CN108220924A - A kind of preparation method of Copper thin film - Google Patents
A kind of preparation method of Copper thin film Download PDFInfo
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- CN108220924A CN108220924A CN201810077450.9A CN201810077450A CN108220924A CN 108220924 A CN108220924 A CN 108220924A CN 201810077450 A CN201810077450 A CN 201810077450A CN 108220924 A CN108220924 A CN 108220924A
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/08—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material
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Abstract
The present invention provides a kind of preparation method of Copper thin film, this method includes：Using liquid metal as template, NaOH solution is deposition liquid phase medium, and copper-containing compound is added in into NaOH solution, prepares Copper thin film.Copper thin film physical characteristic prepared by the present invention is uniform, fine and close, thickness uniform, controllable, it is easy to operate, efficiently convenient, the continuous controllable flexible Copper thin film from nanoscale to micro-meter scale thickness can be achieved, with higher conductivity, there is stronger production applicability, can be applied in the fields such as metal line, microfluidic device, biochip or semiconductor chip surface technology in super large-scale integration and microelectromechanical systems (MEMS).
Description
Technical field
The present invention relates to field of material preparation more particularly to a kind of preparation methods of Copper thin film.
Background technology
Metallic copper has high conductivity and low electromigration, gradually substitution aluminium and be applied to the hardware cloth of integrated circuit
In line, in super large-scale integration and microelectromechanical systems (MEMS) metal line to the hair of sub-micro technology
It opens up, the packaging density of device is continuously increased in chip, and plural layers interconnection process is manufactured as research neck important in industry
Domain.Metal thin copper film line width develops to tens nano-fabrication techniques.However the reduction of characteristic size causes semiconductor devices
Performance is constantly subjected to the influence of RC delays, hinders the developing steps of microelectronics manufacturing industry.
The method of the Copper thin film prepared at present mainly has surface chemistry sedimentation and vapour deposition process：Surface chemistry sedimentation
It is that self-catalysis can be carried out on the matrix surface with catalytic activity using the metal salt in same solution and reducing agent
The principle of redox reaction forms metal or alloy coating in matrix surface chemical deposition.Vapour deposition process is divided into as physics
Be vapor-deposited (PVD) and chemical vapor deposition (CVD).PVD technique is mainly that ionized physical vapor deposition prepares deposition copper seed
Crystal layer；CVD technology presoma and reactant are existed simultaneously in reaction chamber, under certain reaction condition, betide gas phase or
The deposition process of person's substrate surface.
Therefore, the preparation method of traditional Copper thin film is to deposit to prepare in the surface of solids, and there are thin film separation hardly possible, technique is multiple
It is miscellaneous, the shortcomings of coating stress is big, it is difficult to realize the separation of flexible Copper thin film.
Invention content
In order to solve in traditional Copper thin film preparation method, it need to deposit and prepare in the surface of solids, there are thin film separation hardly possible, works
The problems such as skill is complicated, and coating stress is big, the present invention provides a kind of preparation method of Copper thin film, including：It is heavy using liquid metal
Product module plate, NaOH solution are deposition liquid phase medium, and copper-containing compound is added in into NaOH solution, prepares Copper thin film.
Preferably, the preparation method of this Copper thin film specifically includes：S1, by liquid metal precipitants in NaOH solution；S2,
The copper-containing compound that D90 grain sizes are 50nm-1 μm is added in NaOH solution；S3, heating NaOH solution, by sedimentation time, obtain
It is grown in the Copper thin film of liquid metal surface；S4, Copper thin film and liquid metal are detached, obtains Copper thin film.
Preferably, in step S4, Copper thin film is Nanometer Copper.
Preferably, in step S1, liquid metal is alloy, and the component of alloy includes 60-90wt%Ga, 10-30wt%In,
0-30wt%Sn, 0-2wt%Zn.
Preferably, in step S1, a concentration of 0.1-2mol/L of NaOH solution, the volume ratio of liquid metal and NaOH solution is
0.1~10:10.
Preferably, in step S2, the mass ratio of copper-containing compound and NaOH solution is 0.01~1:100；Copper-containing compound
Component include CuO.
Preferably, in step S3, NaOH solution is heated to 25-95 DEG C；Sedimentation time is 1-48h.
Preferably, NaOH solution, liquid metal and copper-containing compound are placed in quartz glass culture dish.
Be preferably based on this Copper thin film preparation method production chip, suitable for include metal line, microfluidic device,
The MEMS of biochip or semiconductor chip (super large-scale integration and microelectromechanical systems) is applied.
The present invention provides a kind of preparation method of Copper thin film, using the liquid metal that is located in NaOH solution as growth mould
Plate adds the copper-containing compound of CuO in NaOH solution, obtains being grown in the Copper thin film of liquid metal surface by heating,
Copper-containing compound and liquid metal are detached again, obtain Copper thin film.Copper thin film physical characteristic prepared by the present invention uniformly, cause
Close, thickness uniform, controllable is easy to operate, efficiently convenient, it can be achieved that continuous controllable soft from nanoscale to micro-meter scale thickness
Property Copper thin film, have higher conductivity, have stronger production applicability, can be in super large-scale integration and microelectron-mechanical
The fields such as metal line, microfluidic device, biochip or semiconductor chip surface technology are applied in system (MEMS).
Description of the drawings
Fig. 1 is the schematic diagram according to the Copper thin film preparation method of a preferred embodiment of the invention；
Fig. 2 is the flow chart according to the Copper thin film preparation method of a preferred embodiment of the invention；
Fig. 3 is the XRD diagram of Copper thin film prepared according to the embodiment of the present invention 1；
Fig. 4 is the SEM cross-section diagrams of Copper thin film prepared according to the embodiment of the present invention 2；
Fig. 5 is the SEM cross-section diagrams of Copper thin film prepared according to the embodiment of the present invention 3；
Fig. 6 is the SEM exterior views of Copper thin film prepared according to the embodiment of the present invention 3；
Wherein：
1. 2. liquid metal of Copper thin film, 3. copper-containing compound
4.NaOH solution.
Specific embodiment
With reference to the accompanying drawings and examples, the specific embodiment of the present invention is described in further detail.Implement below
Example is used to illustrate the present invention, but be not limited to the scope of the present invention.
Fig. 1 is according to the schematic diagram of the Copper thin film preparation method of a preferred embodiment of the invention, as shown in Figure 1, this hair
It is bright to provide a kind of preparation method of Copper thin film, including：Using liquid metal as deposition template, NaOH solution is situated between for deposition liquid phase
Matter adds in copper-containing compound into NaOH solution, prepares Copper thin film.
Specifically, the present embodiment immerses liquid metal conduct using NaOH solution as deposition liquid phase medium in NaOH solution
Template is deposited, copper-containing compound is added in into NaOH solution, makes copper-containing compound that reduction reaction occur in NaOH solution, so as to
In Copper thin film prepared by liquid metal surface generation.
Fig. 2 is according to the flow chart of the Copper thin film preparation method of a preferred embodiment of the invention, as shown in Fig. 2, this hair
It is bright to provide a kind of preparation method of Copper thin film, including：S1, liquid metal 2 is deposited in NaOH solution 4；It is S2, molten in NaOH
The copper-containing compound 3 that D90 grain sizes are 50nm-1 μm is added in liquid 4；S3, heating NaOH solution 4, by sedimentation time, are given birth to
Grow the Copper thin film 1 on 2 surface of liquid metal；S4, Copper thin film 1 and liquid metal 2 are detached, obtains Copper thin film 1.
Specifically, liquid metal 2 and NaOH solution 4 are immiscible, liquid metal 2 are deposited in NaOH solution 4, NaOH is molten
Liquid 4 is used as template as deposition liquid phase medium, liquid metal 2；It is 50nm-1 μm that D90 grain sizes will be added in NaOH solution 4 again
Copper-containing compound 3；Then will wherein immerse has liquid metal 2, and the copper-containing compound that D90 grain sizes are 50nm-1 μm is mixed into solution
3 NaOH solution 4 heats so that copper-containing compound 3 is deposited on 2 surface of liquid metal, finally extracts copper-containing compound 3 out, will
Copper-containing compound 3 and liquid metal 2 detach, and obtain required Copper thin film 1.
Further, in order to form more careful Copper thin film 1,3 grain size of copper-containing compound for adding in NaOH solution 4 is preferred
For 50-200nm.
Liquid metal 2 of the present embodiment to be immersed in NaOH solution 4 adds group as template in NaOH solution 4
Part includes the copper-containing compound 3 of CuO, obtains being grown in the Copper thin film 1 on 2 surface of liquid metal by heating, then by cupric chemical combination
Object 3 and liquid metal 2 detach, and obtain Copper thin film 1.
Based on above-described embodiment, in step S1, liquid metal 2 is alloy, and the component of alloy includes 60-90wt%Ga, 10-
30wt%In, 0-30wt%Sn, 0-2wt%Zn.
Further, in order to form more careful Copper thin film 1, the component of liquid metal 2 is preferably 65-75wt%Ga,
15-25wt%In, 10-15wt%Sn, 0.5-1wt%Zn.
Further, in step S1,4 a concentration of 0.1-2mol/L of NaOH solution, the body of liquid metal 2 and NaOH solution 4
Product is than being 0.1~10:10.
Further, in step S2, the mass ratio of copper-containing compound 3 and NaOH solution 4 is 0.01~1:100；Cupric
The component for closing object 3 includes CuO.
Based on above-described embodiment, in step S3, NaOH solution 4 is heated to 25-95 DEG C；Sedimentation time is 1-48h.
Specifically, in order to enable copper-containing compound 3 is deposited on 2 surface of liquid metal, will wherein immerse has liquid metal 2,
The NaOH solution 4 that the copper-containing compound 3 that D90 grain sizes are 50nm-1 μm is mixed into solution is heated to 25-95 DEG C, by 1-48h's
Sedimentation time obtains being grown in the Copper thin film 1 on 2 surface of liquid metal.
Based on above-described embodiment, in step S4, Copper thin film 1 is Nanometer Copper.
Specifically, liquid metal 2 and Copper thin film 1 are detached, obtains the Copper thin film 1 for Nanometer Copper.
Based on above-described embodiment, NaOH solution 4, liquid metal 2 and copper-containing compound 3 are placed in quartz glass culture dish
In.
Specifically, NaOH solution 4 has stronger alkalinity, and the experimental situation of 1 preparation method of this Copper thin film uses quartzy glass
Glass culture dish so that NaOH solution 4, liquid metal 2 and copper-containing compound 3 are placed with being prepared in quartz glass culture dish
Process.
Based on above-described embodiment, three specific complete embodiments of the preparation method of this Copper thin film are given below, in detail
It is described below：
Embodiment 1
S1, it is 75.5wt%Ga by 5 parts of component, the liquid metal of 24.5wt%In adds in 10 parts of a concentration of 1mol/L
NaOH solution in, make liquid metal precipitants in NaOH solution；
S2,1 part of D90 grain size 50nm is added in NaOH solution, purity is 99.99% CuO powder；
S3, NaOH solution being heated to 50 DEG C with water-bath, CuO powder carries out reduction reaction, by the sedimentation time of 12h,
Obtain being grown in the Copper thin film of liquid metal surface；
The liquid metal of S4, extraction surface growth Copper thin film, liquid metal and Copper thin film are detached, obtain Copper thin film, is surveyed
Try its object phase.
Fig. 3 is the SEM cross-section diagrams of Copper thin film prepared according to the embodiment of the present invention, as shown in Figure 3, it can be seen that embodiment
1 Copper thin film prepared is made of Nanometer Copper, and thickness is about 300nm.
Embodiment 2
S1, by 10 parts of component be 68.5wt%Ga, 20.5wt%In and 10.5wt%Sn liquid metal, add in 10 parts
In the NaOH solution of a concentration of 0.5mol/L, make liquid metal precipitants in NaOH solution；
S2, added in NaOH solution by 0.01 part of D90 grain size 50nm, CuO powder that purity is 99.99% and 0.01 part it is pure
Spend the CuCl for 99.99%2The copper-containing compound of composition；
S3, NaOH solution is heated to 30 DEG C with water-bath, copper-containing compound carries out reduction reaction, by deposition for 24 hours
Time obtains being grown in the Copper thin film of liquid metal surface；
The liquid metal of S4, extraction surface growth Copper thin film, liquid metal and Copper thin film are detached, obtain Copper thin film, is surveyed
Try its microscopic appearance.
Fig. 4 is the XRD diagram of Copper thin film prepared according to the embodiment of the present invention, as shown in Figure 4, it can be seen that embodiment 2 is made
Standby Copper thin film is made of fine copper.
Embodiment 3
S1, by 5 parts of component be 67.5wt%Ga, 20.5wt%In, 10.5wt%Sn and 1wt%Zn liquid metal,
It adds in the NaOH solution of 10 parts of a concentration of 0.5mol/L, makes liquid metal precipitants in NaOH solution；
S2, added in NaOH solution by 0.02 part of D90 grain size 50nm, CuO powder that purity is 99.99%, 0.03 part it is pure
Spend the CuCl for 99.99%2With the CuSO that 0.5 part of purity is 99.99%4The copper-containing compound of composition；
S3, NaOH solution is heated to 50 DEG C with water-bath, copper-containing compound carries out reduction reaction, by the deposition of 36h
Time obtains being grown in the Copper thin film of liquid metal surface；
The liquid metal of S4, extraction surface growth Copper thin film, liquid metal and Copper thin film are detached, obtain Copper thin film, is surveyed
Try its microscopic appearance.
Fig. 5 is the SEM cross-section diagrams of Copper thin film prepared according to the embodiment of the present invention, and Fig. 6 is according to embodiment of the present invention system
The SEM exterior views of standby Copper thin film, as shown in Figure 5 and Figure 6, it can be seen that Copper thin film prepared by embodiment 3 is made of Nanometer Copper.
It should be noted that the number in embodiment 1, embodiment 2, embodiment 3 refers to volume ratio.
Based on above-described embodiment, the chip of the preparation method production based on this Copper thin film, suitable for including metal line, micro-
Flow MEMS (the super large-scale integration and microelectromechanical systems) applications of device, biochip or semiconductor chip.
The present invention provides a kind of preparation method of Copper thin film, using the liquid metal that is located in NaOH solution as growth mould
Plate adds the copper-containing compound of CuO in NaOH solution, obtains being grown in the Copper thin film of liquid metal surface by heating,
Copper-containing compound and liquid metal are detached again, obtain Copper thin film.Copper thin film physical characteristic prepared by the present invention uniformly, cause
Close, thickness uniform, controllable is easy to operate, efficiently convenient, it can be achieved that continuous controllable soft from nanoscale to micro-meter scale thickness
Property Copper thin film, have higher conductivity, have stronger production applicability, can be in super large-scale integration and microelectron-mechanical
The fields such as metal line, microfluidic device, biochip or semiconductor chip surface technology are applied in system (MEMS).
Finally, method of the invention is only preferable embodiment, is not intended to limit the scope of the present invention.It is all
Within the spirit and principles in the present invention, any modification, equivalent replacement, improvement and so on should be included in the protection of the present invention
Within the scope of.
Claims (8)
1. a kind of preparation method of Copper thin film, which is characterized in that including：
Using liquid metal as deposition template, NaOH solution is deposition liquid phase medium, and cupric chemical combination is added in into the NaOH solution
Object prepares the Copper thin film.
2. a kind of preparation method of Copper thin film according to claim 1, which is characterized in that including：
S1, the liquid metal is immersed in the NaOH solution；
S2, the copper-containing compound that D90 grain sizes are 50nm-1 μm is added in the NaOH solution；
S3, the heating NaOH solution, by sedimentation time, obtain being grown in the Copper thin film of the liquid metal surface；
S4, the Copper thin film and the liquid metal are detached, obtains the Copper thin film.
3. a kind of preparation method of Copper thin film according to claim 2, which is characterized in that in step S1, the liquid gold
Belong to for alloy, the component of the alloy includes 60-90wt%Ga, 10-30wt%In, 0-30wt%Sn, 0-2wt%Zn.
4. the preparation method of a kind of Copper thin film according to claim 2, which is characterized in that in step S1, the NaOH is molten
The volume ratio of a concentration of 0.1-2mol/L of liquid, the liquid metal and the NaOH solution is 0.1~10:10.
5. a kind of preparation method of Copper thin film according to claim 2, which is characterized in that in step S2, the cupric
The mass ratio for closing object and the NaOH solution is 0.01~1:100；The component of the copper-containing compound includes CuO.
6. the preparation method of a kind of Copper thin film according to claim 2, which is characterized in that described in the step S3
NaOH solution is heated to 25-95 DEG C；The sedimentation time is 1-48h.
7. a kind of preparation method of Copper thin film according to claim 2, which is characterized in that in the step S4, the copper
Film is Nanometer Copper.
A kind of 8. chip of the preparation method production based on claim 1-7 any one of them Copper thin films, which is characterized in that institute
It states chip to apply suitable for MEMS (super large-scale integration and microelectromechanical systems), the field of the MEMS applications includes
Metal line, microfluidic device, biochip or semiconductor chip.
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Citations (5)
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| CN101483149A (en) * | 2009-02-13 | 2009-07-15 | 华中科技大学 | Production method for through wafer interconnection construction |
| CN101582396A (en) * | 2008-05-05 | 2009-11-18 | 英飞凌科技股份有限公司 | Semiconductor device and manufacturing of the same |
| WO2015180845A1 (en) * | 2014-05-26 | 2015-12-03 | L'air Liquide Societe Anonyme Pour L'etude Et L' Exploitation Des Procedes Georges Claude | Method for removing metal from high-boiling hydrocarbon fractions |
| CN107557718A (en) * | 2016-06-24 | 2018-01-09 | 中国科学院理化技术研究所 | A kind of method for preparing inorganic nano material layer on flexible material surface |
| CN107573922A (en) * | 2017-08-01 | 2018-01-12 | 北京梦之墨科技有限公司 | A kind of liquid metal quantum material and preparation method thereof |
-
2018
- 2018-01-26 CN CN201810077450.9A patent/CN108220924B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101582396A (en) * | 2008-05-05 | 2009-11-18 | 英飞凌科技股份有限公司 | Semiconductor device and manufacturing of the same |
| CN101483149A (en) * | 2009-02-13 | 2009-07-15 | 华中科技大学 | Production method for through wafer interconnection construction |
| WO2015180845A1 (en) * | 2014-05-26 | 2015-12-03 | L'air Liquide Societe Anonyme Pour L'etude Et L' Exploitation Des Procedes Georges Claude | Method for removing metal from high-boiling hydrocarbon fractions |
| CN107557718A (en) * | 2016-06-24 | 2018-01-09 | 中国科学院理化技术研究所 | A kind of method for preparing inorganic nano material layer on flexible material surface |
| CN107573922A (en) * | 2017-08-01 | 2018-01-12 | 北京梦之墨科技有限公司 | A kind of liquid metal quantum material and preparation method thereof |
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