CN110791746A - Method and device for rapidly filling vertical silicon through hole with liquid alloy - Google Patents

Method and device for rapidly filling vertical silicon through hole with liquid alloy Download PDF

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CN110791746A
CN110791746A CN201911086230.3A CN201911086230A CN110791746A CN 110791746 A CN110791746 A CN 110791746A CN 201911086230 A CN201911086230 A CN 201911086230A CN 110791746 A CN110791746 A CN 110791746A
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filling
alloy
reaction chamber
tsv
silicon
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CN110791746B (en
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马立民
冯剑雨
王乙舒
郭福
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Beijing University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • C23C16/402—Silicon dioxide
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/12—Semiconductors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
    • H01L21/76802—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing by forming openings in dielectrics
    • H01L21/76814—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing by forming openings in dielectrics post-treatment or after-treatment, e.g. cleaning or removal of oxides on underlying conductors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H01L21/76898—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics formed through a semiconductor substrate

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Abstract

A method and a device for rapidly filling a vertical silicon through hole with liquid alloy relate to the field of microelectronic packaging. The filling material is solder alloy, a silicon dioxide insulating layer is deposited on the surface of the TSV silicon chip and in the blind hole in a chemical vapor mode in advance, a titanium blocking layer is deposited on the hole wall through the physical vapor phase, a copper layer is plated on the surface of the silicon chip on which the silicon dioxide is deposited to serve as a wetting layer, the obtained silicon chip is placed in a vacuum chamber, the alloy is heated and melted, due to the wettability between the solder alloy and the copper, the alloy is pressed when being completely contacted with the silicon chip after being melted, the pressure in the vacuum chamber is kept after the pressing, and the filling is completed after the temperature is cooled. The invention can improve the filling efficiency of the Through Silicon Via (TSV) and complete the hole-free filling of the solder alloy for the TSV with the high aspect ratio. The alloy and the TSV hole wall are firmly combined, and the filling process is simple. The TSV rapid filling device comprises a vacuum outlet, a nitrogen inlet, and a valve control device for the outlet and the inlet. The device comprises a pressure gauge, a reaction chamber, a heating device and a temperature display device.

Description

Method and device for rapidly filling vertical silicon through hole with liquid alloy
Technical Field
The invention relates to the technical field of microelectronic packaging, in particular to a method and a device for quickly filling silicon through holes with alloy.
Background
Moore's law has led the development of electronic information technology since 1965, however, with the advent of smaller line width technology, it is becoming more and more difficult to integrate higher density circuits and implement more functions on a single chip, three-dimensional integrated packaging technology is considered as the first choice solution for realizing miniaturization and multi-functionalization of devices, and Through Silicon Via (TSV) technology is the core of three-dimensional integrated packaging technology, which can implement vertical up-and-down interconnection between stacked chips, and this structure can play a role in signal conduction and heat transfer, thereby completing three-dimensional integration.
The TSV is usually manufactured by etching a blind hole on a silicon wafer through a Bosch process, and then depositing a seed layer and a barrier layer on a hole wall, wherein the filling of the through hole is the most critical link in the TSV manufacturing process and has the highest cost, and the traditional filling method generally uses electroplated copper to fill the TSV blind hole. The pore size of TSVs is typically a few microns to tens of microns, and can reach depths of tens to hundreds of microns. Due to its high aspect ratio structure, the copper electroplating process generally requires several to tens of hours, the filling efficiency is low, and the electrolyte and additives are toxic and also pollute the environment.
A novel filling method is urgently needed to solve the problem, at present, most of the problems are that the electroplating process parameters are changed to reduce defects in the filling process, but the problems of long time consumption and high production cost are still not solved. Therefore, it is necessary to develop a new filling method that is faster and cheaper, and improves the production efficiency.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method and a device for quickly filling TSV by using solder alloy, and aims to improve the TSV filling speed and the production efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for rapidly filling TSV by using liquid alloy is characterized by comprising the following steps:
(1) marking an etching area on the surface of a silicon wafer by using photoresist, and forming a blind hole by ion etching;
(2) depositing a silicon dioxide insulating layer on the wall of the blind hole of the silicon chip obtained in the step (1) and the surface of the silicon chip by using chemical vapor deposition, and depositing a titanium barrier layer on the surface of the silicon dioxide on the wall of the blind hole by using physical vapor deposition; chemically plating a layer of copper on the surface of the silicon dioxide layer on the surface of the silicon chip as a wetting layer;
(3) putting the silicon chip obtained in the step (2) into HNO3Cleaning in the solution, taking out the acid-washed silicon wafer, and then putting the silicon wafer in absolute ethyl alcohol for ultrasonic cleaning to remove surface pollutants and impurities;
(4) placing the silicon wafer cleaned in the step (3) in a ventilation place for airing;
(5) placing the dried silicon chip and the alloy block required for filling into a filling groove, placing the filling groove into a filling device, at the moment, a vacuum outlet of the filling device and a nitrogen inlet valve are both in a closed state, the reaction chamber is sealed, the vacuum outlet and the nitrogen inlet valve are opened, the vacuum pump is opened, the reaction chamber and a nitrogen transmission pipeline are in a vacuum state at the moment, the vacuum pump and the valves are closed, the reaction chamber is in a sealed state, the vacuum state of the reaction chamber is confirmed, the heating device is opened at the moment to heat the temperature of the reaction chamber to be above an alloy melting point, the alloy is spread on the surface of the silicon wafer after melting, the nitrogen inlet valve is opened, the valve at the nitrogen inlet is closed after nitrogen is input, the gas pressure in the reaction chamber is kept to be 0.2-0.5 MPa to overcome surface tension, the filling of the TSV is completed at the moment, the.
The silicon chip in the step (2) is a silicon chip with blind holes, the surface of the silicon chip is plated with copper, and due to the wettability between the solder alloy and the copper, the molten alloy can spread on the surface of the silicon chip;
the hole wall is deposited with a silicon dioxide insulating layer and a titanium barrier layer, and does not include a copper seed layer.
The scheme of the invention has the following beneficial effects:
(1) the pretreatment acid washing and the ultrasonic cleaning can remove oxides and impurities on the surface of the TSV hole wall due to long-time placement, so that filling is easier to perform and is not affected by the impurities, copper is plated on the surface of the silicon chip, and the wettability between the solder alloy and the silicon chip is improved.
(2) The vacuum pumping treatment is carried out before the filling, the compression of air in a blind hole area by extruding solder alloy in the filling process is avoided, and therefore the damage of a silicon wafer is avoided, the filling of the molten alloy is completed under the pressure of nitrogen, the physical process is substantial, the filling process is rapid, the waiting time is the process of heating to a melting point and cooling to room temperature, the filling process is 1-2 hours, the filling process is simple, and compared with the process that Cu electroplating consumes hours or even more than ten hours, the production efficiency is greatly improved, the cost is reduced, and the environment pollution caused by the Cu electroplating process is avoided.
(3) The sample adopting the filling method does not need to deposit a copper seed layer on the hole wall, thereby further saving the cost.
(4) The filling method can realize the non-hole filling of the blind hole TSV under sufficient pressure.
Drawings
FIG. 1 is a schematic diagram of a process for filling TSVs with an alloy according to the present invention;
FIG. 2 is a view showing the structure of a sample;
FIG. 3 is a schematic structural diagram of the alloy rapid filling device of the present invention;
FIG. 4 Electron micrograph of silicon wafer filled with alloy of example 2
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific examples.
A method for rapidly filling TSV by using liquid alloy comprises the following steps:
1) pretreatment of
Marking an etching area on the surface of a silicon wafer by using photoresist, and forming a blind hole by deep reactive ion etching; and then depositing a silicon dioxide insulating layer on the wall of the blind hole of the silicon wafer and the surface of the silicon wafer by using chemical vapor deposition, and depositing a titanium barrier layer on the surface of the silicon dioxide on the wall of the blind hole by using physical vapor deposition. Chemically plating a layer of copper on the surface of the silicon dioxide layer on the surface of the silicon chip as a wetting layer;
2) filler alloy
Drying the cleaned silicon wafer, placing the silicon wafer and alloy blocks required by filling into a filling groove, placing the filling groove into a filling device, sealing a reaction chamber with a vacuum outlet and a nitrogen inlet valve both in a closed state, opening the vacuum outlet and the nitrogen inlet valve, opening a vacuum pump, keeping the reaction chamber and a nitrogen transmission pipeline in a vacuum state, closing the vacuum pump and the valves, keeping the reaction chamber in a sealed state, observing the reading of a pressure gauge, confirming the vacuum state of the reaction chamber after a period of time, opening a heating device to heat the reaction chamber to a temperature higher than the melting point of the alloy, spreading the alloy on the surface of the silicon wafer after the alloy is melted due to the wettability of the solder alloy and the copper on the surface of the silicon wafer, opening the nitrogen inlet valve, closing the valve at the nitrogen inlet after inputting the nitrogen, keeping the gas pressure in the reaction chamber, and finishing the filling of the TSV, and (4) closing the heating device, and taking out the sample after the temperature is cooled to the room temperature.
Preferably, no copper seed layer is deposited on the silicon wafer via walls in step 1).
Preferably, the silicon wafer in the step 1) is a silicon wafer containing blind holes, and before filling the sample, the surface of the silicon wafer is plated with a layer of copper.
Preferably, the pre-vacuuming treatment in step 2) can avoid the reaction force generated by the gas inside the blind hole during the filling process.
Preferably, the reaction chamber and the valves are sealed in the step 2), and the pressure of the nitrogen transmission pipeline is required to meet the requirement of nitrogen pressure, and is generally 5 MPa.
Preferably, the range of the pressure gauge in the step 2) is-0.1 MPa to 4 MPa.
Preferably, the heating device in the step 2) has a range above the melting point of the alloy.
The invention also provides a rapid filling device which comprises a sealed reaction chamber, a vacuum pump, a nitrogen input device, a vacuum outlet control valve, a nitrogen inlet control valve, a filling groove, a heating device and a temperature sensor.
Example 1
The rapid filling device for alloy filled TSV provided by the invention comprises a sealed reaction chamber, a vacuum pump, a nitrogen input device, a vacuum outlet control valve, a nitrogen inlet control valve, a filling groove, a heating device and a temperature sensor, wherein the vacuum chamber is shown in figure 3.
Example 2
The TSV rapid filling method provided by the embodiment comprises the following steps:
the first step is as follows: the sample selected in the example is a TSV (through silicon Via) blind hole silicon wafer with the diameter of 10 microns, the depth of 100 microns and the aspect ratio of 10 and copper plated on the surface, the silicon wafer is cut into small pieces with the diameter of 5mm x 5mm by utilizing laser, and the cut small pieces are placed in 20% HNO (hydrogen sulfide organic oxide)3Soaking in the solution for 20s, taking out with tweezers, placing into a beaker containing anhydrous ethanol, and cleaning with ultrasonic cleaner for 10 min.
The second step is that: polishing Sn3.0Ag0.5Cu solder alloy with sand paper, removing surface oxidation film, ultrasonic cleaning in a beaker filled with absolute ethyl alcohol to remove surface impurities, and air drying
The third step: and (3) placing the sample tank containing the solder alloy and the sample in a reaction chamber of the filling device, sealing the reaction chamber, and closing valves at a vacuum outlet and a nitrogen inlet.
The fourth step: vacuumizing and checking air tightness, opening a valve at a vacuum outlet, opening a switch of a vacuum pump, observing the reading of a pressure gauge, closing the vacuum pump and the valve at the vacuum outlet, observing the reading of the pressure gauge again after a period of time, and if the reading is unchanged, ensuring that the air tightness is good.
The fifth step: melting the solder alloy: the reaction chamber is heated by a heating device to a temperature above the melting point of the solder alloy, which in this example is 217 ℃ so the heating temperature is 250 ℃.
And a sixth step: applying nitrogen pressure: and fifthly, opening a valve at a nitrogen inlet when the solder alloy in the step five is in a molten state, applying 0.5MPa of nitrogen pressure, and closing the valve, wherein the reading of a pressure gauge is 0.5 MPa.
The seventh step: solidifying the solder alloy: and closing the heating device, cooling the reaction chamber to room temperature in air, opening the reaction chamber, and taking out the TSV sample.

Claims (4)

1. A method for rapidly filling TSV by using liquid alloy is characterized by comprising the following steps:
(1) marking an etching area on the surface of a silicon wafer by using photoresist, and forming a blind hole by ion etching;
(2) depositing a silicon dioxide insulating layer on the wall of the blind hole of the silicon chip obtained in the step (1) and the surface of the silicon chip by using chemical vapor deposition, and depositing a titanium barrier layer on the surface of the silicon dioxide on the wall of the blind hole by using physical vapor deposition; chemically plating a layer of copper on the surface of the silicon dioxide layer on the surface of the silicon chip as a wetting layer;
(3) putting the silicon chip obtained in the step (2) into HNO3Cleaning in the solution, taking out the acid-washed silicon wafer, and then putting the silicon wafer in absolute ethyl alcohol for ultrasonic cleaning to remove surface pollutants and impurities;
(4) placing the silicon wafer cleaned in the step (3) in a ventilation place for airing;
(5) placing the dried silicon chip and the alloy block required for filling into a filling groove, placing the filling groove into a filling device, at the moment, a vacuum outlet of the filling device and a nitrogen inlet valve are both in a closed state, the reaction chamber is sealed, the vacuum outlet and the nitrogen inlet valve are opened, the vacuum pump is opened, the reaction chamber and a nitrogen transmission pipeline are in a vacuum state at the moment, the vacuum pump and the valves are closed, the reaction chamber is in a sealed state, the vacuum state of the reaction chamber is confirmed, the heating device is opened at the moment to heat the temperature of the reaction chamber to be above an alloy melting point, the alloy is spread on the surface of the silicon wafer after melting, the nitrogen inlet valve is opened, the valve at the nitrogen inlet is closed after nitrogen is input, the gas pressure in the reaction chamber is kept to be 0.2-0.5 MPa to overcome surface tension, the filling of the TSV is completed at the moment, the.
2. The method for rapidly filling TSVs according to claim 1, wherein the reaction chamber, the valve and the nitrogen transmission pipeline in the step (5) are sealed, and the pressure resistance of the nitrogen transmission pipeline is required to meet the requirement of the nitrogen pressure, and is required to be 5 MPa.
3. The method for rapidly filling TSVs according to claim 1, wherein the range of the pressure gauge in the step (5) is-0.1 MPa to 2 MPa.
4. The TSV rapid filling device is characterized by comprising a sealed reaction chamber, a vacuum pump, a nitrogen input device, a vacuum outlet control valve, a nitrogen inlet control valve, a filling groove, a heating device and a temperature sensor.
CN201911086230.3A 2019-11-08 2019-11-08 Method and device for rapidly filling vertical silicon through hole with liquid alloy Active CN110791746B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112331613A (en) * 2020-11-25 2021-02-05 哈尔滨工业大学 Method for rapidly filling liquid metal to TSV (through silicon Via) based on ultrasonic-pressure composite process
WO2023109327A1 (en) * 2021-12-17 2023-06-22 腾讯科技（深圳）有限公司 Silicon wafer and method for filling silicon hole therein

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CN103681390A (en) * 2013-12-20 2014-03-26 中国电子科技集团公司第五十八研究所 TSV (Through Silicon Via) technology based preparation method for wafer level silicon substrate
US9455188B2 (en) * 2013-01-18 2016-09-27 Globalfoundries Inc. Through silicon via device having low stress, thin film gaps and methods for forming the same
CN108109955A (en) * 2017-12-13 2018-06-01 华中科技大学 A kind of composite material and its fill method for being used to fill vertical silicon hole TSV
CN109037145A (en) * 2018-07-11 2018-12-18 宁波芯健半导体有限公司 A kind of TSV through hole and its sputtering technology
CN109166818A (en) * 2018-07-27 2019-01-08 北京工业大学 A method of for molten solder filling silicon through holes
CN109273403A (en) * 2018-09-27 2019-01-25 中国电子科技集团公司第五十四研究所 A kind of TSV filling perforation method
CN109628968A (en) * 2019-01-30 2019-04-16 中南大学 A kind of TSV method for quickly filling and device

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9455188B2 (en) * 2013-01-18 2016-09-27 Globalfoundries Inc. Through silicon via device having low stress, thin film gaps and methods for forming the same
CN103681390A (en) * 2013-12-20 2014-03-26 中国电子科技集团公司第五十八研究所 TSV (Through Silicon Via) technology based preparation method for wafer level silicon substrate
CN108109955A (en) * 2017-12-13 2018-06-01 华中科技大学 A kind of composite material and its fill method for being used to fill vertical silicon hole TSV
CN109037145A (en) * 2018-07-11 2018-12-18 宁波芯健半导体有限公司 A kind of TSV through hole and its sputtering technology
CN109166818A (en) * 2018-07-27 2019-01-08 北京工业大学 A method of for molten solder filling silicon through holes
CN109273403A (en) * 2018-09-27 2019-01-25 中国电子科技集团公司第五十四研究所 A kind of TSV filling perforation method
CN109628968A (en) * 2019-01-30 2019-04-16 中南大学 A kind of TSV method for quickly filling and device

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112331613A (en) * 2020-11-25 2021-02-05 哈尔滨工业大学 Method for rapidly filling liquid metal to TSV (through silicon Via) based on ultrasonic-pressure composite process
CN112331613B (en) * 2020-11-25 2023-03-14 哈尔滨工业大学 Method for rapidly filling liquid metal to TSV (through silicon Via) based on ultrasonic-pressure composite process
WO2023109327A1 (en) * 2021-12-17 2023-06-22 腾讯科技（深圳）有限公司 Silicon wafer and method for filling silicon hole therein

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