step 3, drying the glass substrate coated with the BCB glue in a spinning mode for 90-180 s at the temperature of 90-120 ℃;
and 4, carrying out gas plasma activation treatment on the glass substrate dried in the step 3, wherein the specific treatment process parameters are as follows: the gas flow is 30-50 sccm, the vacuum degree is 10-30 Pa, the radio frequency power is 50-180W, and the activation time is 120-200 s;
and 5, aligning the activated substrate, fixing and pressurizing by using a clamp, and then carrying out heating curing bonding in a nitrogen atmosphere.
2. The method for BCB bonding of glass substrates according to claim 1, wherein the acetone cleaning in step 1 is performed by: placing the glass substrate in acetone, and carrying out hot bath for 10-20 min in a water bath heating mode; the process of washing with absolute ethanol is as follows: and (3) placing the glass substrate in absolute ethyl alcohol for ultrasonic treatment for 3-5 min.
3. The method for BCB bonding of a glass substrate according to claim 1, wherein the process parameters for preparing the BC paste by spin coating in the step 2 are as follows: spin-coating at 1000rad/min for 10s, then spin-coating at 2000-5000 rad/min for 30s, and finally spin-coating at 1000rad/min for 10 s.
4. The method for BCB bonding of glass substrates according to claim 1, wherein the gas of the gas plasma in step 4 is argon or nitrogen.
5. The method for BCB bonding of glass substrates according to claim 1, wherein the total time from the completion of the plasma activation to the transfer of the nitrogen atmosphere in step 5 should not exceed 30min and the transfer should be performed in a dust-free environment.
6. The method for BCB bonding of glass substrates according to claim 1, wherein the specific process of step 5 is as follows: applying pressure of 0.2-0.6 Mpa on a glass substrate to be bonded, and then heating the glass substrate to 100-150 ℃ from room temperature within 30min, and keeping the temperature for 10-15 min; and then heating to the curing temperature of 200-275 ℃, preserving the heat for 30-60 min, and then naturally cooling to the room temperature.
7. The method for BCB bonding of glass substrates according to claim 1, wherein the purity of the nitrogen gas in step 5 is greater than 99.9% and the gas flow rate is 5000sccm to 6000 sccm.
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JPH09219586A (en) * | 1996-02-08 | 1997-08-19 | Toshiba Corp | Wiring substrate and its manufacturing method |
JP2002118168A (en) * | 2000-10-10 | 2002-04-19 | Murata Mfg Co Ltd | Thin film circuit board and its producing method |
JP2004014848A (en) * | 2002-06-07 | 2004-01-15 | Murata Mfg Co Ltd | Thin-film circuit board and its manufacturing method |
US20070072330A1 (en) * | 2003-03-05 | 2007-03-29 | Rensselaer Polytechnic Institute | Wafer bonding compatible with bulk micro-machining |
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JP2013243333A (en) * | 2012-04-24 | 2013-12-05 | Tadatomo Suga | Chip-on wafer bonding method and bonding device and structure including chip and wafer |
CN103474366A (en) * | 2013-09-13 | 2013-12-25 | 华进半导体封装先导技术研发中心有限公司 | Blended bonding achieving method |
CN108288582A (en) * | 2018-01-11 | 2018-07-17 | 北京华碳科技有限责任公司 | A kind of wafer scale GaN device substrate transfer method |
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2021
- 2021-03-26 CN CN202110324614.5A patent/CN113072037B/en active Active
Patent Citations (9)
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JPH09219586A (en) * | 1996-02-08 | 1997-08-19 | Toshiba Corp | Wiring substrate and its manufacturing method |
JP2002118168A (en) * | 2000-10-10 | 2002-04-19 | Murata Mfg Co Ltd | Thin film circuit board and its producing method |
US20020090831A1 (en) * | 2000-10-10 | 2002-07-11 | Murata Manufacturing Co., Ltd. | Thin-film circuit substrate and method of producing same |
JP2004014848A (en) * | 2002-06-07 | 2004-01-15 | Murata Mfg Co Ltd | Thin-film circuit board and its manufacturing method |
US20070072330A1 (en) * | 2003-03-05 | 2007-03-29 | Rensselaer Polytechnic Institute | Wafer bonding compatible with bulk micro-machining |
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CN103474366A (en) * | 2013-09-13 | 2013-12-25 | 华进半导体封装先导技术研发中心有限公司 | Blended bonding achieving method |
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