CN106591837A - Vertical carbon nanofiber array transferring method - Google Patents
Vertical carbon nanofiber array transferring method Download PDFInfo
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- CN106591837A CN106591837A CN201611065243.9A CN201611065243A CN106591837A CN 106591837 A CN106591837 A CN 106591837A CN 201611065243 A CN201611065243 A CN 201611065243A CN 106591837 A CN106591837 A CN 106591837A
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
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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
- C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
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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
- C23C16/26—Deposition of carbon only
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1273—Alkenes, alkynes
- D01F9/1275—Acetylene
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Carbon And Carbon Compounds (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a vertical carbon nanofiber array transferring method. The vertical carbon nanofiber array transferring method comprises the following steps: firstly, preparing a vertical carbon nanofiber array on a growth substrate by use of a chemical vapor deposition method; secondly, placing the vertical carbon nanofiber array obtained in the first step into ion sputtering equipment, and sequentially plating the surface of each fiber of the carbon nanofiber array with a Ti metal coating and an Au metal coating by use of an ion sputtering method; thirdly, placing the top end of the vertical carbon nanofiber array with the metal coatings, obtained in the second step, on the surface of a gold-plated bonding pad, and applying pressure and temperature to form Au-Au bonding, wherein the coating on the surface of the gold-plated bonding pad is an Au coating; and fourthly, lowering the temperature till the growth substrate and the bonding pad are cooled to room temperature, removing the growth substrate, and transferring the vertical carbon nanofiber array onto the surface of the bonding pad. The vertical carbon nanofiber array transferring method can form Au-Au bonding, enhances the bonding stability and has better process compatibility.
Description
Technical field
The present invention relates to a kind of method of transfer fiber array, and in particular to a kind of vertical carbon nanofiber arrays of transfer
Method.
Background technology
With miniaturization of electronic products and the development trend of multifunction, the packaging density and power density of electronic product by
Cumulative to add, traditional electronic interconnection material cannot meet demand for development in terms of mechanical strength and heat dispersion, need exploitation
New interconnection material.With nanotechnology and the reach of science, nano material becomes popular research object.
Carbon nano-fiber is a kind of monodimension nanometer material, its specific surface area is big, size is little, mechanical performance is excellent, high temperature and
Chemical stability is high, high current density can be carried, with the potentiality for becoming interconnection material of new generation.
Study what relatively broad vertical carbon nanofiber arrays were prepared generally by chemical vapour deposition technique at present.Base
This technological process is that the catalyst layers such as Fe, Ni are deposited with the carriers such as silicon.Then catalyst layer dispersion Cheng Na is made by heating
The catalyst particle of meter level.When the carbonaceous gas such as acetylene, methane are passed through at high temperature, carbon atom can deposit shape on catalyst particle
Into carbon nano-fiber.
Generally at 700 DEG C or so, most of electronic package materials cannot bear the growth temperature of high-quality carbon nano-fiber
This temperature.Therefore, vertical carbon nanofiber arrays need to be manufactured separately and then answer within the temperature range of electronic material can bear
Use in the middle of encapsulating structure.
Vertically the transfer techniques of carbon nanofiber arrays are the key links that it is able to apply in a package.It is main at present
Transfer method is to plate metal In in target location.The gold to be formed is reacted by the In and nanofiber surface metallization coating that melt
Category bonding realizes transfer.
However, In metal strength is low, oxidizable, can be to interconnection structure（Interconnection structure refers to pad/interconnection material/pad
This general electronic package interconnections structure）Intensity and reliability adversely affect.And, In metals are not Electronic Packagings
Middle bond pad surface commonly uses coating material, and the membership that adds of In metals causes technique unstable and cost increase.
The content of the invention
It is an object of the invention to provide a kind of method for shifting vertical carbon nanofiber arrays, this method solves existing skill
The problems such as technique that Electronic Packaging causes is unstable and cost increases is carried out using In metals in art, it is possible to increase interconnection structure
Intensity and reliability, while having more preferable processing compatibility.
In order to achieve the above object, the invention provides a kind of method of the vertical carbon nanofiber arrays of transfer, the method
Comprising：
The first step：Using chemical vapour deposition technique, vertical carbon nanofiber arrays are prepared on growth substrate；
Second step：Vertical nanofiber array obtained by the first step is put in ion sputtering equipment, is existed using ion sputtering process
The Ti coats of metal and the Au coats of metal are successively plated on every fiber surface of carbon nanofiber arrays；
3rd step：The top of the vertical carbon nanofiber arrays with the coat of metal obtained by second step is placed in into gold plated pads table
Face, described gold plated pads overlay coating is Au coating, and applying pressure and temperature makes vertical carbon nanofiber arrays with plating gold solder
Au-Au bondings are formed between panel surface coating；
4th step：Reduce temperature and be down to room temperature to the temperature of growth substrate and pad, growth substrate is removed, vertical carbon Nanowire
Dimension array is transferred to bond pad surface.
Described chemical vapour deposition technique is comprised the following steps that：
Step 1：Using silicon as described growth substrate, Ni catalyst layers are made on the silicon die, the silicon is placed into
In chemical vapor deposition growth equipment；
Step 2：Silicon is heated to into 450 ~ 640 DEG C, makes catalyst layer be changed into scattered catalyst particle, while being passed through NH3
The oxide on gas reduction metallic catalytic particles surface；
Step 3：Temperature is lifted rapidly to 700 ~ 800 DEG C, and is passed through C2H2Gas carries out the growth of carbon nanofiber arrays, raw
After length terminates, make silicon be cooled to room temperature, obtain described vertical carbon nanofiber arrays.
NH described in step 23The flow that gas is passed through is 100 ~ 300sccm.
C described in step 32H2The flow that gas is passed through is 30 ~ 60sccm.
A diameter of 25 ~ 100 nm of every fiber in described carbon nanofiber arrays, length is 5 ~ 15 μm, between fiber
Spacing be 200 ~ 500nm.
The thickness of the Ti coats of metal described in second step is 10 ~ 20nm.
The thickness of the Au coats of metal described in second step is 80 ~ 120nm.
Pressure described in 3rd step is 5 ~ 20MPa, and temperature is 200 ~ 300 DEG C.
Apply pressure and the time of temperature described in 3rd step is 3 ~ 10min.
The thickness of the Au coating on the gold plated pads surface described in the 3rd step is 50 ~ 300nm.
The method of the vertical carbon nanofiber arrays of transfer that the present invention is provided, solves in prior art to enter using In metals
The problems such as technique that row Electronic Packaging is caused is unstable and cost increases, with advantages below：
（1）The method of the vertical carbon nanofiber arrays of transfer of the present invention does material for transfer using Au, because Au is main biography
The bond pad surface coating material of system, therefore other non-Au materials can be avoided to add, to traditional material composition, pad coating structure
And do not have big impact on subsequent welding technique for sticking etc.；
（2）The method of the vertical carbon nanofiber arrays of transfer of the present invention forms Au-Au keys between carbon nano-fiber and pad
Close, can strengthen the stability of bonding, Au metals are not easy to oxidation, than with other materials such as indium metal, macromolecular adhesive material
Material transfer nanofiber effect is good, little to interconnecting electrical property and Effect of Thermal Performance.
Specific embodiment
Technical scheme is described further with reference to embodiments.
Method of the present invention for providing a kind of vertical carbon nanofiber arrays of transfer, the method it is specific as follows：
The first step：Using chemical vapour deposition technique, vertical carbon nanofiber arrays are prepared on growth substrate；
Chemical vapour deposition technique is comprised the following steps that：
Step 1：Using silicon as growth substrate, Ni catalyst layers are made on the silicon die, the silicon is placed into chemical gas
In phase deposition growing equipment；
Step 2：Silicon is heated to into 450 ~ 640 DEG C（It is preferred that 625 DEG C）, continue 5 ~ 10 min（It is preferred that 5min）, make catalysis
Oxidant layer is changed into scattered catalyst particle, while being passed through 100 ~ 300sccm（It is preferred that 200sccm）NH3Gas reduction metal catalytic grain
The oxide in sublist face；
Step 3：Temperature is lifted rapidly to 700 ~ 800 DEG C（It is preferred that 700 DEG C）, and it is passed through 30 ~ 60sccm（It is preferred that 40sccm）
C2H2Gas carries out the growth of carbon nanofiber arrays, after growth terminates, makes nitrogen of the silicon by being passed through be cooled to room temperature, obtains
To vertical carbon nanofiber arrays in every fiber a diameter of 25 ~ 100 nm（It is preferred that 42nm）, length is 5 ~ 15 μm（It is preferred that
8μm）, interfibrous spacing is 200 ~ 500 nm（It is preferred that 200nm）.
Second step：Ti metal-plateds are successively plated using ion sputtering process on every fiber surface of carbon nanofiber arrays
Layer and the Au coats of metal, by the vertical nanofiber obtained by the first step ion sputtering equipment is put into, and the Ti ion sputtering times are 10 ~
30s（It is preferred that 20s）, the Au ion sputtering times are 80 ~ 100s（It is preferred that 90s）, thickness can be obtained and be respectively 10 ~ 20nm（It is preferred that 20nm）
With 80 ~ 120nm（It is preferred that 100nm）The Ti coats of metal and the Au coats of metal；
3rd step：The top of the vertical carbon nanofiber arrays with the coat of metal obtained by second step is placed in into gold plated pads table
Face, the gold plated pads overlay coating is Au coating, and thickness of coating is 50 ~ 300nm, and the pressure of applying is 5 ~ 20MPa（It is preferred that
10MPa）, temperature is 200 ~ 300 DEG C（It is preferred that 300 DEG C）, the time is 3 ~ 10min（It is preferred that 5min）, make vertical carbon nano-fiber battle array
Row are bonded with formation Au-Au between gold plated pads overlay coating；
4th step：Reduce temperature and be down to room temperature to the temperature of growth substrate and pad, growth substrate is removed, vertical carbon Nanowire
Dimension array is transferred to bond pad surface.
The method of the vertical carbon nanofiber arrays of transfer of the present invention plates Au on carbon nanofiber arrays, metal Au
Material for transfer is done, Au is main traditional bond pad surface coating material, it is to avoid other non-Au materials are added, to traditional material
Composition, pad coating structure and big impact is not had on subsequent welding technique for sticking etc., and Au stability is preferably, than with
Other materials such as indium metal, macromolecular adhesive material transfer nanofiber effect is good, to interconnecting electrical property and Effect of Thermal Performance
It is little, with more preferable processing compatibility.
In sum, method of the present invention for providing a kind of vertical carbon nanofiber arrays of transfer, the method is done with Au
Material for transfer, the method that Au-Au bondings are formed between carbon nano-fiber and pad, can strengthen the stability of bonding, and
Impact will not be produced on interconnection structure, with more preferable processing compatibility.
Although present disclosure has been made to be discussed in detail by above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read the above, for the present invention's
Various modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. the method for the vertical carbon nanofiber arrays of a kind of transfer, it is characterised in that the method is included：
The first step：Using chemical vapour deposition technique, vertical carbon nanofiber arrays are prepared on growth substrate；
Second step：Vertical nanofiber array obtained by the first step is put in ion sputtering equipment, is existed using ion sputtering process
The Ti coats of metal and the Au coats of metal are successively plated on every fiber surface of carbon nanofiber arrays；
3rd step：The top of the vertical carbon nanofiber arrays with the coat of metal obtained by second step is placed in into gold plated pads table
Face, described gold plated pads overlay coating is Au coating, and applying pressure and temperature makes vertical carbon nanofiber arrays with plating gold solder
Au-Au bondings are formed between panel surface coating；
4th step：Reduce temperature and be down to room temperature to the temperature of growth substrate and pad, growth substrate is removed, vertical carbon Nanowire
Dimension array is transferred to bond pad surface.
2. the method for the vertical carbon nanofiber arrays of transfer according to claim 1, it is characterised in that described chemical gas
Phase sedimentation is comprised the following steps that：
Step 1：Using silicon as described growth substrate, Ni catalyst layers are made on the silicon die, the silicon is placed into
In chemical vapor deposition growth equipment；
Step 2：Silicon is heated to into 450 ~ 640 DEG C, makes catalyst layer be changed into scattered catalyst particle, while being passed through NH3Gas
The oxide of body reducing metal catalytic particle surface；
Step 3：Temperature is lifted rapidly to 700 ~ 800 DEG C, and is passed through C2H2Gas carries out the growth of carbon nanofiber arrays, raw
After length terminates, make silicon be cooled to room temperature, obtain described vertical carbon nanofiber arrays.
3. the method for the vertical carbon nanofiber arrays of transfer according to claim 2, it is characterised in that described in step 2
NH3The flow that gas is passed through is 100 ~ 300sccm.
4. the method for the vertical carbon nanofiber arrays of transfer according to claim 2, it is characterised in that described in step 3
C2H2The flow that gas is passed through is 30 ~ 60sccm.
5. the method for the vertical carbon nanofiber arrays of transfer according to any one in claim 1-4, it is characterised in that
A diameter of 25 ~ 100 nm of every fiber in described carbon nanofiber arrays, length is 5 ~ 15 μm, and the spacing between fiber is
200 ~500nm。
6. the method for the vertical carbon nanofiber arrays of transfer according to any one in claim 1-4, it is characterised in that
The thickness of the Ti coats of metal described in second step is 10 ~ 20nm.
7. the method for the vertical carbon nanofiber arrays of transfer according to any one in claim 1-4, it is characterised in that
The thickness of the Au coats of metal described in second step is 80 ~ 120nm.
8. the method for the vertical carbon nanofiber arrays of transfer according to any one in claim 1-4, it is characterised in that
Pressure described in 3rd step is 5 ~ 20MPa, and temperature is 200 ~ 300 DEG C.
9. the method for the vertical carbon nanofiber arrays of transfer according to claim 8, it is characterised in that described in the 3rd step
The time for applying pressure and temperature be 3 ~ 10min.
10. the method for the vertical carbon nanofiber arrays of transfer according to any one in claim 1-4, its feature exists
In the thickness of the Au coating on the gold plated pads surface described in the 3rd step is 50 ~ 300nm.
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| CN201611065243.9A CN106591837A (en) | 2016-11-28 | 2016-11-28 | Vertical carbon nanofiber array transferring method |
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| CN201611065243.9A CN106591837A (en) | 2016-11-28 | 2016-11-28 | Vertical carbon nanofiber array transferring method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108109981A (en) * | 2017-12-05 | 2018-06-01 | 上海无线电设备研究所 | The method that solder joint thermal fatigue resistance is improved using vertical carbon nano-tube fibre array |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896207A (en) * | 2014-04-14 | 2014-07-02 | 河南省科学院应用物理研究所有限公司 | Carbon nano-tube array bonding method based on force-electric thermal coupling |
-
2016
- 2016-11-28 CN CN201611065243.9A patent/CN106591837A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896207A (en) * | 2014-04-14 | 2014-07-02 | 河南省科学院应用物理研究所有限公司 | Carbon nano-tube array bonding method based on force-electric thermal coupling |
Non-Patent Citations (1)
| Title |
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| ROBERT CROSS,ET AL.: "A metallization and bonding approach for high performance carbon nanotube thermal interface materials", 《NANOTECHNOLOGY》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108109981A (en) * | 2017-12-05 | 2018-06-01 | 上海无线电设备研究所 | The method that solder joint thermal fatigue resistance is improved using vertical carbon nano-tube fibre array |
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